CN102676606A - Process for clarifying and removing impurities from fermentation liquor of xylose mother liquid - Google Patents

Process for clarifying and removing impurities from fermentation liquor of xylose mother liquid Download PDF

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Publication number
CN102676606A
CN102676606A CN2012101684555A CN201210168455A CN102676606A CN 102676606 A CN102676606 A CN 102676606A CN 2012101684555 A CN2012101684555 A CN 2012101684555A CN 201210168455 A CN201210168455 A CN 201210168455A CN 102676606 A CN102676606 A CN 102676606A
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liquid
membrane
film
ion exchange
xylose mother
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孙鲁
于军伟
杜瑞锋
刘晓娟
王学敏
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Shandong Futian Pharmaceutical Co Ltd
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Shandong Futian Pharmaceutical Co Ltd
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Abstract

The invention discloses a process for clarifying and removing impurities from a fermentation liquor of a xylose mother liquid, and belongs to the technical field of function sugar-alcohol production. According to the production process, a membrane separation technology is adopted, and the fermentation liquor of the xylose mother liquid in an arabinose production process is processed, wherein a membrane core of a membrane system is an ultrafiltration membrane, and monosaccharide is not intercepted basically. The production process comprises the following steps: (1) fermenting; (2) clarifying and removing proteins from the fermentation liquor; (3) decoloring; (4) performing ion exchange; (5) performing multiple-effect concentration; (6) decoloring; (7) performing chromatographic separation; (8) performing ion exchange; (9) performing vacuum concentration; (10) centrifuging crystals; and (11) drying, screening and packaging crystal arabinose to obtain tabular crystal arabinose. Vacuum drum filtration is changed into membrane filtration in the arabinose production process, the consumption of kieselguhr is reduced, the quality of a dialysis fluid is stable and is influenced by raw materials a little, the efficiency of the subsequent decoloring process is improved and the cost and labor intensity are reduced.

