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2017
Editors
Hojong Kim
Shafiq Alam
Neale R. Neelameggham
Harald Oosterhof
Takanari Ouchi
Xiaofei Guan
The Minerals, Metals & Materials Series
Hojong Kim Shafiq Alam
•
Neale R. Neelameggham
Harald Oosterhof Takanari Ouchi
•
Xiaofei Guan
Editors
Rare Metal Technology 2017
123
Editors
Hojong Kim Harald Oosterhof
Pennsylvania State University Umicore
University Park, PA Olen
USA Belgium
Shafiq Alam Takanari Ouchi
University of Saskatchewan Massachusetts Institute of Technology
Saskatoon, SK Cambridge, MA
Canada USA
Neale R. Neelameggham Xiaofei Guan
IND LLC Watertown, MA
South Jordan, UT USA
USA
ISSN 2367-1181 ISSN 2367-1696 (electronic)
The Minerals, Metals & Materials Series
ISBN 978-3-319-51084-2 ISBN 978-3-319-51085-9 (eBook)
DOI 10.1007/978-3-319-51085-9
TMS owns copyright; Springer has full administrative rights
Library of Congress Control Number: 2016960563
© The Minerals, Metals & Materials Society 2017
This work is subject to copyright. All rights are reserved by the Publisher, whether the whole or part
of the material is concerned, specifically the rights of translation, reprinting, reuse of illustrations,
recitation, broadcasting, reproduction on microfilms or in any other physical way, and transmission
or information storage and retrieval, electronic adaptation, computer software, or by similar or dissimilar
methodology now known or hereafter developed.
The use of general descriptive names, registered names, trademarks, service marks, etc. in this
publication does not imply, even in the absence of a specific statement, that such names are exempt from
the relevant protective laws and regulations and therefore free for general use.
The publisher, the authors and the editors are safe to assume that the advice and information in this
book are believed to be true and accurate at the date of publication. Neither the publisher nor the
authors or the editors give a warranty, express or implied, with respect to the material contained herein or
for any errors or omissions that may have been made.
Printed on acid-free paper
This Springer imprint is published by Springer Nature
The registered company is Springer International Publishing AG
The registered company address is: Gewerbestrasse 11, 6330 Cham, Switzerland
Preface
Rare Metal Technology 2017 is the proceedings of the symposium on rare metal
extraction and processing sponsored by the Hydrometallurgy and Electrometallurgy
Committee of the TMS Extraction and Processing Division. The symposium has
been organized to encompass the extraction of rare metals as well as rare extraction
processing techniques used in metal production and mineral processing. This is the
fourth symposium since 2014, which will be held in San Diego, California.
This symposium intends to cover research and developments in the extraction
and processing of less common rare metals that are not covered by other TMS
symposia. These elements include antimony, bismuth, barium, beryllium, boron,
calcium, chromium, gallium, germanium, hafnium, indium, manganese, molybde-
num, platinum group metals, rare earth metals, rhenium, scandium, selenium,
sodium, strontium, tantalum, tellurium, and tungsten. These are rare metals of low
tonnage sales compared to high tonnage metals such as iron, copper, nickel, lead,
tin, zinc, or light metals such as aluminum, magnesium, or titanium and electronic
metalloid silicon. Rare processing includes bio-metallurgy, hydrometallurgy, and
electrometallurgy, as well as extraction of values from electric arc furnace
(EAF) dusts, and less common waste streams not discussed in recycling symposia.
Rare high-temperature processes included microwave heating, solar-thermal reac-
tion synthesis, molten salt electrochemical processes, cold crucible synthesis of the
rare metals, and the design of extraction equipment used in these processes as well
as laboratory and pilot plant studies.
This volume covers extraction and processing techniques of various platinum
group metals, rare earth elements as well as other less common metals such as
arsenic, indium, antimony, molybdenum, chromium, titanium, and vanadium,
including electrochemical processing, aqueous processing, biological separation,
and microwave heating. The symposium is organized into the following sessions:
(1) Rare-Earth Elements, (2) Platinum Group Metals, and (3) Base and Rare Metals
(Co, Cr, Sn, Ti, Mo and V).
We acknowledge the efforts of the symposium organizers and proceedings
editors: Hojong Kim, Shafiq Alam, Neale R. Neelameggham, Harald Oosterhof,
Takanari Ouchi, and Xiaofei Guan. The support from TMS staff members Trudi
v
vi Preface
Dunlap and Patricia Warren is greatly appreciated in assembling and publishing the
proceedings. We sincerely thank all the authors, speakers, and participants and look
forward to continued collaboration in the advancement of science and technology in
the area of rare metal extraction and processing.
Hojong Kim
Lead Organizer
Contents
Part I Rare Earth Elements I
The Economics of the Search Minerals Direct Extraction
Process for Rare Earth Element Recovery . . . . . . . . . . . . . . . . . . . . . . . . 3
David Dreisinger and Greg Andrews
Recovery of Critical Rare Earth Elements for Green Energy
Technologies . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
Jyothi Rajesh Kumar and Jin-Young Lee
Selective Reduction and Separation of Europium from Mixed
Rare-Earth Oxides from Waste Fluorescent Lamp Phosphors . . . . . . . . 31
Mark L. Strauss, Brajendra Mishra and Gerard P. Martins
Application of Rare Earths for Higher Efficiencies in Energy
Conversion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
W.D. Judge, Z.W. Xiao and G.J. Kipouros
Microwave Treatment for Extraction of Rare Earth Elements
from Phosphogypsum . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47
Adrian Lambert, Jason Tam and Gisele Azimi
Selective Separation of Rare Earth Chlorides Utilizing
Vapor Phase Extraction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
Katelyn M. Lyons, Jerome P. Downey, Jannette L. Chorney
and Katie J. Schumacher
Microstructure Observation of Oxidation of Nd-Magnet
at High Temperatures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65
Muhamad Firdaus, M. Akbar Rhamdhani, Yvonne Durandet,
W. John Rankin, Kathie Mcgregor and Nathan A.S. Webster
vii
viii Contents
Part II Rare Earth Elements II and Platinum Group Metals
Electrochemical Behavior of Neodymium in Molten
Chloride Salts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 77
L. Diaz, P. Chamelot, M. Gibilaro, L. Massot and J. Serp
Novel Reactive Anode for Electrochemical Extraction
of Rare Earth Metals from Rare Earth Oxides . . . . . . . . . . . . . . . . . . . . 87
Aida Abbasalizadeh, Seshadri Seetharaman, Prakash Venkatesan,
Jilt Sietsma and Yongxiang Yang
Electrochemical Formation of Nd Alloys Using Liquid
Metal Electrodes in Molten LiCl–KCl Systems . . . . . . . . . . . . . . . . . . . . . 93
Hirokazu Konishi, Hideki Ono, Eiichi Takeuchi, Toshiyuki Nohira
and Tetsuo Oishi
Challenges in the Electrolytic Refining of Silver—Influencing
the Co-deposition Through Parameter Control. . . . . . . . . . . . . . . . . . . . . 103
Ann-Kathrin Maurell-Lopez, Bernd Friedrich and Wolfgang Koch
Vapor Treatment for Alloying and Magnetizing Platinum
Group Metals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 119
Yu-ki Taninouchi and Toru H. Okabe
Biotechnological Recovery of Platinum Group Metals from
Leachates of Spent Automotive Catalysts . . . . . . . . . . . . . . . . . . . . . . . . . 129
Norizoh Saitoh, Toshiyuki Nomura and Yasuhiro Konishi
Recovering Palladium from Chloridizing Leaching Solution
of Spent Pd/Al2O3 Catalyst by Sulfide Precipitation . . . . . . . . . . . . . . . . . 137
Qian Li, Qiang Zou, Bin Xu, Yongbin Yang, Xuefei Rao, Long Hu
and Tao Jiang
Mechanism of Intensifying Cyanide Leaching of Gold from
a Calcine by the Pretreatment of Acid or Alkali Washing . . . . . . . . . . . . 147
Yan Zhang, Qian Li, Xiaoliang Liu, Yongbin Yang, Bin Xu, Tao Jiang
and Hongwei Li
Part III Base and Rare Metals
Disclosure of the Kinetic Relations of Semidirect Cemented
Carbide Leaching in Acid Media . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 159
Gregor Kücher, Stefan Luidold, Christoph Czettl and Christian Storf
A New Two-Stage Aluminothermic Reduction Process
for Preparation of Ti/Ti-Al Alloys . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 167
Kun Zhao and Naixiang Feng
Contents ix
Study on Pre-reduction Mechanisms of Chromium Ore
Pellets in SRC Process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 177
Pei-xiao Liu, Yan-xiang Li and Han-jie Guo
Recovery of Valuable Metals from High-Content Arsenic
Containing Copper Smelting Dust . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 183
Xuepeng Li and Dachun Liu
Sulfuric Acid Leaching of Mechanically Activated
Vanadium–Bearing Converter Slag . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 193
Junyi Xiang, Qingyun Huang, Xuewei Lv and Chenguang Bai
Present Status and Development of Comprehensive Utilization
of Vanadium-Titanium Magnetite . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 203
Shiju Zhang, Songli Liu, Wenhui Ma, Kuisong Zhu, Li Cao
and Yongnian Dai
Review of TiO2-Rich Materials Preparation for the
Chlorination Process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 211
Songli Liu, Li Cao, Kuisong Zhu, Shiju Zhang and Kui He
Part IV Poster Session
Adsorbents for Selective Recovery of Heavy Rare Earth Elements . . . . . 219
Takeshi Ogata, Hirokazu Narita and Mikiya Tanaka
Behavior of Sec-Octylphenoxy Acetic Acid (CA-12)
in Yttrium Recovery from High Concentrated Heavy
Rare Earths Mixture. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 225
Corradino Sposato, Alessandro Blasi, Assunta Romanelli,
Giacobbe Braccio and Massimo Morgana
Preparation of Molybdenum Powder from Molybdenite
Concentrate Through Vacuum Decomposition-Acid
Leaching Combination Process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 235
Chongfang Yang, Yuezhen Zhou, Dachun Liu, Wenlong Jiang,
Fansong Liu and Zewei Liu
Pressure Leaching Behavior of Molybdenum-Nickel Sulfide
from Black Shale . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 247
Zhigan Deng, Xingbin Li, Chang Wei, Cunxiong Li, Gang Fan
and Minting Li
Selective Recovery of Scandium From Sulfating Roasting Red
Mud By Water Leaching . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 255
Zhaobo Liu, Hongxu Li and Zihan Zhao
x Contents
Study for Preparation of Industrial Ammonium Molybdate
from Low Grade Molybdenum Concentrate . . . . . . . . . . . . . . . . . . . . . . . 265
Qingwei Qin, Zhenwei Liu, Tiejun Chen, Zili Huang, Jianhong Yang
and Wei Han
Study of a Synergistic Solvent Extracting System to Separate
Yttrium and Heavy Rare Earths: A Deep Investigation
on System Behavior . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 277
Alessandro Blasi, Corradino Sposato, Assunta Romanelli,
Giacobbe Braccio and Massimo Morgana
The Recovery of Bismuth from Bismuthinite Concentrate
Through Membrane Electrolysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 285
Si-yao Peng, Jian-guang Yang, Jian-ying Yang and Lei Jie
Author Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 303
Subject Index. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 305
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About the Editors
Hojong Kim is Assistant Professor of Materials
Science and Engineering, and Norris B. McFarlane
Faculty Professor at the Pennsylvania State University.
