CHEMICALS

De-calcification of Beet Sugar

by Tulsion® Resins

ENERGY | ENVIRONMENT | CHEMICALS

 Welcome to Thermax - an engineering company providing sustainable solutions in energy
Why Tulsion® Ion Exchange Resins?
and environment. The company’s vision for the future is firmly anchored in the belief that to
stay competitive, companies need to adopt sustainable development practices.
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The systems, products and services developed by Thermax help industry achieve better Effective Value
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Water treatment is traditionally one of the largest Our resin manufacturing plant at Dahej, Gujarat,
Even as we convert costs to profits, we help to protect the environment in our own ways. A
applications in the field of ion exchange resins; India is a fully automated plant with state-of-the-
win-win for industry and the society at large. art DCS system and latest digital technologies.
however, it has now evolved to various speciality
Thermax’s business portfolio includes products for heating, cooling, water and waste applications. Hence, we believe in developing and We use clean fuel and modern air scrubbing
management, and specialty chemicals. The company also designs, builds and commissions offering customised solutions to our customers, units that are environment friendly. Every batch
which are efficient, economical and provide value of Tulsion® ion exchange resins is manufactured
large boilers for steam and power generation, turnkey power plants, industrial and municipal
for money. under carefully controlled process parameters
wastewater treatment plants, waste heat recovery systems and air pollution control projects. To date, a number of customers seeking and follows a rigorous quality assurance protocol.
solutions for industrial, municipal, domestic and We have already commenced the Phase–II of
wastewater related problems have benefited our Dahej facility to cater to the growing global
from Thermax products and services. market demand.
Thermax has two other manufacturing facilities at

Thermax Chemicals is Asia’s leading manufacturer of Paudh, Maharashtra, India and Jhagadia, Gujarat,
India for ion exchange resins and performance

Tulsion® ion exchange resins. Product Customisation chemicals respectively.

Our business is about providing ‘effective customer solutions’ through innovation and development, service and co- Our research and development team consists
of highly experienced professionals in the field
operation, reliability, commitment, and customer-centricity. Our dynamic teams focus their energy and resources to
offer the very best solutions for customers’ needs.
of ion exchange resins and speciality polymers, Value Added Services
who can understand the depth of customer
requirements and provide customised solutions
in complete accordance with customer At Thermax, we offer free-of-cost plant audits,
expectations. design proposals, post sales technical support,

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and a very efficient and experienced research
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and development team that understands
Years of customer requirements to the last detail.
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Our technical support team ensures quick

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them to our product management team, who can
Expertise understand their problems, troubleshoot and

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provide optimal solutions.

Industries
Served
Thermax Chemicals is committed to complying with stringent global quality standards and respects
100+
Projects
the environment. Ion exchange business unit is ISO 9001: 2015, ISO 14001: 2015 and ISO 45001: 2018
certified. Many of the Tulsion® resins are also certified for Halal, Kosher and REACH.
Commissioned
Globally
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Years of
Cumulative
Experience

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 Overview carried out to lower the hardness to < 25 mg/100 DS. (New Regeneration System). The gryllus process
Several juice softening processes have been adapted though is most common but do not produce the desired
Reducing hardness from beet sugar following the juice minimize the load on ion exchange softening equipment. by sugar factories such as gryllus process and NRS quality of juice and molasses.
purification process is one of the essential operation Thin juice ion exchange softening is a well established
in the beet sugar processing industry. To optimize the proven process and offer benefits at various stages of
alkalinity in primary carbonation, pH adjustment is sugar processing such as evaporation or vacuum pan SO3-Na+ + CaCl2 SO3-Ca1/2+ + 2 NaCl
performed to reduce or optimize the soda ash which drying due to increased heat transfer, reduction in color
is being added before the second carbonation. This formation, lower temperature exposer, and decrease in Na+ - Sodium ion for exchange Ca - Cationic impurity in juice Cl - Exchangeable chlorides
reduces the hardness in thin sugar juice and also turbidity, etc.