Description

Xylose mother liquid fermented liquid clarification impurity removal process
Technical field
The invention belongs to technical field of functional sugar alcohol production, be specifically related to the xylose mother liquid fermentation liquor treatment technology in the pectinose production process.
Background technology
The industrial production of pectinose is raw material with the xylose mother liquid, removes glucose by fermentation, centrifugally removes yeast, rotary drum filtration, activated carbon decolorizing, IX, chromatographic separation, concentrates, Crystallization Procedure makes.Contain a large amount of albumen in the feed liquid of back by fermentation; Eliminating albumen in the present existing pectinose production technique mainly is through carrying out activated carbon decolorizing behind the vacuum drum precoating diatomite filtration again; But because the particle of zeyssatite itself is bigger; The coating that forms can not be held back the albumen in the fermented liquid, and follow-up activated carbon decolorizing difficulty is big and concentrate the reason liquid glucose viscosity increase of back owing to impurity, influences the follow-up crystallization and the quality of product.
Membrane filtration process makes material through behind the film exactly under the higher pressure, the impurity that molecular weight is bigger is realized physical sepn with other small-molecule substances, and the general temperature of membrane filtration process is lower, and is very favourable to the separating substances of some biologically actives.Patent CN1414001 has introduced " enzyme process prepares the regulate and control method of different oligose "; Through selecting the different film mediums and the size of membrane pore size; Oligose to different polymerization degree separates immediately; Ultrafiltrated separates through the nanofiltration device again, removes micromolecular compounds such as SA monose, disaccharides and water, obtains the oligose of different polymerization degree.Contain more albumen and other macromolecular substance in the xylose mother liquid fermented liquid, feed liquid is muddy, and transparence is lower; Macromolecular substance absorption activated carbons such as albumen; Make feed liquid gac viscosity when decolouring increase, sheet frame stops up serious, and difficulty in filtration increases; Long filtration time makes the filtrating color present grey, and ensuing ion exchange resin is polluted.Select suitable aperture ultra-filtration membrane that fermented liquid is handled, could reduce the content of other macromolecular substance such as proteinochrome, improve the efficient of decolouring, reduce the pollution of diatomaceous consumption and feed liquid, reach the purpose that reduces cost resin.
Summary of the invention
In order to overcome the defective of prior art; The present invention provides the impurity removal process of the xylose mother liquid fermented liquid clarification in a kind of pectinose production technique; Filter the drawback that exists to solve the vacuum drum that uses in the xylose mother liquid fermented liquid clarification removal of impurities operation in the prior art, overcome difficult, the problems such as the zeyssatite consumption is big, energy consumption height of unstable, the follow-up decolouring of the feed liquid quality that exists in the technology.
The technical solution adopted for the present invention to solve the technical problems is to adopt membrane separation technique; Through the film system, what the film core of its film system adopted is ultra-filtration membrane with centrifugate, and it is that 100,000 dalton and molecular weight cut-off are 300,000 daltonian two kinds of films that molecular weight cut-off is arranged; Xylose mother liquid fermented liquid in the pectinose production technique is handled; Ultra-filtration membrane according to the invention can be a rolled film, also can be tubular membrane or hollow cellulose film, and ultra-filtration membrane does not exist monose basically to be held back.Its concrete production craft step is following:
(1) fermentation: xylose mother liquid is added water be assigned to Brix value 16%-20%; Add urea and phosphoric acid and regulate pH to 4.6-5.0; Add yeast, keep leavening temperature, whenever measured the fermented liquid glucose content at a distance from two hours at 33-36 ℃; To glucose content reduce to stop below 1% the fermentation, the centrifugal yeast of removing of fermented liquid;
(2) the fermented liquid clarification removes albumen: centrifugate is passed through the film system; What the film core of its film system adopted is ultra-filtration membrane, and the liquid concentrator of film system and the volume flow ratio of dialyzate are 1:12-1:30, pressure 2.7-3.1Mpa before the film; 30 ℃-50 ℃ of feed temperatures; The Brix value of dialyzate and liquid concentrator is consistent basically with stoste, changes lessly, and liquid concentrator can return in the step (1) fermentation once more;
(3) decolouring: the 4-6% that in the dialyzate of step (2) gained, presses amount of dry matter adds powdered active carbon, and 75 ℃-80 ℃ are incubated 25-35 minute, filters and obtains destainer;
(4) IX: the destainer that step (3) obtains carries out desalting treatment through ion exchange resin and obtains ion exchange liquid;
(5) multiple-effect concentrates: ion exchange liquid is concentrated into the liquid glucose of Brix value for 40-48% through multiple-effect evaporator;
(6) decolouring: the liquid glucose that step (5) is obtained gets into 75 ℃-80 ℃ insulations of powdered active carbon 25-35 minute according to the 4-6% of amount of dry matter, filters to obtain two and take off liquid;
(7) chromatographic separation: two of step (6) is taken off liquid separate, collect chromatographic separation liquid through chromatogram;
(8) IX: the pectinose component liquid of collecting in the step (7) is carried out IX;
(9) vacuum concentration: the ion exchange liquid with step (8) obtains, obtain the vacuum concentration liquid glucose that Brix is 80%-86% through vacuum concentration, vacuum tightness is 9.7*10 4Pa;
(10) crystallization is centrifugal: the vacuum concentration liquid glucose that step (9) is obtained goes to crystallizer tank, 70-80 ℃ of insulation 1-1.5 hour, then with the speed decrease temperature crystalline of 1-2 ℃/h, reduces to 38-42 ℃ and carries out spinning, obtains crystal pectinose and mother liquor;