Dr. Kim received his B.S. from Seoul National
University in South Korea in 2000 and Ph.D. degree at
Massachusetts Institute of Technology (MIT) in 2004
both in Materials Science and Engineering. His doc-
toral research sought to identify the corrosion mech-
anisms of constructional alloys in high temperature
and high pressure steam environments under Prof.
Ronals Latanision in the Uhlig Corrosion Laboratory
at MIT. After graduate research, Dr. Kim worked as a
senior research scientist at Samsung-Corning Precision
Glass Co. Ltd. and as a project lead to improve the
process yield for thin film transistor liquid crystal
display (TFT-LCD) glass melting processes by engi-
neering high temperature materials of refractory
ceramics (alumina and fused zirconia), molybdenum,
and platinum alloys. After five years of industrial
experience, Dr. Kim returned to MIT as a postdoctoral
associate and later as a research scientist to contribute
to the growing need for sustainable technology. He
conducted research on high temperature electrochem-
ical processes, including molten oxide electrolysis for
carbon-free iron and steel production with focus on
developing inert anode materials in molten slags as
well as molten salt liquid metal batteries for large-scale
energy storage.
Dr. Kim’s current research interests embrace the
development of environment-friendly electrochemical
processes for resource extraction/recycling,
xi
xii About the Editors
corrosion-resistant materials, as well as energy storage
systems. He was awarded The Minerals, Metals &
Materials Society (TMS) Young Leaders Professional
Development Award in 2013 from the Extraction and
Processing Division in recognition of his achievement
in the high temperature materials and electrochemical
processing. In 2015, he was chosen to receive a
Doctoral New Investigator Award from the American
Chemical Society Petroleum Research Fund for his
innovative research and education program. He is
currently leading efforts to separate
alkali/alkaline-earth elements from the used nuclear
fuel recycling processes in the molten salt electrolytes.
Dr. Kim is the lead organizer of the present Rare Metal
Extraction & Processing Symposium at the TMS 2017
Annual Meeting and is the vice-chair of the
Hydrometallurgy and Electrometallurgy Committee of
the Extraction and Processing Division.
Shafiq Alam is Associate Professor at the University of
Saskatchewan, Canada. In 1998, he received his Ph.D.
degree in Chemical Engineering from Saga University,
Japan. From 1999 to 2001, he was appointed as a post-
doctoral research fellow at the University of British
Columbia and the University of Toronto, Canada.
Dr. Alam has extensive experience in industrial
operations, management, engineering, design, consult-
ing, teaching, research, and professional services.
Before joining the University of Saskatchewan in 2014,
he was an assistant/associate professor at Memorial
University of Newfoundland for about seven years.
Prior to starting his career in academia, he worked with
many different companies, such as, Shell, Process
Research ORTECH Inc., Fluor Canada Ltd., and the
National Institute of Advanced Industrial Science and
Technology (AIST), Japan. Dr. Alam is highly experi-
enced in the area of mineral processing and extractive
metallurgy, and he possesses two patents and has more
than 140 publications. He is the co-editor of four books
and an associate editor of the International Journal of
Mining, Materials and Metallurgical Engineering
(IJMMME). He is the winner of the 2014 TMS
Extraction & Processing Division’s Technology
Award.
About the Editors xiii
Dr. Alam is a registered professional engineer and
has worked on projects with many different mining
companies including, Falconbridge, INCO (Vale),
Barrick, Hatch, Phelps Dodge, Rambler, Anaconda, etc.
He is an Executive Committee Member of the
Hydrometallurgy Section of the Canadian Institute of
Mining, Metallurgy and Petroleum (CIM) and cur-
rently, he holds the office of secretary (2013–2017). Dr.
Alam is also the chair of the Hydrometallurgy and
Electrometallurgy Committee of the Extraction &
Processing Division (EPD) of The Minerals, Metals &
Materials Society (TMS) for the period of 2015–2017.
He is a co-organizer of many symposia at the interna-
tional conferences through CIM and TMS. Dr. Alam is
also involved in organizing the TMS 2017 Symposium
on Energy, Environment and Materials Process
Engineering, which is an EPD Symposium in Honor of
Ramana Reddy focusing on applications of process
engineering principles in materials processing, energy
and environmental technologies.
Neale R. Neelameggham is ‘The Guru’ at IND LLC,
involved in international consulting in the field of
metals and associated chemicals (boron, magnesium,
titanium, and lithium and rare earth elements),
thiometallurgy, energy technologies, soil biochemical
reactor design, etc. He was a visiting expert at Beihang
University of Aeronautics and Astronautics, Beijing,
China. He was a plenary speaker at the Light Metal
Symposium in South Africa—on low carbon dioxide
emission processes for magnesium.
Dr. Neelameggham has more than 38 years of
expertise in magnesium production and was involved
in process development of its startup company NL
Magnesium through to the present US
Magnesium LLC, UT until 2011. Neelameggham and
Brian Davis authored the ICE-JNME award winning
(2016) paper—“21st Century Global Anthropogenic
Warming Convective Model”—which notes that con-
strained air mass warming is independent of the energy
conversion source—fossil or renewable energy. He is
presently developing Agricoal™ and agricoalture to
improve arid soils.
Dr. Neelameggham holds 16 patents and patent
applications, and has published several technical
xiv About the Editors
papers. He has served on the Magnesium Committee of
Light Metals Division (LMD) of TMS since its incep-
tion in 2000, chaired it in 2005, and in 2007 he was
made a permanent co-organizer for the Magnesium
Symposium. He has been a member of the Reactive
Metals Committee, Recycling Committee, Titanium
Committee, and Program Committee Representative of
LMD and LMD council.
Dr. Neelameggham was the inaugural chair, when in
2008, LMD and EPD (Extraction & Processing
Division) created the Energy Committee, and has been a
co-editor of the energy technology symposium pro-
ceedings through the present. He received the LMD
Distinguished Service Award in 2010. While he was the
chair of Hydro and Electrometallurgy Committee he
initiated the rare metal technology symposium in 2014.
He is co-editor for the 2017 proceedings for the sym-
posia on magnesium technology, energy technology,
rare metal technology, and solar cell silicon.
