EP0635578A1 - Verfahren zur Raffination des braunen Zuckers aus der Rohrzuckerindustrie - Google Patents

Verfahren zur Raffination des braunen Zuckers aus der Rohrzuckerindustrie Download PDF

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Publication number
EP0635578A1
EP0635578A1 EP94401635A EP94401635A EP0635578A1 EP 0635578 A1 EP0635578 A1 EP 0635578A1 EP 94401635 A EP94401635 A EP 94401635A EP 94401635 A EP94401635 A EP 94401635A EP 0635578 A1 EP0635578 A1 EP 0635578A1
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EP
European Patent Office
Prior art keywords
sugar
syrup
phosphating
raw sugar
sugar syrup
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Granted
Application number
EP94401635A
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English (en)
French (fr)
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EP0635578B1 (de
Inventor
Marc-André Theoleyre
Stanislas Baudoin
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Applexion SAS
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Applexion SAS
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    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B30/00—Crystallisation; Crystallising apparatus; Separating crystals from mother liquors ; Evaporating or boiling sugar juice
    • C13B30/04—Separating crystals from mother liquor
    • C13B30/14—Dissolving or refining raw sugar
    • 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
    • C13B20/126—Organic agents, e.g. polyelectrolytes
    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B20/00—Purification of sugar juices
    • C13B20/16—Purification of sugar juices by physical means, e.g. osmosis or filtration
    • C13B20/165—Purification of sugar juices by physical means, e.g. osmosis or filtration using membranes, e.g. osmosis, ultrafiltration