Typical quality of soft beet sugar juice after strong acid cation resin:
Sugar Calcium Brix Polarization
Beet Sugar De-calcification by Tulsion® Resins Decalcified beet Sugar < 25 ppm 16 % 9.5

Ion exchange in general is insoluble solid materials is used; which is the most suitable technique to remove The values depends on inlet feed quality. Brix, polarization and colour remains same as inlet.
that carry exchangeable cations or anions. Thus, any the said impurities. This resin is a Strong Acid Cation
typical ion exchange consists of a polymer matrix and a (SAC) resin in Na+ form, which is generally supplied in
functional group that contains exchangeable ions. gel type. Typical Refining Process
To increase brix and form sugar crystals, the raw
beet sugar juice has to go through evaporation and Upon arrival at the processing plant, the beets are tested impurities are removed using the carbonation process.
crystallization. This raw beet sugar juice contains for quality and sucrose content. Then, it is thoroughly During carbonation, the juice contains a high amount
different amount of undesirable impurities which washed to remove soil and other impurities. The clean of calcium, which is treated using Tulsion® Resin. This
is necessary to remove before forwarding it to beets are forwarded to beet slicers. In the beet slicing process is also called juice softening. After this step,
evaporation and later for crystallization. Many such process, beets are sliced into thin chips to increase the the ‘thin juice’ is concentrated using Multiple Effect
impurities are removed in the initial step of precipitation surface area of the beets so that sugar can be easily Evaporators (MEE) and put through another filtration
and filtration where lime is added. After this step, the extracted. At this stage, pressing is executed to extract process. This filtered juice is taken for the last stage
thin juice only contains a variable concentration of the remaining amount of sugar. The sugar syrup, or ‘raw treatment where it is crystallized, dried, and packed for
hardness (depending on different regions from where juice’ is moved on to the purification process, where domestic or industrial use.
beet is sourced) which has to be removed in order to
avoid scaling in the evaporator. Beet Reception Washing Beet Slicer Extraction Milling
To remove this Ca2+ in exchange with Na+, Tulsion® resin

Lime Tank

Primary Carbonation Settling Tank

Hard Juice Softening process

Secondary Carbonation
Objective of any beet sugar factory is to maximise However, with advanced MDC process (molasses
the sugar recovery from molasses by separating the desugaring by chromatography) which make use of ion
non-sugar content from sugar. The sugar separation exchange resins for chromatographic separation as
is gradual and accomplished in several steps of sugar downstream process of conventional sugar separation,
Evaporator Filtration Vacuum Pan Crystallizer
processing. At each step of process, the sugar content the sugar recoveries are >90%. MDC is mostly
Tulsion®
is improvised and expressed as purity as % of dry preferred by many beet sugar manufacturers because Resin
substance in sugar syrup. By conventional technology, of its efficiency. It uses soft molasses as feed which can Decalcification
the maximum sugar recovery is possible up to 80% be obtained only if the thin juice softening process is
Packaging Dryer Centrifuge

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 Regeneration Process Typical Characteristics of Tulsion® Resins
Ion exchange with very few exceptions is a reversible removed from the resin beads. This low temperature Tulsion® T-4213 MP Na is a strongly acidic, macroporous • The product is designed to have a large pore
process. Due to this reversibility, it is possible to will allow removed calcium to form a soluble complex and polymer-based resin with a sulphonic acid structure, with high capacity, facilitating the kinetics
regenerate the exhausted resin to its original form. of calcium saccharate. The caustic juice containing functional group. It exhibits the following properties: of adsorption and desorption, which enables this
Same can be applied for the process of beet sugar calcium saccharate produced is recycled to the lime • Excellent physical and chemical characteristics & catalyst to be used in polar and non-polar media.
decalcification. When resin beads are completely milk preparation, or to the 1 /2 carbonation, where the
st nd
supplied in sodium form.
loaded with the calcium ions, they will be regenerated saccharate complex is split, calcium gets precipitated
using soft thin juice and NaOH. For regeneration, thin as CaCO3 and sucrose goes back to the juice. Characteristics Tulsion® T-4213 MP Na
juice is cooled down to 40 C so that the calcium is
O
Screen size USS (wet) 16 - 40
Particle size 0.4 to 1.2 mm
After NaOH injection, there are other operations involved in regeneration. These are briefly discussed below:
Total exchange capacity 1.80 meq/ml (min)
Moisture content 50 ± 3%
Sweeten Off Backwash Settling Down of Resin Bed Regeneration Rinse
Effective size 0.45 - 0.55
Swelling (Max) Na+ -> H+ :10%