Harald Oosterhof graduated as a chemical engineer
from Twente University (TU) in the Netherlands in
1994. In the same year he assumed a position as
researcher at TU Delft. His research on antisolvent
crystallization of well-soluble salts was rewarded with
two patents and several publications. After receiving
his Ph.D. from Delft University in 1999, he assumed
the position of project manager at Umicore, a global
materials and technology group that is based in
Belgium. During his first assignment as Project Leader
Hydrometallurgy, he focused on the refining of cobalt,
nickel, and germanium. Since 2011, Dr. Oosterhof has
worked as a scientist in the Recycling and Extraction
Technology group at Umicore’s Central R&D depart-
ment. His main competence areas are special metals
hydrometallurgy, recycling and refining of rare earth
metals, base metal hydrometallurgy, and recycling of
spent rechargeable batteries and superalloys. In his
current job, Dr. Oosterhof is frequently involved in
business development of scarce metals recycling and
he is heading a team of hydrometallurgical specialists.
About the Editors xv
Takanari Ouchi is a research scientist in Materials
Processing Center at Massachusetts Institute of
Technology (MIT). He received his Ph.D. in
Nano-Science and Nano-Engineering from Waseda
University on 2011. He developed electrochemical
deposition processes to fabricate metal nanostructures
with both well-controlled crystallinity and uniformity
at the single nanometer scale and demonstrated the
applicability of these processes to fabrication of bit
patterned magnetic recording media for future hard
disk drives. After completing his doctoral degree, Dr.
Ouchi joined MIT, where he has developed liquid
metal batteries, which is in principle a bi-directional
electrolysis (electro-refining) cell, to apply for the
grid-scale energy storage. He led the systematic
investigation of electrochemical properties of liquid
metal electrodes in molten salt electrolytes and
developed novel lithium, calcium, and sodium
liquid metal batteries. Dr. Ouchi has been an author of
16 peer reviewed papers and conference proceedings
and of 47 talks at conferences. He has constantly
contributed to create the vibrant field of metal extrac-
tion by working as a member of Hydrometallurgy and
Electrometallurgy Committee at The Minerals, Metals
& Materials Society (TMS), organizing technical
symposiums at TMS, and soliciting papers as a guest
editor of JOM. He has earned several awards and
honors, such as TMS Extraction & Processing Division
(EPD) Young Leaders Professional Development
Award in 2015 based on his reputation in the electro-
chemical metal extraction processing.
Xiaofei Guan received his B.S. degree in Applied
Physics from Nankai University, China, in 2009, and
Ph.D. degree in Materials Science and Engineering
from Boston University in 2013. His Ph.D. research in
the group of Prof. Uday Pal was on resource recovery
and recycling, and electrolytic production of energy
intensive metals from minerals. In 2014, he joined the
Ramanathan Research Group at Harvard University as
a postdoctoral fellow, where he led research on energy
conversion and storage devices including solid oxide
fuel cells, protonic ceramic fuel cells, and hydride-air
batteries. He is currently a postdoctoral fellow in the
Clarke Research Group and the Girguis Laboratory at
xvi About the Editors
Harvard University, where his research is centered on
growth and characterization of semiconductor thin
films for solar energy applications, a joint project at
the interface between materials science, microbiology,
and electrochemistry.
Dr. Guan received the Outstanding Ph.D.
Dissertation Award in Materials Science and
Engineering from Boston University in 2014, and the
Young Leaders Professional Development Award
from the TMS Extraction & Processing Division in
2015. He also serves as an advisor and guest editor in
the Recycling and Environmental Technology
Committee for JOM.
Part I
Rare Earth Elements I
The Economics of the Search Minerals
Direct Extraction Process for Rare Earth
Element Recovery
David Dreisinger and Greg Andrews
Abstract The Foxtrot deposit of Search Minerals contains a range of rare earth
element containing minerals including allanite, fergusonite and bastnasite. The
Search Minerals Direct Extraction Process for treating these minerals involves
coarse crushing of the ore to-6 mesh (3.45 mm), acid treatment at 200 °C in a novel
reactor configuration, water leaching, various purification steps to reject iron, alu-
minum and uranium/thorium (present in small amounts) and finally precipitation of
rare earths as a oxalate and calcination to form a mixed rare earth oxide product for
refining. The economics of the process are presented.
Keywords Rare earths Extraction Mixed rare earth oxide Foxtrot Capital
and operating cost
Introduction
Search Minerals Inc. (Search) is exploring and developing a number of deposits for
rare earth element (REE) recovery in Labrador, Canada. The Port Hope Simpson
District is in the southeast of Labrador and is highly prospective for heavy and light
rare earth elements. The Foxtrot deposit sits within the Port Hope Simpson REE
District, which is 70 km long by up to 10 km wide. The infrastructure available at
Foxtrot is excellent; a deep-water port, air strip, and road and power infrastructure
are pre-existing at St. Lewis. The three communities of Port Hope Simpson,
St. Lewis and Mary’s Harbour are in close proximity to the site.
A Preliminary Economic Assessment has been developed for Foxtrot. Roscoe
Postle Associates (RPA) has determined a 43–101 compliant resource for the
Foxtrot deposit [1]. The resource comprises 7.39 Mt of Indicated Resource and
1.96 Mt of Inferred Resource. An NSR cut-off of $165/t was used for material that
could be accessed by open pit mining and $260/t was used for material to be mined
D. Dreisinger (&) G. Andrews
Search Minerals, #211, 901 West 3rd Street, North Vancouver, BC V7P 3P9, Canada
e-mail:
[email protected]© The Minerals, Metals & Materials Society 2017 3
H. Kim et al. (eds.), Rare Metal Technology 2017,
The Minerals, Metals & Materials Series,
DOI 10.1007/978-3-319-51085-9_1
4 D. Dreisinger and G. Andrews
underground. The resource is summarized in Table 1. The deposit is rich in the
critical rare earth elements Pr, Nd, and Dy.
Search Minerals have developed a direct extraction process for recovery of rare
earth elements from the Foxtrot mineralization [2–4]. This process was conceived
to meet the challenges posed in early work on Foxtrot metallurgy. Namely, the new
direct extraction process was designed to (1) eliminate complex and costly bene-
ficiation processes (e.g. gravity, flotation and magnetic separation), (2) reduce the
use of reagents (e.g. acid, base, and oxalic acid) and (3) improve the control and
rejection of key impurities including minor amounts of thorium contained in the
Foxtrot mineralization.
The direct extraction process treats crushed material (eliminating costly grinding
and beneficiation) using a low temperature acid extraction process. The acid treated
material is then water leached to extract rare earths. The leachate is then purified in
a series of steps followed by rare earth oxalate precipitation and calcination. The
mixed rare earth oxide calcine is then available for refining to individual rare earth
elements and final products.
The direct extraction process has now been the subject of an engineering design
and cost study. The details of the process and associated project capital and
operating costs are outlined below.
The Direct Extraction Process
The direct treatment of Foxtrot mineralization was investigated through a series of
studies on acid baking/water leaching, solution purification, RE precipitation, RE
re-dissolution and purification to remove thorium and finally RE precipitation with
oxalic acid and calcination to make a mixed REO. The goal again was simplifi-
cation, cost reduction and production of a premium product. The general flowsheet
for the treatment scheme is shown in Fig. 1.
The testing of the direct extraction process has been reported in Dreisinger et al.
[3, 4]. A summary of the key steps follows.
Table 1 Foxtrot resource [1]
Classification Cut-off Tonnage Pr Nd Dy LREE HREE TREE
$NSR 000s ppm ppm ppm (%) (%) (%)
Open pit
Indicated $165 4129 372 1393 177 0.69 0.17 0.86
Inferred $165 228 368 1378 179 0.68 0.17 0.85
Underground
Indicated $260 3263 429 1602 209 0.78 0.19 0.97
Inferred $260 1730 430 1602 201 0.80 0.19 0.99
Total indicated 7392 397 1485 191 0.73 0.18 0.91
Total inferred 1958 423 1576 199 0.79 0.18 0.97
The Economics of the Search Minerals … 5
Crushing Foxtrot Ore
H2O
H2SO4 Washed Residue to
Acid / Ore Mixing Acid Baking (AB) Water Leaching (WL)
Disposal
Impurity Removal (IR) Barren SoluƟon to
REE PrecipitaƟon(RP)
Fe/Al/Th Hydroxide with MgO, MgCO3 or Environmental
with Na2 CO3
Na2 CO3 Treatment
Th Precipitate + Minor REE ReLeach and
REE PrecipitaƟon
REE (potenƟal recycle Secondary Th Removal
(ROP) with H2 C2 O 4
to AB) with HCl and MgO
Mixed REO for refining CalcinaƟon
Fig. 1 Conceptual flowsheet for testing of the new Foxtrot process
Acid Treatment/Water Leach
The material is crushed to a nominal 6 mesh particle size and treated at 200 °C with
minimum acid followed by water leaching. The average extraction (Table 2) was
78% for the series La-Er. The extractions of Tm–Lu were lower. The radioactive
elements Th and U were extracted but the major gangue elements (Si, Al, Fe, Na,
K) were only weakly extracted. Some Mg, Ca, Ti, P and Mn were also extracted.