Definitions

  • the present invention relates to a process for refining raw sugar, in particular brown sugar from the sugar cane sugar industry.
  • the refined sugar As for the refined sugar (high products), it is subjected to an additional purification comprising operations of recasting, carbonation (treatment by calcium oxide or milk of lime and carbon dioxide) or phosphatation (treatment by calcium oxide or lime milk and phosphoric acid), front filtration or decantation, discoloration and crystallization.
  • this process is free from any tedious and costly preliminary refining operation of raw sugar, which is made possible, quite unexpectedly, according to the invention, by the use of the technique tangential microfiltration and / or tangential ultrafiltration, a well-known technique, simple, flexible, of high yield, rapid, well controlled and with an operating cost much lower than that of the abovementioned refining operation.
  • the present invention overcomes a tedious and expensive operation by implementing a simple operation that consumes little time and energy.
  • the method according to the invention may also comprise a flocculation operation using a flocculating agent, this being able to be carried out simultaneously with operation (b) or before or after this operation (b), setting implementation of such a flocculation operation making it possible to very significantly reduce the amounts of reagents (calcium oxide or lime milk, carbon dioxide and phosphoric acid) to be used in the carbonation or phosphating operation.
  • a flocculation operation using a flocculating agent this being able to be carried out simultaneously with operation (b) or before or after this operation (b), setting implementation of such a flocculation operation making it possible to very significantly reduce the amounts of reagents (calcium oxide or lime milk, carbon dioxide and phosphoric acid) to be used in the carbonation or phosphating operation.
  • the method comprises a flocculation operation and a phosphating operation, in which case calcium oxide (or whitewash), phosphoric acid and the flocculating agent are put used in phosphating and flocculation operations respectively at 200 to 900 ppm (expressed as CaO), 200-900 ppm (expressed in pure H3PO4) and 200-900 ppm (expressed as active product) relative to the material dry raw sugar syrup.
  • calcium oxide or whitewash
  • phosphoric acid and the flocculating agent are put used in phosphating and flocculation operations respectively at 200 to 900 ppm (expressed as CaO), 200-900 ppm (expressed in pure H3PO4) and 200-900 ppm (expressed as active product) relative to the material dry raw sugar syrup.
  • the flocculating agent used in the flocculation operation can in particular consist of a cationic surfactant, in particular a quaternary ammonium compound of tallow fatty acids, such as dioctadecyldimethylammonium chloride, such as NORAMIUM® M2SH marketed by the French company CECA. It may also be derivatives of deacetylated poly-N-acetylglucosamine chitosan derived from chitin such as PROFLOC® SD 340 from the Norwegian company PROTAN BIOPOLYMER.
  • a cationic surfactant in particular a quaternary ammonium compound of tallow fatty acids, such as dioctadecyldimethylammonium chloride, such as NORAMIUM® M2SH marketed by the French company CECA. It may also be derivatives of deacetylated poly-N-acetylglucosamine chitosan derived from chitin such as PROFL
  • the refining process according to the invention will be completed by an operation (d) of discoloration of the sugar syrup resulting from microfiltration and / or of ultrafiltration, and by an operation (e) of crystallization and / or demineralization of the sugar syrup resulting from the bleaching operation to thereby obtain white crystal sugar in the case of crystallization and liquid sugar (syrup) in the case of demineralization.
  • the raw sugar to be refined is brown sugar from a sugar cane sugar refinery, this brown sugar having a dry matter content (essentially sucrose) of the order of 97 to 99% by weight.
  • the brown sugar to be refined is redesigned, that is to say its dissolution in an aqueous medium such as a sweet aqueous solution or preferably water.
  • the aqueous medium is at a temperature sufficient for the remelting operation to take place at a temperature of the order of 50 to 90 ° C, preferably of the order of 80 ° C.
  • the recasting leads to the production of a brown sugar syrup, the quantity of aqueous medium used being preferably chosen so that said syrup has a dry matter content of the order of 40 to 70% by weight.
  • This recasting operation is carried out in a tank 1 provided at its upper part with a supply 2 of brown sugar and a supply 3 with hot water. To obtain a homogeneous syrup, this reservoir is also provided with stirring means 4.
  • the brown sugar syrup resulting from this recasting operation which usually has a coloration of 2500-4500 ICUMSA units (international units) and a cloudiness of 3000-4000 ICUMSA units, is then subjected to a phosphating operation together with an operation flocculation.
  • the syrup is extracted at the base of the reservoir 1 by a conduit 5 connected to the suction of a circulation pump 6 whose delivery is extended by a conduit 7 opening at the top of a reservoir 8 of phosphating / flocculation.
  • the syrup is heated, for example by indirect heat exchange in a heat exchanger 9 arranged on the path of the syrup between the reservoir 1 and the reservoir 8. This exchanger is chosen to bring, if necessary, the syrup to a sufficient temperature so that within the tank 8 prevails a temperature of the order of 70 ° C.