1.) Sweeten off: This is the step to displace syrup beads which are classified after backwash again Backwash settled density 670 to 720 g/l
from the bed to make it ready for regeneration. It get compacted. Temperature stability 120OC
is continued until the brix reaches some low level. 4.) Regeneration: NaOH (5%) along with thin juice pH range 0 to 14
This facilitates easy and proper backwash. is injected from the top, replacing calcium ions
2.) Backwash: Water is injected from the bottom in with sodium ions. Approximately 40% of the
the upward direction to expand the bed to about NaOH quantity used for regeneration is recycled
60 to 80%. Thin beet syrup is used for backwash. back to the carbonation stage which is a huge Typical Operating Conditions for Tulsion® Resins
It can be carried out for 30 to 60 minutes. The main improvement in terms of regenerant cost savings.
purpose of backwash is loosening & reclassifying 5.) Rinse: This is the last step of regeneration, wherein
Parameters Unit Values
the bed. It also helps in removing dirt and filtered excess regenerant is washed from the bed, and
matter. during fast rinse, regenerant which is trapped Resin bed depth (minimum) mm 1000
3.) Settling Down of Resin Bed: After backwash, the in resin beads is also removed. Now, the resin
Operating temperature (Max) C
O
120
bed is allowed to settle down. In this step, the resin Column is ready for another cycle of operation.
Service flow rate BV/hr 2 to 5

Regenerant NaOH + Soft juice

Recycling of Regenerant Regeneration level g/l 80 -100

To be more environmentally friendly, an innovative regenerant is a mixture of decalcified thin juice (cooled) Regenerant concentration % 4-5% NaOH
regeneration process (NRS process) has been and NaOH. The spent regenerant and backwash water
Regeneration time minutes 30-40
developed on the fact that in alkaline conditions, are fully recycled in the process without waste disposal,
the calcium saccharate is soluble in water. So, the the rinse is using hot decalcified juice. Regeneration temperature C
O
<40

Slow rinse With soft juice

Introduction of NRS Slow rinse BV 2

Originally the resins were regenerated with a brine as the NRS process. This New Regeneration System Fast rinse BV 5 (max)
solution. Due to the waste handling cost, the industry (N.R.S.) has been installed worldwide in more than 100
has developed environment friendly alternatives such beet sugar factories.

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 Case Study Applications of Beet Sugar
Case: resin which was employed to remove calcium & other
One of the prestigious beet sugar manufacturers alkaline earth metals from the juice.
in Europe approached Thermax to look upon their
process of beet sugar, and provide a solution for their Result:
ongoing operational problems. Thermax resin technical Tulsion®T-4213 MP Na FG was found suitable for the
team audited customer’s plant and found out that process and helped in the removal of the significant
during the carbonation process in sugar refining, the amount of calcium leading to many advantages like
juice contained a higher amount of calcium which was higher output, reduced maintenance cost and lower
creating problems like turbidity, loss of sugar, a larger water consumption. Customer was delighted with the
mass of molasses, and scale formation in evaporators. improvement in their plant operations and with the
added benefits of using Tulsion ®️resin; partnered with Beverages Betaine
Solution: Thermax for many years and continues to do so.
Thermax team proposed Tulsion®T-4213 MP Na FG

Benefits of Hard Juice Softening Confectionary Bio-fuel

products production
• Reduces the scale forming in evaportors and juice • Energy saving on cleaning cost of evaporators
heaters • Enables the use of energy efficient downstrean
• Provides effcient cystalisation and sugar recovery equipment like plate evaporators and the process
• Reduces or eliminates the use of antiscalent like molasses desugering by chromatographic Advantages
during the evaporation process
The main advantage of ion exchange is increased extraction due to the elimination of impurities and by the same
token, decreased production of molasses. Since, the price of sugar as sacked white sugar is greater than that in the
form of molasses, this is the main economic justification for the process. Other advantages are lesser scaling of heat
Do’s and Don’t’s transfer surfaces in evaporators, heaters, and pans due to a substantial decrease in mineral content in the juices.

S.No Parameter Do’s Don’ts Advantages Offered Over Gel-Type Cation Resins

1 Temperature 1200C Should not be >1200C Low residual hardness < 25 mg /100 g DS
2 Regenerant concentration 4-5% NaOH Not to <4% High volume of treated thin juice per softening cycle Depending on inlet load
3 Regeneration temperature <40 C
O
Should not be >40 C O
Low chemical consumption and effluent generation < 10 BV per cycle effluent generation
4 Backwash After every cycle backwash for 60 minutes
(minimum) Low resin fouling and therefore continuous efficient Continuous operation for > 300 cycles of
Backwash water temp <500C operation regeneration

5 Regenerant hardness Should be <0.01% Low rinse volume and therefore low juice dilution < 6 BV
6 Influent suspended solids Nil Better fuel economy >95 % hardness removal
7 Regenerant recycle In case the recycled regenerant is being used
for regular regeneration, it is recommended
to use fresh regenerant after every 30-50
cycles.