Impurity Removal by Oxidation and Precipitation
The initial removal of impurities was tested by pH adjustment to pH 3.75 with
MgCO3 and oxidation (for Fe removal). More than 90% of the iron was eliminated
along with 88.4% of the thorium. There was also significant rejection of Si, Al, Ti
and P. The losses of REEs ranged from 0.74 to 3.6% from La to Lu.
Bulk Rare Earth Precipitation
The purified solution was treated with a soda ash solution (Na2CO3) at pH 7.25 to
precipitate the REEs into a mixed carbonate product for further purification. The
precipitation of REEs approaches 100% (Table 3). The co-precipitation of Th, U,
Fe, Al is similarly very high. The mixed REE carbonate precipitate may be further
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6 D. Dreisinger and G. Andrews
Table 2 Bulk acid bake—water leach results
Rare earth extraction Impurity extraction
Element Analysis (mg/L or g/t) Extn Element Analysis (mg/L, % or g/t) Extn
Feed PLS Residue (%) Feed PLS Residue (%)
La 1720 144 392 76.7 Th 109 9.35 34.6 70.4
Ce 3720 321 805 78.1 U 22.4 1.2 13.5 44.4
Pr 437 39.7 90.8 79.6 Si 31.32 288 32.44 0.8
Nd 1610 148 330 80.0 Al 3.99 212 3.97 4.6
Sm 297 27.9 63.8 79.6 Fe 7.83 496 7.69 5.5
Eu 15.5 1.51 3.6 79.1 Mg 0.12 43.5 0.07 36.7
Gd 244 22.6 56.1 78.4 Ca 1.45 642 0.96 40.0
Tb 37.3 3.59 8.5 79.2 Na 2.13 47 2.14 2.6
Dy 223 20.8 54.6 77.5 K 3.36 384 3.44 9.2
Ho 43.7 4.09 11.7 76.0 Ti 0.27 4.6 0.28 1.5
Y 1090 107 288 77.0 P 0.01 5 0.02 33.5
Er 122 11.2 36 73.8 Mn 0.23 82.3 0.19 27.6
Tm 17.2 1.49 5.8 69.9
Yb 111 8.56 41.8 64.9
Lu 15.8 1.02 7.3 55.9
Conditions: acid bake at 6 mesh, 200 °C, 2 and 24 h water leach at 90 °C with 600 rpm mixing
intensity
Table 3 REE Prec. results
Rare earth precipitation Impurity precipitation
Element Analysis (mg/L or g/t) Pptn Element Analysis (mg/L, % or g/t) Pptn
Feed Filtrate Ppte (%) Feed Filtrate Ppte (%)
Soln Soln
La 134 0.24 57,700 99.8 Th 0.84 0.04 422 95.7
Ce 315 0.39 129,000 99.9 U 1.07 0.13 467 88.4
Pr 36.3 0.06 15,600 99.8 Al 83.6 0.05 3.67 99.4
Nd 136 0.18 58,800 99.9 Fe 39.3 0.2 1.81 99.5
Sm 26.1 0.05 11,000 99.8 Mg 1550 1560 0.505 0.7
Eu 1.39 0.03 584 97.6 Ca 616 583 1.95 6.6
Gd 23 0.04 10,900 99.8 Na 191 1050 0.125 0.3
Tb 3.62 0.03 1640 99.1 K 298 289 0.03 2.2
Dy 20.8 0.05 9270 99.7 P 5 5 0.003 1.2
Ho 4.08 0.02 1800 99.5 Mn 77.4 68.8 0.131 3.9
Y 107 0.3 42,100 99.7
Er 11.1 0.04 4880 99.6
Tm 1.46 0.04 636 97.1
Yb 7.92 0.03 3470 99.6
Lu 0.93 0.03 409 96.6
Conditions: pH 7.25 with Na2CO3 addition for 3 h at 25 °C [4]
The Economics of the Search Minerals … 7
refined by a re-leach, oxalate precipitation and calcination method to form a mixed
REO for refining. The overall recovery of REEs from the original mineralized
material to mixed carbonate precipitate has been calculated and summarized in
Table 4.
The mixed REE carbonate precipitate was re-dissolved in HCl solution followed
by pH adjustment for purification and oxalic acid precipitation. The REE oxalate
was then calcined to make a mixed REO product. The analysis of the mixed REO
product from the testing is summarized in Table 5. This product was generated in a
continuous kiln test campaign of the acid treatment followed by batch water leach
and purification (as outlined above).
The final product analyzed 98.9% REO+Y with <0.01% S, < 0.01% F, 2 g/t, Th
and 97 g/t U. Other key impurity values were 93 g/t Si, 0.15% Ca, 44 g/t P, 465 g/t
Mn, 34 g/t Cr, 23 g/t Sr, and 56 g/t V. The critical and highly values rare earths (Pr,
Nd, Eu, Tb, Dy, Y) accounted for 37.95% of the Mixed REO oxide.
The direct extraction process has been demonstrated to be technically feasible.
The Foxtrot mineralization can be crushed, acid treated, and leached with the
leachate purified to recover a mixed rare earth oxide for refining. At the present time
Table 4 Overall recovery (%) of rare earth elements from Foxtrot material to mixed carbonate
precipitate
La Ce Pr Nd Sm Eu Gd Tb Dy Ho Y Er Tm Yb Lu
75.9 77.3 78.9 79.3 78.9 78.4 77.6 78.4 76.7 75.3 76.3 73.1 69.2 64.3 55.4
Table 5 Chemical analysis Rare earth Impurity
of the mixed REO calcine
Element Analysis (%) Element Analysis (g/t)
product from the kiln testing
La 12.0 Th 2.1
Ce 31.4 U 96.6
Pr 3.87 Si 93.5
Nd 15.4 Al <53
Sm 2.53 Fe 69.9
Eu 0.147 Mg 92
Gd 2.13 Ca 1572
Tb 0.314 Na <300
Dy 2.00 K <83
Ho 0.413 Ti <60
Y 9.8 P 43.6
Er 1.07 Mn 465
Tm 0.156 Zn <200
Yb 0.705 F 290
Lu 0.0887 Ctot <100
TREE 82.0 S <100
LREE 65.2
HREE 16.8
TREO 98.9
8 D. Dreisinger and G. Andrews
Search Minerals are embarking on a $1.9M CDN pilot plant program to continue
the “scaling up of the process” as part of the drive to commercialization. This pilot
plant program will confirm the process parameters in large-scale equipment while
providing product for refinery evaluation.
Engineering and Cost Studies
The engineering and cost studies have proceeded in two steps. First, SNC Lavalin
(Australia) has prepared a concept study focusing on the processing of rare earth
mineralization to a mixed rare earth oxide product [5]. Second, Roscoe Postle
Associates (RPA) have completed a Preliminary Economic Assessment on the
Foxtrot Deposit at a processing rate of 1000 tpd from underground and open pit
resources [1]. The results of the SNC Lavalin study were used as the basis for the
processing plant cost in the PEA produced by RPA. The SNC Lavalin study costs
were updated by RPA to take into account changes in currency exchange rates and
the cost of raw materials (e.g. steel and other metal prices).
SNC Lavalin Engineering and Cost Study [5]
The SNC Lavalin engineering and cost study comprised the following items.
• Testwork Review
• Process Design Criteria
• Preliminary METSIM® Model
• Preliminary Mass Balance
• Block Flowsheet
• Major Equipment List
• Operating Cost Estimate
• Capital Cost Estimate
• Study Report
The project battery limits were defined as:
• Reclaim from the ROM stockpile (pre-crushed to 100% passing 30 mm).
• Acid storage tank inlet at the port.
• Reagents as delivered to site (except sulphuric acid) and product dispatch from
site.
• Boundaries of the residue storage facility.
• Water supply from a client identified year round water source, including an
allowance for pumping and a water supply pipeline.
• Power supply ‘over the fence’ from a utility supplier, including an allowance for
a transmission line and incoming transformers and distributions.
The Economics of the Search Minerals … 9
• Liquid effluent disposal (barren solution) to sea requirements after a long
pipeline to the port.
The following items were excluded from the scope of work:
• Resource definition and mining.
• Testwork and testwork management.
• Engineering development and studies prior to project commitment.
• Project definition and scheduling.
• Study of social and environmental issues.
• Definition of or obtaining project approvals and permits.
• Financial modeling.
• Power delivery outside of the battery limits.
• Water delivery outside of the battery limits.
• Logistics of reagents and product outside of the battery limits.
• Port logistics.