  • a flocculating agent is then introduced. More precisely, the latter is brought to the upper part of the reservoir 8, from a reservoir 10 of flocculating agent, comprising at its base an extraction duct 11 connected to the suction of a circulation pump 12, of which the discharge is connected to a conduit 13 leading to the reservoir 8.
  • the reservoir 10 may be provided with heating means (not shown) such as an internal jacket in which a hot fluid circulates, for example hot water or water vapor, these heating means making it possible, in the case where the flocculating agent is solid or pasty at room temperature, to bring it in liquid form with a view to pumping it by the pump 12.
  • this flocculating agent consists of NORAMIUM® M2SH whose melting point is of the order of 60 ° C
  • the heating means are designed to bring the latter to a temperature of the order of 60-65 ° C.
  • the quantity of flocculating agent used is in the order of 200 to 900 ppm of active product relative to the dry matter of the brown sugar syrup; for example in the case of NORAMIUM® M2SH, this amount will preferably be of the order of 500 ppm of active product relative to the dry matter of the syrup.
  • lime milk (at a concentration of 200 g / l expressed as CaO) is introduced into the tank 8 in an amount of the order of 300 ppm expressed as CaO relative to the dry matter of the syrup, then phosphoric acid (for example a 90% solution) until neutralization, ie approximately 250 ppm expressed as pure phosphoric acid and relative to the dry matter of the syrup.
  • phosphoric acid for example a 90% solution
  • the introduction of the milk of lime and of the phosphoric acid into the tank 8 is carried out in the same way as for the flocculating agent, that is to say respectively from a tank 14 of milk of lime and a reservoir 15 of phosphoric acid, via extraction conduits 16, 17, circulation pumps 18, 19 and conduits 20, 21 connected to said pumps and ending at reservoir 8.
  • the reservoir 8 and provided with stirring means for carrying out a violent mixing of its contents.
  • the flocculating agent could, as a variant, be introduced into the reservoir 8 at the same time or after the milk of lime and the phosphoric acid, preference being however given to the procedure described above.
  • the flocculating agent there is precipitation of part of the dyes and suspended solids. A large part of the remaining dyes and suspended solids is removed by the phosphating operation, the calcium phosphate formed by the reaction between whitewash and phosphoric acid precipitating with occlusion of said dyes and suspended solids.
  • the syrup having undergone the flocculation / phosphating is withdrawn from this reservoir 8 by a pump 22 discharging into a unit 23 of tangential microfiltration or tangential ultrafiltration. If necessary, the syrup thus withdrawn can be reheated so that the operation in this unit 23 takes place at around 80 ° C.
  • the membrane used in unit 23 may have a cut-off threshold of 10 nm to 1 ⁇ m (preferably of the order of 0.1 ⁇ m), the syrup circulating with a tangential speed of the order of 1 to 8 m / s (preferably 4 to 6 m / s) and the permeate flow rate being of the order of 20 to 80 liters / hour.m2 of membrane (preferably 35-50 liters / hour.m2 of membrane).
  • a membrane use can be made of organic polymer or ceramic membranes. Good results have been obtained with a zirconium oxide membrane on a ceramic support, manufactured by the French company TECH-SEP.
  • the permeate from unit 23 (coloring on the order of 1000-2000 ICUMSA units and cloudiness of less than 20 ICUMSA units) is conveyed through a conduit 24 into a storage tank 25, from which it is withdrawn by a pump. 26 to be brought to the head of a two-stage bleaching column 27, 28.
  • These columns are packed with a material adsorbing the dyes such as animal black, activated carbon or preferably a bleaching resin; it may be a strong anionic resin in the form of chloride (for example, IRA® 900 resin from Rohm and Haas).
  • the bleaching operation in this column is preferably carried out at 70-90 ° C, in particular at 80 ° C.
  • the discolored syrup (coloration ⁇ 400 ICUMSA units) is brought into a tank 29.
  • This discolored syrup can then be transformed into either crystal sugar or demineralized syrup.
  • the syrup is brought by a pump 30 into an evaporator 31, for example a falling-stream evaporator, then the concentrated syrup is brought by a pump 32 into a crystallization unit 33 where it undergoes several successive crystallizations (three in the example illustrated in the figure) to deliver crystal sugar and a crystallization drain.
  • the discolored syrup is brought, by a pump 34, from the reservoir 29 into a demineralization unit 35 which can for example consist of a column packed with a mixture of cationic resins in H+ form and anionic in OH ⁇ form.
  • This column in a mixed bed of resins can be replaced by two columns filled one with cationic resin in H+ form and the other with anionic resin in OH ⁇ form. After the demineralization treatment, a syrup with a coloration ⁇ 20 ICUMSA units is obtained.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Organic Chemistry (AREA)
  • Water Supply & Treatment (AREA)
  • Electrochemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Jellies, Jams, And Syrups (AREA)
  • Confectionery (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Saccharide Compounds (AREA)
  • Seasonings (AREA)
  • Disintegrating Or Milling (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
EP94401635A 1993-07-19 1994-07-13 Verfahren zur Raffination des braunen Zuckers aus der Rohrzuckerindustrie Expired - Lifetime EP0635578B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9308826A FR2707997B1 (fr) 1993-07-19 1993-07-19 Procédé de raffinage d'un sucre brut, notamment de sucre roux provenant de l'industrie sucrière de la canne à sucre.
FR9308826 1993-07-19

