WO1999024623A2 - Procede de purification du jus brut resultant du raffinage du sucre - Google Patents

Procede de purification du jus brut resultant du raffinage du sucre Download PDF

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Publication number
WO1999024623A2
WO1999024623A2 PCT/EP1998/006841 EP9806841W WO9924623A2 WO 1999024623 A2 WO1999024623 A2 WO 1999024623A2 EP 9806841 W EP9806841 W EP 9806841W WO 9924623 A2 WO9924623 A2 WO 9924623A2
Authority
WO
WIPO (PCT)
Prior art keywords
sugar
calcium hydroxide
clay mineral
juice
mixture
Prior art date
Application number
PCT/EP1998/006841
Other languages
German (de)
English (en)
Other versions
WO1999024623A3 (fr
Inventor
Carlos Martinez Reyes
José Antonio Ortiz Niembro
Raùl CHACÓN RODRIGUEZ
Original Assignee
Süd-Chemie AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Süd-Chemie AG filed Critical Süd-Chemie AG
Priority to AU21515/99A priority Critical patent/AU2151599A/en
Publication of WO1999024623A2 publication Critical patent/WO1999024623A2/fr
Publication of WO1999024623A3 publication Critical patent/WO1999024623A3/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B20/00—Purification of sugar juices
    • C13B20/14—Purification of sugar juices using ion-exchange materials
    • C13B20/144—Purification of sugar juices using ion-exchange materials using only cationic ion-exchange material
    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B20/00—Purification of sugar juices
    • C13B20/02—Purification of sugar juices using alkaline earth metal compounds
    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B20/00—Purification of sugar juices
    • C13B20/12—Purification of sugar juices using adsorption agents, e.g. active carbon
    • C13B20/123—Inorganic agents, e.g. active carbon