The testwork review highlighted the results presented in this paper as a basis for
design. The SNC Lavalin review concluded that a simple direct acid bake and water
leaching process has been developed for treatment of Foxtrot mineralization that
involves crushing to 6 mesh particle size, application of 100 kg/t of H2SO4 to the
material at 200 °C for 2 h followed by a 24 h water leach to produce a weakly
acidic product leach solution. Favourable material handling characteristics of the
acid/feed mixture and calcine as well as easy filtration characteristics of the water
leach residue have led to the development of a much more operable acid bake
circuit than other “typical” REE acid bake circuits. The review also highlighted
areas where future testing and process development would be most useful including
optimization of crush size for balance between leaching and solids handling,
reduced impurity levels (e.g. U) in the final concentrate, determining solid-liquid
separation design parameters, determining oxidant requirements in impurity
removal and a general reduction in reagent requirements. The current pilot plant
program is designed to address these areas.
The conceptual block flow diagram is shown in Fig. 2.
Feed Preparation
The purpose of feed preparation is to mine and crush the mineralization to a size of
100% passing 3.45 mm, while minimizing the fines generated. This sized feed is
approaching the minimum size possible for a dry crushing circuit. This is achieved
by:
1. Open cut mining with in pit crushing to below 30 mm and delivered to the run
of mine (ROM) stockpile at the processing facility.
2. Further size reduction by high pressure grinding rollers (HPGR, in closed circuit
with a vibrating screen) during day shift will ensure an appropriately sized feed
10 D. Dreisinger and G. Andrews
Fig. 2 Conceptual block flow diagram [5]
for the continuous operation of the acid mixing and acid bake section of the
facility.
3. This area is supported by a small dust collection system for control of dusts,
recognizing that this is the highest risk factor when handling low radiation
mineralization. Dust collected is mixed back with the feed to the acid mixing
process.
Mixing and Acid Baking
The purpose of the mixing stage is to intimately mix the crushed ore with con-
centrated (93%) sulphuric acid at a rate of 100 kg of acid (100% equivalent) for
every tonne of ore. This mixture must then be heated and maintained at 200 °C for
90 min. This section of the plant operates continuously 24 h a day. This is achieved
by:
1. A pug mixer is used to intimately mix the acid with the ore. A recycled filter
cake from the later Secondary Th Removal stage is also added to pug mill to
minimize REE losses.
2. A Holo-Flite® preheater to raise the temperature of the mixture to 200 °C. The
Holo-Flite® heater is an indirect heat exchanger utilising hollow screws and
jacketed walls for heating of bulk solids and pastes. The screws provide
movement of the solids similar to a screw conveyor while also improving the
heat transfer by further mixing of the solids. The action of the Holo-Flite®
system (screw conveyor movement) is expected to mimic the “rabbling” used in
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Condition of repair.
No. 26 has been demolished. Nos. 27 and 28 are in good repair.
The Council’s collection contains:—
[191]Entrance doorcases to Nos. 27 and 28 (measured drawing).
Entrance doorcases to Nos. 27 and 28 (photograph).
[191]Ornamental cast lead cistern, No. 27 (measured drawing).
[191]Ornamental cast lead cistern, No. 26 (measured drawing).
[191]Carved deal stair bracket (measured drawing).
[191]Cast lead rain-water head, No. 26 (with others) (measured
drawing).
XXXVII.—Nos. 55 and 56, GREAT QUEEN
STREET.
Ground landlords.
The United Grand Lodge of Antient Free and Accepted
Masons of England.
General description and date of
structure.
The largest of the three sections into which Aldwych Close was
divided, when roads were formed thereon, was that lying to the south
of Great Queen Street, and east of Wild Street. In 1618[192] Henry
Holford leased to John Ittery the southern portion of this section,
and on 13th August, 1629, Richard Holford sold the remainder to Sir
William Cawley and George Strode in trust for Sir Edward Stradling
and Sir Kenelm Digby.[193] A wall was erected parallel to Great Queen
Street, and distant from it 197 feet, dividing Stradling’s part from
Digby’s. The later history of Stradling’s portion, lying to the south of
the dividing wall, is dealt with later.[194] Here we are concerned with
that in the ownership of Sir Kenelm Digby, forming the site of the
houses and gardens on the south side of Great Queen Street as far as
Aldwych Close extended. The ground in question (including that
purchased by Sir Edward Stradling) is described on 13th August,
1629, as “late in the tenure of Richard Brett and John Parker,”[195]
and a petition of the inhabitants of the district, dated[196] 1st
September, 1629, states that Parker and Brett had “divers times
attempted to build on a little close called Old Witch, which has
always lain open, free to all persons to walk therein, and sweet and
wholesome for the King and his servants to pass towards Theobalds.”
It is further alleged that Parker and Brett had been imprisoned for
these attempts, “but now they have pulled down the bridges and
stiles, and carried great store of bricks thither, and give forth
threatening speeches that they will go forward.” The petitioners
asked that the proposed buildings might be stopped, and expressed
their willingness to take a lease of the close and plant trees.
Parker and Brett seem in this latest instance to have been
merely acting for Sir Kenelm Digby, for the report[197] of the
Commissioners for Buildings, made only nine days later, definitely
mentions the latter as the person desirous of building. The
Commissioners expressed themselves as adverse to Digby’s proposal,
which for a time dropped.
On 27th March, 1630, both Digby and Stradling petitioned for
a licence for each “to build a house with stables and coach houses in
Old Witch Close.” The Attorney-General was instructed to draw the
licence, but although Stradling in due course built his mansion[198],
there is no evidence that Digby ever availed himself of the
permission.
The ground seems to have been used as a garden[199] until
1635. On 13th April in that year Digby sold it to William Newton for
building purposes. No licence to Newton to build can be traced, but
on 7th May, 1636, one was granted to Sir Robert Dalyell,[200] who
probably assigned it to Newton. From that document[201] it appears
that the intention was to build “14 faire dwelling houses or
tenementes to conteyne in front one with another neere 40 (fortie)
feete a peice fitt for the habitacon of able men.” Permission to build
that number of houses “to front only towardes Queene’s Streete” was
granted, as well as “twelve coach howses and stables in some remote
part of the said ground,” all to be built of brick or stone, “according
to the true intent and meaning of our Proclamations in that behalfe
published.”
Signature of William Newton.
Newton seems to have taken care that the houses erected on
that part of Great Queen Street which was on the site of Purse Field
should conform generally to the style of those built in accordance
with the above-mentioned licence on the site of Aldwych Close[202].
The houses as a whole occupied 13 ground plots, having a total
frontage of about 628 feet, and a depth of 200 feet. Their general
character was the same throughout; the main cornices and front
roofs were continuous, but the pilasters were so arranged as to
indicate the separate buildings without the usual expedient of
placing a pilaster partly on one plot and partly on another.[203] On the
middle house was placed a statue of Charles I.’s Queen, Henrietta
Maria. It has already been noticed[204] that Newton a few years later
adorned the central house in Lincoln’s Inn Fields with a crowned
female bust, and there can be no doubt that this was also in honour
of the Queen.
Various statements have been made as to the designer of the
houses on the south side of Great Queen Street. Horace Walpole, in
his Anecdotes of Painting[205] writes as follows: “Vertue says that Mr.
Mills, one of the four surveyors appointed after the fire of London,
built the large houses in Queen Street, Lincoln’s Inn Fields, but this
must be a mistake, as we have seen in the preceding volume that
Gerbier, a contemporary, and rival, ascribed them to Webb.” It is
known[206] that Peter Mills built the original houses on the site of
Nos. 66 to 68, Great Queen Street, but there is no evidence that he
had any hand in the erection of other houses on the south side of the
street.
The reference concerning Gerbier [1591?–1667], to which
Walpole alludes as occurring in his previous volume, seems to be the
following: “He [Gerbier] ridicules the heads of lions, which are
creeping through the pilasters on the houses in Great Queen Street
built by Webb, the scholar of Inigo Jones.” If this ascription could be
found in any of Gerbier’s works it would be very valuable evidence,
but it has not been discovered, and the passage relating to the
pilasters contains no mention of Webb.[207]
Bagford [1650–1716], writing somewhat later, says:[208] “He
[Inigo Jones] built Queen Street, also designed at first for a square,
and as reported at ye charge of ye Jesuits; in ye middle whereof was
left a niche for ye statue of Henrietta Maria, and this was ye first
uniform street and ye houses are stately and magnificent.... These
buildings were ye designes of ye Ld. Arundell, who was ye first that
introduced brick building into England (I mean for private houses).”
That some architect was commissioned by Newton to design
the façade, and possibly the principal internal features, is most
probable; but the above evidence is unfortunately not sufficient to
enable him to be identified.
Hollar’s careful engraving (Plate 3) shows the long straight
roof of the road frontage, but the rear elevations show that the roofs
were varied for individual houses and were treated with gables.
Whoever was the designer of the façade to Great Queen Street, he
was probably employed by Newton as architect for the houses built
on the west side of Lincoln’s Inn Fields three years afterwards. These
show a distinct advance in design, being treated as a single
symmetrical composition, with a central feature composed of three
houses of increased height, the side wings being of equal lengths.[209]
The beautiful drawings by J. W. Archer[210] reproduced on
Plate 16 exemplify the similarity of the two designs to a very marked
degree, the only important difference in detail being that in Great
Queen Street the Corinthian order was employed, in Lincoln’s Inn
Fields the Ionic.