Publications (2)

Publication Number Publication Date
EP0635578A1 true EP0635578A1 (de) 1995-01-25
EP0635578B1 EP0635578B1 (de) 1999-11-03

Family

ID=9449354

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EP94401635A Expired - Lifetime EP0635578B1 (de) 1993-07-19 1994-07-13 Verfahren zur Raffination des braunen Zuckers aus der Rohrzuckerindustrie

Country Status (10)

Country Link
US (1) US5865899A (de)
EP (1) EP0635578B1 (de)
AT (1) ATE186331T1 (de)
AU (1) AU674755B2 (de)
BR (1) BR9402810A (de)
CA (1) CA2128366C (de)
CO (1) CO4370780A1 (de)
DE (1) DE69421458D1 (de)
FR (1) FR2707997B1 (de)
ZA (1) ZA945133B (de)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5468301A (en) * 1994-04-07 1995-11-21 International Food Processing Incorporated Process for producing refined sugar
EP0655507A3 (de) * 1993-11-12 1996-03-20 Applexion Verfahren zur Herstellung von Kristallzucker aus einem wässrigen Zuckersaft, z.B. Zuckerrohr-oder Zuckerrübesaft.
US5759283A (en) * 1996-05-14 1998-06-02 The Western Sugar Company Method for processing sugar beets to produce a purified beet juice product
WO2000060128A1 (en) * 1999-04-07 2000-10-12 Aeci Limited Treatment of sugar juice
EP2499266A4 (de) * 2009-11-11 2014-04-09 Carbo Ua Ltd Zusammensetzungen und verfahren für verbesserte carbonatierungsklärung von zuckerlaugen und sirups
US9163293B2 (en) 2009-11-11 2015-10-20 Carbo-UA Limited Compositions and processes for improving phosphatation clarification of sugar liquors and syrups
US9175358B2 (en) 2009-11-11 2015-11-03 Carbo-UA Limited Compositions and processes for sugar treatment
EP2944701A1 (de) 2014-05-16 2015-11-18 Sociedade Portuguesa do Ar Líquido Verfahren zur Karbonisierung
US9605324B2 (en) 2009-12-23 2017-03-28 Carbo-UA Limited Compositions and processes for clarification of sugar juices and syrups in sugar mills

Families Citing this family (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU688197B2 (en) * 1995-02-16 1998-03-05 Csr Limited Process for refining raw sugar
AUPN118095A0 (en) * 1995-02-16 1995-03-09 Csr Limited Improved process for the refining of sugar
US6096136A (en) * 1996-10-18 2000-08-01 Board Of Supervisors Of Louisiana State University And Agricultural And Mechanical College Method for producing white sugar
US6037456A (en) * 1998-03-10 2000-03-14 Biosource Technologies, Inc. Process for isolating and purifying viruses, soluble proteins and peptides from plant sources
US6174378B1 (en) * 1999-08-19 2001-01-16 Tate Life Industries, Limited Process for production of extra low color cane sugar
US6375751B2 (en) * 1999-08-19 2002-04-23 Tate & Lyle, Inc. Process for production of purified cane juice for sugar manufacture
US6387186B1 (en) * 1999-08-19 2002-05-14 Tate & Lyle, Inc. Process for production of purified beet juice for sugar manufacture
US6485574B1 (en) * 2000-06-23 2002-11-26 Chung-Chi Chou Process for pretreating colored aqueous sugar solutions to produce a low colored crystallized sugar
US6656287B2 (en) 2002-04-15 2003-12-02 Co2 Solutions, Llc System to produce sugar from plant materials
FR2838751B1 (fr) * 2002-04-17 2007-03-09 Applexion Ste Nouvelle De Rech Procede et installation de fabrication de sucre raffine a partir de jus sucre
FR2907687B1 (fr) * 2006-10-30 2008-12-26 Applexion Procede de purification de sialyllactose par chromatographie
FR2925349A1 (fr) * 2007-12-20 2009-06-26 Applexion Procede de separation sequence multicolonnes d'un derive metallique ionique
US9055752B2 (en) * 2008-11-06 2015-06-16 Intercontinental Great Brands Llc Shelf-stable concentrated dairy liquids and methods of forming thereof
UA112972C2 (uk) 2010-09-08 2016-11-25 Інтерконтінентал Грейт Брендс ЛЛС Рідкий молочний концентрат з високим вмістом сухих речовин
US9080221B2 (en) 2011-12-02 2015-07-14 Amalgamated Research Llc System and process for refining sugar
CN103757143A (zh) * 2014-01-10 2014-04-30 河南工业大学 一种糖汁澄清方法
WO2018029500A1 (en) 2016-08-08 2018-02-15 Rhodia Poliamida E Especialidades S.A. New components to clarify sugar cane juice in a process for producing crystal or raw sugar
CN108929391A (zh) * 2018-07-24 2018-12-04 北京美亚斯磷脂技术有限公司 一种菊糖提取液的纯化方法
CN109628649A (zh) * 2018-12-21 2019-04-16 广东省生物工程研究所（广州甘蔗糖业研究所） 一种糖汁高质量清净方法
ES2779058B2 (es) * 2019-02-13 2021-04-12 Seppelec S L Procedimiento para obtener jarabe de azúcar refinado a partir de azúcar crudo para su aplicación en plantas embotelladoras de bebidas azucaradas no alcohólicas y jarabe así obtenido
GB202310865D0 (en) 2023-07-14 2023-08-30 Sudeco International Ltd Chemical-free processes and methods of neutralisation, clarification, purification and decolourisation for sugar manufacturing and correlated effluents