Definitions

  • the invention relates to a method for cleaning the raw juice obtained during sugar refining.
  • sugar is mainly produced from sugar cane and sugar beet.
  • the physical composition of the raw sugar solutions made from these plants differs only slightly, so that the refining of the sugar solutions made from them is similar.
  • the sugar refining process is divided into the following sub-steps:
  • Raw juice extraction In the case of sugar beet, the fruits are washed, crushed and extracted with small amounts of water at an elevated temperature. The raw juice is then extracted by pressing. In the case of sugar cane usually
  • REPLACEMENT BUTT (RULE 26) the insoluble organic material is freed of its sugar substances by pressing and extraction with hot water.
  • Juice cleaning The raw juice has a more or less gray-black opalescent appearance and is freed of its non-sugar substances by the so-called juice cleaning. Cleaning increases the ratio of sucrose to total dry matter. As the proportion of sucrose in the sugar solution increases, the amount of sugar to be crystallized increases.
  • the yield of sugar is largely determined by the second process stage, juice cleaning.
  • the raw juice obtained from the plants by extraction or by mechanical pressing contains, in addition to the desired sugar (sucrose), other components that have to be removed during sugar refining.
  • These so-called non-sugar substances include both organic compounds, e.g. Invert sugar, raffinos and ketoses, organic acids, proteins, polypeptides, amino acids, enzymes etc., as well as inorganic compounds, e.g. Salts of potassium, sodium, calcium and magnesium, with the anions chloride, phosphate, sulfate and nitrate.
  • the raw juice is acidic due to an excess of anions.
  • the low pH promotes the hydrolysis of sucrose, which is linked to a reduction in the sugar yield.
  • the raw juice is usually mixed with calcium hydroxide (lime milk) added to raise the pH to 10.8 to 11.9 (beet sugar) or 7.0 to 8.5 (cane sugar).
  • colloidal NZ substances are precipitated by breaking the colloids.
  • Anions of inorganic and organic acids are bound by the formation of poorly soluble calcium salts.
  • Organic polymers are also often added to act as flocculants.
  • the excess calcium hydroxide is precipitated by introducing CO2 or SO 2 into the raw juice by forming poorly soluble CaC0 3 or CaS ⁇ 3 .
  • This treatment is called carbonation or sulfitation.
  • the precipitates formed here also serve as crystallization nuclei or adsorption surfaces for other precipitation products.
  • the carbon dioxide or sulfur dioxide required for this stage is produced in affiliated plants by burning CaCÜ 3 (lime burning) or by burning sulfur. The process is to be classified as harmful due to the exhaust gases formed and the release of non-adsorbed gases during sugar juice treatment.
  • the sludge resulting from carbonization or sulfitation must be filtered, washed and dewatered because it binds considerable amounts of sugar solution.
  • the filter cake is usually used as fertilizer lime. In order to use the fertilizer lime without problems, the moisture must be reduced until there is good spreadability.
  • the object of the present invention was to develop an improved process for cleaning the raw juice obtained in sugar refining, which can be operated with little technical effort in existing plants and in which the proportion of calcium hydroxide added can be kept low, so that carbonation or sulfitation reduced or even completely avoided and the yield of crystalline sugar can be increased.
  • the invention thus relates to a process for cleaning the raw juice obtained in the refining of sugar by treating the raw juice with calcium hydroxide; the process is characterized in that the raw juice is treated with a mixture of calcium hydroxide and a clay mineral selected from the smectite and kaolin group, the proportion of calcium hydroxide being less than about 70% by weight, and the clay mineral together with the separates the remaining calcium hydroxide and the poorly soluble calcium salts formed from the purified thin juice.
  • the proportion of calcium hydroxide in the mixture is preferably about 10 to 60% by weight.
  • the clay mineral is preferably first added to the raw juice sets, whereupon the calcium hydroxide is added.
  • the clay mineral can also be added to the raw juice simultaneously with or after the addition of calcium hydroxide or as a clay mineral / calcium hydroxide mixture.
  • the smectic or kaolin clay minerals have the property of being colloid-breaking, adsorptive and ion-exchanging due to their ion exchange ability and their large surface area. It is believed, without being limited to a theory, that these clay minerals break the colloids present and at the same time act as adsorbents for the compounds released in the process. They therefore fulfill the function of the calcium carbonate or calcium sulfite formed in the known carbonation or sulfitation. They also bind excess calcium hydroxide or the poorly soluble calcium salts formed. The amount of calcium hydroxide used can be reduced, whereby carbonation or sulfitation can be reduced or even completely avoided.
  • the alkali ions present in the raw juice are replaced by alkaline earth ions, which contributes to increasing the crystallization yield. If ion exchangers are used in downstream processes, the removal of the alkali ions leads to a longer service life of the ion exchangers.
  • an easily filterable and dewatered sludge continues to be formed, which contains residual calcium hydroxide (bound to the clay mineral) and poorly soluble calcium salts and which is used as a fertilizer can be used.
  • the clay mineral acts as a filter aid during precipitation and as a fertilizer when applied as a fertilizer, which promotes an even and steady release of the fertilizer in the soil.
  • the thin juices produced by the process according to the invention have a light color, and a lighter product is also obtained in the subsequent thick juice production.
  • the crystalline sugar is also lighter in color.
  • the overall yield of granulated sugar increases.
  • Bentonite in particular calcium bentonite and / or acid-activated bentonite, is preferably used as the smectitic clay mineral and / or halloysite.
  • Halloysite is a kaolin-like clay mineral and has the formula Al 4 (OH) 8 [Si 4 0 10 ] .H 2 0.
  • smectitic clay minerals are hectorite, nontronite, ver iculite and ilite.
  • an untreated, filtered raw cane sugar juice from a Central American sugar refinery is treated with the clay minerals mentioned and with Ca (0H) 2 at a temperature of 30 ° C.
  • a large-scale refined sugar solution was also analyzed for comparison (see comparative example).
  • the adsorbents used were cleaned by conventional methods, ie the accompanying minerals (quartz, feldspar) were removed by a hydrocyclone or decanter treatment.
  • the cleaned adsorbents were dried and ground.
  • Acid-activated smectites were processed using conventional methods, e.g. prepared by acid treatment of raw smectites with subsequent drying and grinding, or by acid activation of raw smectites in aqueous suspensions with subsequent filtration, washing, drying and grinding.
  • the halloysite was prepared in a similar way.
  • the products used have a water content of approximately 8 to 12% by weight and a dry sieve residue on a 63 / m sieve of approximately 20 to 30% by weight.
  • the specific surface was generally between about 50 and 200 m 2 / g, the ion exchange capacity in general between about 30 and 100 mVal / lOOg.
  • the specific surface was determined using the BET method (single point method with nitrogen according to DIN 66 131).
  • the ion exchange ability was determined as follows:
  • the dried clay mineral was reacted with a large excess of aqueous NH 4 Cl solution under reflux for one hour. After standing for 16 hours at room temperature, the mixture was filtered, the filter cake was washed, dried and ground, and the NH 4 content in the clay mineral was determined according to the Kjeldahl method.
  • Raw juice with a pH of 5.2 and a sucrose content of about 12% by weight was neutralized with a Ca (OH) 2 solution (3 ° Be) to a pH of 8.0.
  • the mixture was then mixed with various amounts of acid-activated bentonite, which was obtained by coating a Ca-bentonite (specific surface 130 m 2 / g) with 3 wt.% Conc.
  • Sulfuric acid had been prepared (SAS-1), and mixed with various amounts of Ca bentonite (S1).
  • the specific surface areas were as follows: SAS-1: 130 m 2 / g; Sl: 45 m 2 / g.
  • the cation exchange capabilities were as follows: SAS-1: 68 meq / 100g; Sl: 70 mVal / lOOg.
  • the pH value resulting after the filtration and the degree of transmission (transmittance) at 550 nm (thickness of the measuring cell 1 cm) were determined.
  • the Gardner number was also determined. The Gardner number is determined spectroscopically using comparison solutions (ASTM method D1544, 10 mm measuring cell). Bright solutions have a low Gardner number and high transmittance.
  • Ad / Ca (OH) 2 denotes the weight ratio between adsorbent and Ca (OH) 2.
  • Untreated raw sugar solution filtered cannot be determined 0 5.2
  • the raw sugar solution of Example 1 was prepared by introducing 2% by weight of a mixture of Ca (0H) 2 and an acid-activated bentonite, which had been prepared by slurry activation of the Ca-bentonite (S1) from Example 1 with 35% by weight of sulfuric acid (SAS- 2), treated (specific surface area 220 m 2 / g; cation exchange capacity 35 mVal / lOOg). After the filtration, the sugar solution was analyzed.
  • the halloysite had a specific one Surface area of 153 m 2 / g and a cation exchange capacity of 58 mVal / lOOg.
  • the following procedure was used in a typical Central American sugar refinery based on cane sugar.
  • the stated% by weight values relate to the mass of sugar cane used.
  • the sulfur dioxide was obtained by burning sulfur.
  • Ca (0H) 2 (7-9 ° Be) was added to the raw sugar solution until a pH of 7.0 to 7.5 was reached. This required 0.094% by weight of Ca (OH) 2 .
  • the temperature was 32 to 36 ° C.
  • the mixture was heated to about 100 ° C by indirect heating and under gentle Stirring held at this temperature for 40 min.
  • a polyacrylamide flocculant (7.3 ppb) was added to improve the precipitation reactions.
  • the filtrate (purified thin juice) was concentrated under reduced pressure at a temperature of 100 ° C.
  • the crystal sugar obtained was 10.4% by weight.
  • the proportion of non-crystallizable material (molasses) in the total solids content of the purified thin juice was 3.9% by weight.
  • the temperature here was 32 to 36 ° C. The mixture was heated to about 100 ° C. by indirect heating and kept at this temperature for 40 minutes with gentle stirring.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Non-Alcoholic Beverages (AREA)