A description of the exterior of the only remaining fragment of
the Great Queen Street houses, Nos. 55 and 56, will suffice for the
whole. The front is constructed mostly of brick, the ground storey
having originally formed a simple base for the Corinthian order of
pilasters. These embrace the height of the first and second stories,
the bases and capitals being of stone, the ornament of the latter
boldly carved, and the volutes and abacus spreading to an unusual
extent. (Plates 18 and 19.)
The pilasters were ornamented, if, as seems probable, it is to
these houses that Gerbier referred when, writing about 25 years after
their erection, he criticised certain “incongruities” perpetrated by
those pretending knowledge in ornaments “by placing between
windows pilasters through whose bodies lions are represented to
creep; as those in Queen Street without any necessity, or ground for
the placing lions so ill.”[211] These lions were probably of stucco, and
affixed to the pilasters in a position similar to that of the ornaments
of the Tudor rose and fleur de lis on the houses in Lincoln’s Inn
Fields, and those at the eastern end of the north side of Great Queen
Street.[212] Walpole,[213] writing in 1763, continued the ridicule of
these offending ornaments, but by 1783 they must have been
removed, for the engraving by Bottomley of the Freemasons’ Tavern
(Plate 22) does not show them, nor can they now be traced on the
brickwork of the pilasters.
Between the first and second floor windows is introduced a
slightly projecting ornamental device in brickwork, of somewhat
Jacobean character, which on the façade of the houses in Lincoln’s
Inn Fields was represented by a band, formerly seen at No. 2,
Portsmouth Street. The same feature is also shown in the Wilton
House picture of Lincoln’s Inn Fields.[214]
Above the capitals the entablature has been much restored,
and its former beauty correspondingly diminished. The architrave
appears to have been of wood, with three fascias (Plate 19), and
crowning this is the bed mould of the cornice, which has large
wooden modillions, shaped and enriched with acanthus leaves.
The modillions support a cyma and fascia with panelled soffit,
the cyma forming the front of a leaden gutter.
Surmounting the cornice was the high pitched roof, shown by
Hollar, with hipped dormer windows, of one and two lights
alternating. Though none of them retain the whole of their original
construction, the two on the right of the illustration may possibly be
in their original form.
The present Nos. 55 and 56 represent one half of what must
have been the largest of the houses.[215] This was the mansion of
which one of the earliest occupiers was the Earl of St. Albans
(Marquess of Clanricarde).
The house may be identified in two ways. (1) The frontages of
the house of the Earl of St. Albans, and of the three houses to the
east, are stated to be 88[216], 44, 44 and 88 feet respectively, and the
last mentioned house is said to be bounded on the east by a gateway,
which, from the description, was obviously Middle Yard. The western
boundary of the four houses in question may thus be shown to
correspond with the western side of New Yard, i.e., the western
boundary of No. 55. (2) On 23rd January and 8th February, 1639–
40, Newton sold certain plots of ground, containing frontages of 41
and 45½ feet, having a depth of 190 feet, and after 120 feet
diminishing in width from 83 to 60 feet. These plots are stated to be
bounded on the east by the dwelling house and garden of the Earl of
St. Albans. From the shape of the property disclosed by the above
figures, and the actual frontages given, there can be no doubt that the
houses afterwards erected thereon occupied the sites of the present
Nos. 51 to 54.[217] The house of the Earl of St. Albans was therefore
No. 55 and upwards.
The house was already in existence in January, 1637–8,[218]
and as the licence for building had only been obtained in May, 1636,
the erection of the house may, with practical certainty, be assigned to
the year 1637.
In the 1638 deed it is described as “all that one new erected
double messuage or tenement with appurtenances, scituate in
Queenes Streete ... contayninge in front towardes Queenes Streete
aforesaid 88 feet ... and sydinge eastwards upon the house in the
tenure of the Lord Leiger Embassador of Spayne, together with a
gardyn plott lyinge on the back side of the said messuage and
adjoyninge thereunto.”
The original mansion therefore occupied the site of the
present Nos. 55 and 56, and adjoining property in New Yard,
together with that of the western block of the present Freemasons’
Buildings.
The first division of the house took place in, or shortly after,
1684. In that year Lord Belasyse purchased the property, and at the
date of his will, five years later, the house had for some time been in
double occupation.
The division had, however, not been carried out in a very
thorough fashion. In 1718 it was stated that “there are severall
roomes, chambers and other apartments ... which interfere or mix
within each other very inconvenient for separate familyes to inhabit
therein severally and apart from each other.” In that year, therefore,
an arrangement[219] was made whereby “the kitchen under a roome
heretofore called ... Mr. Stonor’s dressing-roome,[220] the larder
backwardes next the garden under part of a room ... called Mr.
Stonor’s bedchamber ... which were then both used and enjoyed with
the house in possession of ... Henry Browne ... were to be added to
the inheritance of the house of the said Thos. Stonor in exchange” for
“the cellar under the foreparlour next Queen Street, and the
uppermost room or garrett over the said parlour, the lesser cellar
adjoyning to that last before mentioned cellar and the room
backwards next the garden up two pair of stairs over the back
parlour, and upper with drawing roome,” structurally part of
Browne’s house, but occupied as part of Stonor’s.
Other alterations took place in 1732–3, when the western half
was divided, and probably portions of the present party wall, to the
east of No. 56, date from this and the earlier period.
During the last century many further alterations and partial
rebuildings were carried out. Shortly before 1816, the extensive
grounds in the rear were utilised for buildings, for in a deed[221] of
that year reference is made to “all those stables, coach houses and
workshops and premises erected ... in New Yard ... and which before
the erecting of the said ... stables, coach houses, shops and other
premises, was a garden ground.”
Subsequently the external west wall was rebuilt, and the
south-western premises, extending over the entrance to the yard (see
Plate 17) were erected.
The eastern half of the original mansion seems to have been
demolished between 1840 and 1846, for J. Nash, in a sketch made in
the former year, gives the complete elevation, whereas Archer in
1846 (Plate 16) shows a commonplace building on the site of the
eastern half.
Having regard to the
many alterations which the
premises have undergone, it is
not surprising that very little of
the first building is left. Of the
original walls remaining, that to
the street is the most important.
Several of the chimney breasts,
and parts of the walls to which
they are attached, are also
original work, but it is extremely
doubtful if any of the external
walls at the rear is coeval with
the erection of the house. This
Nos. 55–58, GREAT QUEEN STREET IN
1840.
will account for the fact that
Evelyn’s “long gallery”[222] no
longer exists.
The notable feature of No. 55 internally is the staircase.
Although the treads and risers are modern, the deal balustrading
between the ground and first floors may date from the erection of the
house in 1637, or from its re-occupation by the Digby family after the
Restoration, i.e., before 1664 (see p. 52). The staircase extends from
the ground to the first floor. It is constructed of straight strings,
moulded and carved; the centre moulding has a band of laurel leaves
and berries alternating with oak leaves, acorns and oak apples, while
the upper member is enriched with acanthus. The three newels are
square. The one at the ground floor level rests on the 19th-century
floor, and has a simple capping of mouldings similar to those on the
handrail. The newel at the half landing is of similar design to that
below and receives the strings of both flights. The newel at the first
floor level has a modern capping, but carries the original pendant
below, the enrichment taking the form of the open flower of a
waterlily. The balusters are turned as ornamental pillars, their
capitals being floriated together with the vase-like swellings included
in their bases. Two of the base members are also carved. The
handrail of the lower flight is notched and fitted to the string of the
upper, the mouldings continue along the string downwards to the
newel, and a triangular panel fills the spandril space beneath instead
of diminishing balusters.
The simple character of the elliptical archway at the end of the
passage leading from the street to the staircase may be noted.
On the second floor of No. 56, is a deal balustrade (Plate 21),
which doubtless formed part of the original staircase landing, but has
now been adapted to protect an opening in the floor. The detail is
very similar to that of the staircase formerly at No. 52, Lincoln’s Inn
Fields,[223] which was erected shortly after this date.
The panelling of the room at the end of the ground floor
passage is apparently contemporary with the erection of the house.
The present front room on the second floor was at first two
separate apartments. Near the end of the 17th or early in the 18th
century, a wide opening was formed in the partition, the original
door and doorway, and part of the surrounding wall being, however,
left. Probably at the same time, the little lobby and powder closet
were formed. The latter has a small opening in its southern wall.
The small staircase in front of the opening leading to the attics
appears to have been erected about 1732–3, as also the portion of the
staircases leading from the second to the first floors, and a short
length of balustrading (Plate 21) at the first floor level.
The front room on the ground floor was dismantled early in
the 19th century and nothing of interest is left.
Condition of repair.
The premises are in good repair.
Biographical Notes.
The indenture[224] relating to the sale of the freehold by Newton on
26th October, 1639, to Sir Henry Compton, Sir Lewis Dive and Thos.