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Publication number Priority date Publication date Assignee Title
FR2135169A1 (de) * 1971-04-23 1972-12-15 Danske Sukkerfab
GB2090861A (en) * 1981-01-14 1982-07-21 Danske Sukkerfab Purifying sugar juice
AU624560B1 (en) * 1990-11-13 1992-06-11 Csr Limited Sugar refining process
JPH04249000A (ja) * 1991-01-30 1992-09-04 Nansei Togyo Kk 廃糖蜜の清浄法

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US3166442A (en) * 1963-05-23 1965-01-19 Minerals & Chem Philipp Corp Method for treating sugar liquor
US3563799A (en) * 1967-10-02 1971-02-16 Industrial Filter Pump Mfg Co Purified liquid sugar concentrate and method of manufacturing same
GB1350261A (en) * 1970-10-16 1974-04-18 Hitachi Shipbuilding Eng Co Sugar refining process
US3799806A (en) * 1972-04-20 1974-03-26 Danske Sukkerfab Process for the purification and clarification of sugar juices,involving ultrafiltration

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2135169A1 (de) * 1971-04-23 1972-12-15 Danske Sukkerfab
GB2090861A (en) * 1981-01-14 1982-07-21 Danske Sukkerfab Purifying sugar juice
AU624560B1 (en) * 1990-11-13 1992-06-11 Csr Limited Sugar refining process
JPH04249000A (ja) * 1991-01-30 1992-09-04 Nansei Togyo Kk 廃糖蜜の清浄法

Non-Patent Citations (2)

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DATABASE WPI Section Ch Week 9242, Derwent World Patents Index; Class D17, AN 92-344727 *
S.BUDAVARI ET AL.: "The Merck Index", 1989, MERCK, RAHWAY,N.J. *

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0655507A3 (de) * 1993-11-12 1996-03-20 Applexion Verfahren zur Herstellung von Kristallzucker aus einem wässrigen Zuckersaft, z.B. Zuckerrohr-oder Zuckerrübesaft.
US5468301A (en) * 1994-04-07 1995-11-21 International Food Processing Incorporated Process for producing refined sugar
US5468300A (en) * 1994-04-07 1995-11-21 International Food Processing Incorporated Process for producing refined sugar directly from sugarcane
US5759283A (en) * 1996-05-14 1998-06-02 The Western Sugar Company Method for processing sugar beets to produce a purified beet juice product
WO2000060128A1 (en) * 1999-04-07 2000-10-12 Aeci Limited Treatment of sugar juice
EP2499266A4 (de) * 2009-11-11 2014-04-09 Carbo Ua Ltd Zusammensetzungen und verfahren für verbesserte carbonatierungsklärung von zuckerlaugen und sirups
US9163293B2 (en) 2009-11-11 2015-10-20 Carbo-UA Limited Compositions and processes for improving phosphatation clarification of sugar liquors and syrups
US9163292B2 (en) 2009-11-11 2015-10-20 Carbo-UA Limited Compositions and process for improving carbonatation clarification of sugar liquors and syrups
US9175358B2 (en) 2009-11-11 2015-11-03 Carbo-UA Limited Compositions and processes for sugar treatment
US9605324B2 (en) 2009-12-23 2017-03-28 Carbo-UA Limited Compositions and processes for clarification of sugar juices and syrups in sugar mills
EP2944701A1 (de) 2014-05-16 2015-11-18 Sociedade Portuguesa do Ar Líquido Verfahren zur Karbonisierung
US9938591B2 (en) 2014-05-16 2018-04-10 L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Method for carbonation

Also Published As

Publication number Publication date
CA2128366A1 (en) 1995-01-20
ATE186331T1 (de) 1999-11-15
BR9402810A (pt) 1995-04-04
ZA945133B (en) 1995-03-16
FR2707997A1 (fr) 1995-01-27
CO4370780A1 (es) 1996-10-07
DE69421458D1 (de) 1999-12-09
US5865899A (en) 1999-02-02
EP0635578B1 (de) 1999-11-03
AU6755194A (en) 1995-01-27
FR2707997B1 (fr) 1995-09-29
CA2128366C (en) 2005-12-06
AU674755B2 (en) 1997-01-09

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