Abstract

L'invention concerne un procédé permettant de purifier le jus brut résultant du raffinage du sucre, selon lequel on traite ce jus brut avec de l'hydroxyde de calcium. Ce procédé se caractérise en ce que l'on traite le jus brut avec un mélange constitué d'hydroxyde de calcium et d'un minéral des argiles réfractaires sélectionné dans le groupe des smectites et des kaolins, la proportion d'hydroxyde de calcium dans le mélange étant inférieure à environ 70 % en poids, et en ce que l'on sépare le minéral des argiles réfractaires, avec l'hydroxyde de calcium résiduel et les sels de calcium formés difficilement solubles, du jus léger purifié.
PCT/EP1998/006841 1997-11-03 1998-10-28 Procede de purification du jus brut resultant du raffinage du sucre WO1999024623A2 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU21515/99A AU2151599A (en) 1997-11-03 1998-10-28 Method for purifying the raw juice resulting from sugar refining

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19748494.8 1997-11-03
DE19748494A DE19748494A1 (de) 1997-11-03 1997-11-03 Verfahren zur Reinigung des bei der Zuckerraffination anfallenden Rohsaftes

Publications (2)

Publication Number Publication Date
WO1999024623A2 true WO1999024623A2 (fr) 1999-05-20
WO1999024623A3 WO1999024623A3 (fr) 1999-07-15