Brewer, refers to the house as “late in the tenure of the Rt. Hon. Thomas,
Lord Arundell, Baron of Warder, now deceased.”
Thomas Arundell, first Baron Arundell of Wardour, was born in
1560. He greatly distinguished himself in the wars against the Turks in
Hungary, and for his valour, was, in 1590, created Count of the Holy Roman
Empire. He was raised to the English peerage by James I. in 1605, and died
in 1639.
In the sale mentioned above, Compton, Dive and Brewer were acting
on behalf of the Marquess of Clanricarde, and the latter is referred to as
actually in occupation of the house in January, 1639–40.[225]
Ulick De Burgh, Marquess of Clanricarde, Earl of St. Albans,
was born “in Clanricarde House, Great Queen Street, Lincoln’s Inn
Fields, London”[226] in 1604. The exact position of this house is not
known, but it must have been on the north side of the street, as the
south was not built on for many years afterwards. From his father
he inherited, together with the viscounty of Galway, vast estates and
an enormous influence in the south of Ireland. He sat in the Short
De Burgh. Parliament, and accompanied the King in his expedition against the
Scots in 1640. His occupation of the house on the south side was
brief, for in September, 1641, he disposed of the property to the Earl
of Bristol.[227] In the summer of the latter year[228] he had taken up his
residence in Ireland. During the troublous times that followed the outbreak
of the Irish rebellion in that year, Clanricarde played a prominent part.
Although many of his relatives joined the Irish Confederation, he alone
among the Irish Roman Catholic nobility remained loyal to the king, kept
Galway, of which he was governor, neutral, and made “his houses and towns
a refuge, nay even a hospital, for the distressed English.”[229] When the
Viceroy, Ormonde, quitted Ireland in 1650, Clanricarde was appointed his
deputy, but his efforts against the parliamentary forces were rendered
fruitless by the distrust with which he was regarded by many of the Irish
royalists. In 1652 he received Charles’s permission to make the best terms
possible with the parliamentarians, and articles were accordingly
concluded, by virtue of which he was able in the same year to withdraw
from Ireland. Though expressly excepted by statute from pardon for life and
estate, he was enabled, by permits renewed from time to time, to retire for
the remainder of his life to his seat at Summerhill, Kent, where he died in
1657. Though he was the object of bitter denunciation by the native Irish
faction, he has earned the commendation of Hallam as being “perhaps the
most unsullied character in the annals of Ireland.”[230]
John Digby, first Earl of Bristol, who followed Clanricarde in the
occupation of the house in Great Queen Street, was the son of Sir George
Digby, of Coleshill, Warwickshire, and was born in 1580. He gained the
favour of James I. and was knighted in 1607. Four years later he was sent as
ambassador to Madrid, and from that time until 1624 was frequently
employed on diplomatic missions of first-rate importance. In 1618 he was
raised to the peerage, and in 1622 was created Earl of Bristol. In the
following year, while engaged at Madrid in connection with a project for the
marriage of the Infanta Maria and Prince Charles, he managed to offend
bitterly both the latter and Buckingham, who had come to Spain on a
surprise visit. In 1624 he came home and found himself in disgrace. For the
first few years of Charles’s reign, he continued to be an object of the king’s
resentment and spent several months in the Tower. After 1628 he took no
part in politics until the war against the Scots in 1639. He was the leader of
the Great Council held at York in 1640. Though he came forward in the
Long Parliament as a reformer of the government, yet when it became
necessary to take up a definite side in the civil strife he threw in his lot with
the king. He was with him at Oxford for some time after the battle of
Edgehill, removing thence to Sherborne, and subsequently, in 1644, to
Exeter. On the capitulation of that city to Fairfax in 1646, he was given a
pass to go beyond the seas. He died in Paris in 1653, and by his will[231]
bequeathed to his second son, John, his house in Queen Street. This house
had formed his residence at the most from September, 1641, to some time
before the battle of Edgehill in October, 1642. By the parliament he was
regarded with peculiar abhorrence, due partly, no doubt, to the acts of his
uncontrollable son, and in August, 1644, an ordinance was passed providing
inter alia that “the house of John, Earl of Bristol ... in Queen Street ... with
the gardens, stables, edifices and buildings thereunto belonging, with their
appurtenances, heretofore the mansion house of the said Earl of Bristoll,”
should be granted to Lady Brooke for her life, and after her decease to her
youngest son, Fulke Greville.
There is, however, no evidence that Lady Brooke[232]
ever lived there, and the next record that has been found as
to the occupation of Bristol House is contained in a deed[233]
of 1654, by which Antony Wither purchased from the
“Trustees for the Sale of Estates forfeited for Treason, all that
messuage or tenement ... situate in the parish of St. Giles-in-
the-Fields ... in a streete there called Queene Streete ... late in Digby.
the tenure or occupation of Thomas, Lord Fayrfax, and now
or late in the tenure ... of Sir William Paston, Knt., ... which
said premises ... are mentioned to have bin late parcell of the possessions of
John, Earle of Bristoll ... whose estate hath bin and is thereby declared and
adjudged to be justly forfeited by him for his treason against the Parliament
and people of England.”
Thomas Fairfax, third Baron Fairfax, was the son of Ferdinando,
second Lord Fairfax, and was born at Denton, in Yorkshire, on 17th
January, 1612. He served in the Low Countries under Sir Horace Vere,
whose daughter he afterwards married. He held a command during the first
Scotch war, and was knighted by the king in January, 1640. On the outbreak
of the Civil War he took up arms on behalf of the Parliament and gained
great distinction. In 1645, consequent upon the compulsory retirement of
officers who were members of either house (his father among others), he
was appointed to the chief command of the parliamentary forces. He arrived
in London on 18th February, accompanied by his uncle, Sir William
Constable,[234] and two or three officers, and took up his quarters at “the
house in Queen Street, Lincoln’s Inn, which had been hired for the new
general during his stay in London.”[235] During his absence in the field his
house in Queen Street was occupied by his father, with whom he kept up a
constant correspondence.[236] In June, 1645, Fairfax amply vindicated the
Parliament’s choice by his annihilation of the royal army at Naseby, and on
12th November, 1646, having brought the first portion of the Civil War to a
successful close, he returned to London to receive the thanks of Parliament
and of the City. Accompanied by dense crowds, “he was conducted to his
house in Queen Street, Lincoln’s Inn, amidst deafening cheers and the
ringing of bells; and was received at the door by his wife and his father, the
old lord, with his new bride.”[237] Two days later both houses of Parliament
paid a congratulatory visit to Fairfax in his house in Queen Street. His
father died in March, 1648. In the second portion of the Civil War, which
began later on in the same year, Fairfax was at first principally occupied
with the siege of Colchester, and his execution of Lucas and Lisle on the
surrender of that town in July, 1648, though bitterly denounced, seems not
to have been without justification. In the events which led up to the death of
Charles in 1649 he seems to have been an unwilling instrument of the army.
In 1650 he resigned the commandership-in-chief, to which he had again
been elected, rather than take part in the attack on Scotland, and during the
whole of the remaining period, until the death of Cromwell, he lived in
retirement at Nun Appleton, in Yorkshire. He took a leading part in
bringing about the Restoration, but after that was successfully accomplished
he again retired to Nun Appleton, where he spent the rest of his days in
religious exercises. He died on 16th October, 1665.
As the house in Great Queen Street had been provided by
Parliament for use as his official residence, his occupation of it
probably ceased on his resignation in June, 1650.
Of Sir William Paston’s residence we have but little record.
There is, however, a letter from him, headed “Queen Street,” and
presumably written from this house, dated 30th January, 1650–51.
[238] The deed mentioned above leaves it uncertain whether he was,
Fairfax. in June, 1654, still in occupation of the house.[239] He had been high
sheriff of Norfolk in 1636, was created a baronet in June, 1642, and died in
February, 1663. He was the father of the first Earl of Yarmouth.
At the Restoration the house again came into the hands of the Digby
family. In a deed of 6th January, 1663–4,[240] it is referred to as “now in the
tenure of George, Earl of Bristol, or his assignes,” and in the Hearth Tax
Rolls for 1665 and 1666, the Earl of Bristol is shown as in occupation of the
house. This was George, the second Earl, who was born at Madrid, in
October, 1612. When only twelve years old he appeared at the bar of the
House of Commons on behalf of his father, who had been committed to the
Tower, and his graceful person, gallant bearing, and eloquent speech made
a great impression. He enjoyed a distinguished career at Oxford, and
afterwards displayed some literary ability in the Letters between the Lord
George Digby and Sir Kenelm Digby, Knt., concerning Religion, written in
1638–9. He entered Parliament in 1640, where, although at first hostile to
the Court, he afterwards became one of its strongest adherents. He was
responsible for the proposal for the prosecution of the five members, and
even suggested that they should be followed into the City and taken by
force. In February, 1642, he was impeached of high treason and fled to
Holland, but soon returned. In September, 1643, he was appointed one of
the secretaries of state, and as one of the king’s chief advisers did
incalculable harm to the royal cause. In October, 1645, he was made
lieutenant-general of the royal forces north of the Trent, and was defeated at
Sherburn. The next few years he spent chiefly in Ireland, whence, on its
surrender to the Parliament, he escaped to the Continent, gaining and
losing favour in France, joining Prince Charles at Bruges and accompanying
him to Spain. In 1657 he became a Roman Catholic. On the Restoration he
returned to England. Being debarred from office on account of his religion,
his energy found vent in an unreasoning hostility to Clarendon, in which he
went so far that he provoked the keenest resentment on the part of the king,
and had to remain in concealment for nearly two years. He died at Beaufort
House, Chelsea,[241] in March, 1677, leaving behind him a reputation for
brilliant but misdirected ability.