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 Glossary of Beet Sugar Processing Affination
Process of mixing the raw sugar or low purity massecuite
Raffinate (CMS)
Raffinate ( concentrated molasses solid) molasses with
with high purity sugar syrup to increase the purity of the high mineral and low amount of sucrose
mother liquor
Sediment in Sugar Diffusion Juice
Water insoluble and suspended substances particularly Product of the diffusion station CSD
not visible to naked eyes PAC Crustal size distribution
Powdered activation carbon
Cossets
Ash Content Product of the slicing station CV Value
Water soluble salts of inorganic and organic compounds Recovery Coefficient of variation in sugar crystal characterises the
% of the refined sugar produced per unit of raw sugar uniformity of the crystal size.
Polarimeter process on mass base
Conductivity Ash Instrument that measures the optically active substances
Ash determined by conductivity like sugar Floc
Mother Liquor Cloudy and turbid precipitates
Sucrose crystal covered with low purity sugar syrup
Moisture Content of Sugar Refractometer
Moisture content of sugar usually maintained @< 0.03 % Measures the dry substance(DS) content in a solution Speecks
Extract Processing Material in sugar that can be seen without microscope
Products of MDC process, processed in to GR like caramelised sugar, hardness and rust particles
GR Sugar BOD (Granulated refined) sugar
Granulated refined sugar -a product of centrifuging white Amount of oxygen required by organisms to consume
massecuite dissolved organic matter Saponin
Continuous SMB A colloidal material that produces flocs on beverages
Continuous simulated moving bed chromatographic comes from beet scene carried to sugar
RDS of Sugar (Brix) COD process in which the resin remains fixed and the and
Refractometer dry solid content or refractometric dry Amount of oxygen necessary for chemical oxidising input and output moves around the resin
substances which is the dry substance measured by the agent to oxidise all the reduced species required by Liquid Invert Sugar
refractometer, which is also called as brix applicable for organisms to consume dissolved organic matter Solution of sugar and invert sugar in water
pure sugar solution as the RI Sequential SMB
Sequential simulated moving bed chromatographic
TOC MA
process in which input and output operates sequentially
Massecuites Amount of organic carbon in the given amount of waste moves around the resin Mean aperture- average crystal size of the sugar
Sugar crystal surrounded by syrup water
HFCS Seeding
Standard Liquor VOC Process of adding of the fine particle that serve as base
High fructose corn syrup
Product of melting high raw sugar and low raw sugar in Volatile organic compound's - compounds of carbon for crystal growth in super saturated liquor
thick juice to produce feed for the first crystallisation and hydrogen that often contain oxygen, sulfer, nitorgen,
fluorine and chlorine Hard Molasses
Second Carbonation
Molasses having hardness > 3 meq
High Green High Wash Syrup Nox Process in which the carbonation gas is added to the
Mother liquor from centrifuging the white A massecuites filtered first carb juice to adjust the ph of 9-9.2 and
Oxides of nitrogen ( NO and NO2) Molasses alkalinity of 0.02-0.03% as CaO )
Runoff syrup from final stage of crystallisation
Low Green Syrup PCC
Mother liquor from centrifuging high raw B massecuites First Carbonation
Precipitated calcium carbonate NRS Juice Softening Process in which carbonated gas is added to the heated
New regeneration system that consist of regeneration of limed juice until the pH 10.8 to 11 and alkalinity of 0.08 to
Thick Juice MDC resin bed by NaOH and sugar syrup 0.11 % as CaO is reached
Product of the evaporating station Process of molasses de-sugaring by chromatographic
process Garrulus Juice Softening Pre-liming
Thin Juice Low green syrup with high Na, & K is used to regenerate Which small amount of lime is added to the juice
Product of the purification station Remelt Liquor the resin.
Liquor produced from raw sugars from different sugar of Diffusion Juice
Carbonation Lime Residue crystallisation melted in remelt syrup Soft Juice Product of diffusion station -juice has DS about 15% and
Product of the first carb operation (lime cake) Juice that can be processed to generate soft molasses purity is 85 to 90 %
Remelt Syrup
Hardness ( Lime Scale ) Raw or affined sugar is melted in melter with high purity Thin Juice Diffusion Process
Total water soluble salts of calcium and magnesium water to produce the syrup of 60% DS Product of purification having some hardness and feed Movement of sucrose and noon-sucrose substances
to the evaporators from higher concentrated side (Inside the beet cells) to
Purification lower concentrated side through protoplasm
Alkalinity
Remelt syrup purified to remove insoluble solids,
Alkalinity produced by alkali metal salts like sodium, Betaine
gums, polysachrides, colorants by precipitation
potassium , calcium & magnesium salts methods combine with purification by phosphoric acid One of the nitrogenous compound present in sugar beet
(phosphating) and lime (carbonation ) that ends up in molasses
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