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PCT/EP1998/006841 WO1999024623A2 (fr) 1997-11-03 1998-10-28 Procede de purification du jus brut resultant du raffinage du sucre

Country Status (4)

Country Link
AU (1) AU2151599A (fr)
DE (1) DE19748494A1 (fr)
WO (1) WO1999024623A2 (fr)
ZA (1) ZA989833B (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005042787A1 (fr) * 2003-10-30 2005-05-12 Südzucker Aktiengesellschaft Mannheim/Ochsenfurt Procede de reduction de la consommation de chaux lors du lavage de jus de betterave a sucre
WO2008139431A2 (fr) * 2007-05-16 2008-11-20 Gabba, Lorenzo Francesco Procédé et composition pour traiter du jus de sucre brut
US9476104B2 (en) 2013-10-15 2016-10-25 Spray Engineering Devices Limited Cold juice clarification process

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1748086A1 (fr) 2005-07-27 2007-01-31 Süd-Chemie Ag Adsorbant et méthode de purification de jus de sucre
EP2236630A1 (fr) * 2009-04-02 2010-10-06 Süd-Chemie Ag Procédé de purification de jus de sucre brut

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB191306785A (en) * 1912-04-06 1914-03-19 Wladimir Guerrero Improvements in or relating to the Treatment of Cane Juices.
US5110363A (en) * 1991-01-17 1992-05-05 The Board Of Supervisors Of Louisiana State University And Agricultural And Mechanical College Composition, and method for the clarification of sugar-bearing juices, and related products

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE168030C (fr) *
DE2408410A1 (de) * 1973-02-23 1974-08-29 Calcium Products Corp Kalksteinkoerner und verfahren zu ihrer herstellung
DD235387A3 (de) * 1983-09-26 1986-05-07 Guenter Voels Verfahren zur konditionierung von kalkschlamm
US5262328A (en) * 1991-01-17 1993-11-16 Louisiana State University Board Of Supervisors Composition for the clarification of sugar-bearing juices and related products
JPH04248999A (ja) * 1991-01-30 1992-09-04 Nansei Togyo Kk 糖液の処理法

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB191306785A (en) * 1912-04-06 1914-03-19 Wladimir Guerrero Improvements in or relating to the Treatment of Cane Juices.
US5110363A (en) * 1991-01-17 1992-05-05 The Board Of Supervisors Of Louisiana State University And Agricultural And Mechanical College Composition, and method for the clarification of sugar-bearing juices, and related products

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
CHEMICAL ABSTRACTS, vol. 86, no. 14, 4. April 1977 Columbus, Ohio, US; abstract no. 92211w, A.A.LIPETS ET AL.: "Purification of diifusion juice using bentonites" XP002101016 & SAKH.PROM-ST., Bd. 12, 1976, Seiten 14-18, *
PATENT ABSTRACTS OF JAPAN vol. 017, no. 030 (C-1018), 20. Januar 1993 -& JP 04 248999 A (NANSEI TOUGIYOU KK), 4. September 1992 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005042787A1 (fr) * 2003-10-30 2005-05-12 Südzucker Aktiengesellschaft Mannheim/Ochsenfurt Procede de reduction de la consommation de chaux lors du lavage de jus de betterave a sucre
DE10350672B4 (de) * 2003-10-30 2009-10-29 Südzucker Aktiengesellschaft Verfahren zur Reduzierung des Kalkverbrauches bei der Zuckerrübensaft-Reinigung
US7955635B2 (en) 2003-10-30 2011-06-07 Sudzucker Aktiengesellschaft Process for reducing the lime consumption in sugar beet juice purification
US8893612B2 (en) 2003-10-30 2014-11-25 Sudzucker Aktiengesellschaft Process for reducing the lime consumption in sugar beet juice purification
WO2008139431A2 (fr) * 2007-05-16 2008-11-20 Gabba, Lorenzo Francesco Procédé et composition pour traiter du jus de sucre brut
WO2008139431A3 (fr) * 2007-05-16 2009-03-19 Gabba Lorenzo Francesco Procédé et composition pour traiter du jus de sucre brut
US9476104B2 (en) 2013-10-15 2016-10-25 Spray Engineering Devices Limited Cold juice clarification process

Also Published As

Publication number Publication date
DE19748494A1 (de) 1999-05-06
ZA989833B (en) 1999-04-28
AU2151599A (en) 1999-05-31
WO1999024623A3 (fr) 1999-07-15

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