His residence in Great Queen Street seems to have terminated before
1671,[242] for under date of 26th May in that year, Evelyn records: “The Earl
of Bristol’s house in Queen Street was taken for the Commissioners of Trade
and Plantations, and furnished with rich hangings of the King’s. It consisted
of seven rooms on a floor, with a long gallery, gardens, etc.... We then took
our places at the Board in the Council Chamber, a very large roome
furnished with atlasses, maps, charts, globes, etc.”[243] Evelyn had only
recently (see Diary for 28th February) been appointed on the Council of
Foreign Plantations,[244] and the above entry refers to the first occasion on
which he attended as a member, and gives no clue as to the date on which
the house had been taken for the use of either of the Commissions.[245] On
12th February, 1671–2, Evelyn records the determination of the Council to
meet in future at Whitehall.[246]
The Hearth Tax Rolls for 1673 and 1675 show the Earl of Devonshire
as then in occupation of the house. He would, indeed, seem to have
acquired most of the interests in the premises by or before July, 1667,[247]
and it is quite possible that his residence extended on both sides of the short
occupation by the Boards of Trade and Plantations.
William Cavendish, third Earl of Devonshire, was born in
1617. He derived his education in part from his father’s old tutor,
Thomas Hobbes, the philosopher, in whose company he travelled
abroad from 1634 to 1637. At the beginning of the Civil War he
embraced the royalist cause, and on being impeached by
Parliament, refused to submit, and left the country. In 1645 he
returned to England, and on payment of a large fine received a
Cavendish. pardon for his former delinquency. During the remainder of the
Commonwealth period he lived in retirement at Latimers, in
Buckinghamshire, and even after the Restoration he resided mainly in the
country. He was one of the original fellows of the Royal Society, and in 1669
was appointed a commissioner of trade.[248] He died in 1684 at
Roehampton.
In June, 1674, the Earl of Devonshire had sold the remainder of the
original 99 years’ lease of the house to the Earl of Sunderland,[249] who in
the Jury Presentment Roll for 1683 is shown in occupation of the house. He
parted with his interests in the property in April, 1684, and his occupation
may therefore with reasonable certainty be assigned to the period 1674–84.
[250]
Robert Spencer, second Earl of Sunderland, the only
son of Henry Spencer, the first Earl, and “Sacharissa,” was
born in 1640, and succeeded to the earldom only three years
later. In 1665 he married Lady Anne Digby, younger
daughter of the second Earl of Bristol. In preparation for his
future political career, he now began paying court to the royal
favourites, and in 1671 invited Mdlle. de Keroualle
Spencer.
(afterwards Duchess of Portsmouth) “to his town house in
Queen Street, and lost enormous sums to her at basset.”[251]
This can hardly have been Bristol House, for the facts seem quite
inconsistent with Sunderland’s residence there so early as 1671. More
probably it was his mother’s house at the eastern end of Great Queen Street.
From 1671 to 1678 he was employed on several diplomatic errands abroad.
In 1679 he became secretary of state for the northern department, but in
1681 incurred the king’s displeasure, and consequently lost both his
secretaryship and his seat on the Privy Council. Afterwards he regained his
place by the influence of the Duchess of Portsmouth, and on the accession
of James II. in 1685 he speedily ingratiated himself with the new king, who
made him Lord President of the Council. While assiduously cultivating
James’s favour, he was also receiving a substantial secret pension from
Louis XIV. for the promotion of French interests, and through his wife’s
lover, Henry Sidney, was furnishing William of Orange with particulars of
the most secret transactions of the English Court. By degrees his position
became more and more difficult and, although in 1687 he had embraced the
Roman Catholic faith, not all his duplicity could prevent the growing
dissatisfaction with which James regarded what he considered as his
lukewarm service, and in 1688 he was dismissed and fled to Holland.
Though excepted from the Act of Indemnity, he was in 1691 permitted to
return to England. He declared himself again a Protestant, and his advice
soon became indispensable to William. His influence gradually grew until in
1697 all the hatred and jealousy with which he was regarded came to a head,
and he resigned in a panic. The rest of his life he passed in seclusion at
Althorp, and he died in 1702. “With the possible exception of
Northumberland in Edward VI.’s reign, it is doubtful whether English
history has to show a more crafty and unprincipled intriguer.”[252]
In the course of 1684 all interests in the house in Great Queen Street
were acquired[253] by John, Lord Belasyse,[254] and the premises were now
divided into two, afterwards respectively Nos. 55–56, and Nos. 57–58. The
later history of the latter will come naturally under the head of the
Freemasons’ Hall, a part of which now occupies the site.
As regards Nos. 55–56, we learn that prior to 1689[255] this portion of
the original mansion had been occupied by the Duke of Norfolk.
Henry Howard, seventh Duke of Norfolk, was born in January, 1655,
and succeeded to the title in January, 1684. He was noted for his staunch
Protestantism. He joined in the invitation to the Prince of Orange, and on
the latter’s landing brought over the eastern counties to his interest. He died
at Norfolk House, St. James’s Square, in 1701. His residence at Nos. 55–56,
Great Queen Street must have fallen in the period 1684–1689.
Subsequently the house was occupied by Thomas Stonor, who had
married the Hon. Isabella Belasyse, to whom her father, Lord Belasyse, had
bequeathed this portion of the original house. Stonor is shown in
occupation in 1698, 1700 and 1703. In 1718 the house was sold[256] to Sir
Godfrey Kneller, then already in occupation of the premises.
Sir Godfrey Kneller (originally Gottfried Kniller) was born at Lübeck
in 1646, son of a portrait painter. He was at first intended for the military
profession, but his love for painting proved so strong that his father sent
him to Amsterdam to study under Ferdinand Bol. In 1672 he went to Italy,
and soon acquired a considerable reputation. Afterwards he visited
Hamburg, and in 1675 came to England, where his work attracted the notice
of the Duke of Monmouth, by whose influence he was in 1678 introduced to
Charles II. He at once leaped into popularity, and after the death of Sir Peter
Lely in 1680 reigned supreme in the domain of portrait painting. He
acquired great wealth, and, though he lost heavily in the South Sea Bubble,
he left a large fortune. His residence at Nos. 55–56, Great Queen Street
seems to have commenced about 1703,[257] and here he lived until his death
in 1723. By his will[258] he left to his wife, amongst other property, “all that
my messuage or house, outhouses, stableyards and garden thereunto
belonging in Great Queen Street ... in which I now dwell,” as well as the next
door house (Nos. 57–58), which he had also purchased. He also mentions
the “six pictures of mine and my wife’s relations painted by myself, and now
in my great dining room in my said dwelling house in Great Queen Street,
and also the three pictures put up for ornament over the doors in the said
room.”
The well-known interchange of wit between Kneller and Dr. Radcliffe
is by several authors[259] said to have taken place in Great Queen Street.
Radcliffe, it appears, was Kneller’s next door neighbour, and there being
great intimacy between them, Kneller allowed the former to have a door
into his garden where he had a fine collection of flowers. On Radcliffe’s
servants picking the flowers, Kneller sent word to the doctor that he would
shut up the door. The latter replied that he might do anything with it but
paint it; whereupon Kneller rejoined that he could take anything from the
doctor but his physic. There is, however, no evidence that Radcliffe ever
lived in Great Queen Street. He settled in Bow Street, Covent Garden in
1684[260]; he was still in Covent Garden in 1706 according to the Catalogue
of the College of Physicians; and the issues of the Catalogue for 1707
onwards show him at Southampton Square. He died in 1714. Wheatley and
Cunningham[261] appear to be right in assigning the incident to the time
when Kneller was living in the Piazza, Covent Garden.
No records concerning the occupation of the house are available
between 1723 and 1730. It would seem, however, that prior to the latter
year, the Earl of Bellamont had been resident there,[262] for the entry in that
year consists of the name “Lord Bellment,” erased, and followed by the
name of Robert Holdmay. In 1732 the house is shown as empty, and on its
re-occupation in the following year it was further divided, as at present, into
the two houses Nos. 55 and 56. The names of the residents, as given on the
ratebooks, from that time until 1800 are as follows:—