(11) dry, screening and packing: the crystal pectinose is dry, screening, packing back warehouse-in are preserved.
Positively effect of the present invention is: the vacuum drum in the pectinose production technique is filtered change membrane filtration into; Reduced the zeyssatite consumption; It is little and stable that mass of dialysate is influenced by raw material, improved the efficient of follow-up decoloration process, helps reducing production costs and labour intensity.
Specific embodiment
Below in conjunction with specific embodiment the present invention is further specified.
Embodiment 1
(1) fermentation: get 3 tons of xylose mother liquids and add water and be assigned to Brix value 18.5%, add 10 kilograms in urea and phosphoric acid 2L, adjusting pH to 4.8; Add the active dry yeast 120 kg; Keep leavening temperature at 35 ℃, whenever measured the fermented liquid glucose content at a distance from two hours, glucose content reduces to 0.9% after 4 hours; Stop fermentation, the centrifugal yeast of removing of fermented liquid;
(2) the fermented liquid clarification removes albumen: adopt membrane separation technique; Centrifugate through the film system, is handled the xylose mother liquid fermented liquid in the pectinose production technique, centrifugate is passed through the film system; What the film core of its film system adopted is ultra-filtration membrane; The film core is 300,000 daltonian tubular ultra-filtration membranes for seeing through molecular weight, and the liquid concentrator of film system and the volume flow ratio of dialyzate are 1:20, and pressure maintains 3.1Mpa before the film; Feed temperature maintains 30-45 ℃, and the Brix value of dialyzate and liquid concentrator is respectively 17.5% and 19.5%;
(3) decolouring: in the dialyzate of step (2) gained, press 5% of amount of dry matter and add powdered active carbon, 75 ℃ are incubated 30 minutes, filter and obtain destainer;
(4) IX: the destainer that step (3) obtains carries out desalting treatment through ion exchange resin and obtains ion exchange liquid;
(5) multiple-effect concentrates: it is 44% liquid glucose that ion exchange liquid is concentrated into the Brix value through multiple-effect evaporator;
(6) decolouring: the liquid glucose that step (5) is obtained gets into 75 ℃ of insulations of powdered active carbon 30 minutes according to 5% of amount of dry matter, and filtration obtains two and takes off liquid;
(7) chromatographic separation: two of step (6) is taken off liquid separate, collect chromatographic separation liquid through chromatogram;
(8) IX: the pectinose component liquid of collecting in the step (7) is carried out IX;
(9) vacuum concentration: the ion exchange liquid that step (8) is obtained, obtaining Brix through vacuum concentration is 86% vacuum concentration liquid glucose, vacuum tightness is 9.7*10 4Pa;
(10) crystallization is centrifugal: the vacuum concentration liquid glucose that step (9) is obtained goes to crystallizer tank, 70 ℃ of insulations 1 hour, then with the speed decrease temperature crystalline of 1.5 ℃/h, reduces to 40 ℃ and carries out spinning, obtains crystal pectinose and mother liquor;
(11) drying, screening and packing: after crystal pectinose drying, screening, packing, warehouse-in is preserved.
Metal detection and quality inspection result are following:
Figure 370124DEST_PATH_IMAGE002
Embodiment 2
(1) fermentation: get 2.5 tons of xylose mother liquids and add water and be assigned to Brix value 16%, add 8.3 kilograms in urea and phosphatase 11 .7L, adjusting pH to 4.8; Add the active dry yeast 120 kg; Keep leavening temperature at 35 ℃, whenever measured the fermented liquid glucose content at a distance from two hours, glucose content reduces to 0.5% after 4 hours; Stop fermentation, the centrifugal yeast of removing of fermented liquid;
(2) the fermented liquid clarification removes albumen: adopt membrane separation technique; Centrifugate through the film system, is handled the xylose mother liquid fermented liquid in the pectinose production technique, centrifugate is passed through the film system; What the film core of its film system adopted is ultra-filtration membrane; The film core is the rolling ultra-filtration membrane below 100,000 dalton for seeing through molecular weight, and the liquid concentrator of film system and the volume flow ratio of dialyzate are 1:15, pressure 2.8Mpa before the film; Feed temperature maintains 30-45 ℃, and the Brix value of dialyzate and liquid concentrator is respectively 15% and 18%;
(3) decolouring: in the dialyzate of step (2) gained, press 5% of amount of dry matter and add powdered active carbon, 80 ℃ are incubated 30 minutes, filter and obtain destainer;
(4) IX: the destainer that step (3) obtains carries out desalting treatment through ion exchange resin and obtains ion exchange liquid;
(5) multiple-effect concentrates: it is 44% liquid glucose that ion exchange liquid is concentrated into the Brix value through multiple-effect evaporator;
(6) decolouring: the liquid glucose that step (5) is obtained gets into 80 ℃ of insulations of powdered active carbon 30 minutes according to 5% of amount of dry matter, and filtration obtains two and takes off liquid;
(7) chromatographic separation: two of step (6) is taken off liquid separate, collect chromatographic separation liquid through chromatogram;
(8) IX: the pectinose component liquid of collecting in the step (7) is carried out IX;
(9) vacuum concentration: the ion exchange liquid that step (8) is obtained, obtaining Brix through vacuum concentration is 86% vacuum concentration liquid glucose, vacuum tightness is 9.7*10 4Pa;
(10) crystallization is centrifugal: the vacuum concentration liquid glucose that step (9) is obtained goes to crystallizer tank, 80 ℃ of insulations 1 hour, then with the speed decrease temperature crystalline of 1.5 ℃/h, reduces to 40 ℃ and carries out spinning, obtains crystal pectinose and mother liquor;
(11) dry, screening and packing: the crystal pectinose is dry, screening, packing back warehouse-in are preserved.
Metal detection and quality inspection result are following:

Claims (2)

1. an xylose mother liquid fermented liquid is clarified impurity removal process; It is characterized in that adopting membrane separation technique; Through the film system, what the film core of film system adopted is ultra-filtration membrane with centrifugate, and it is that 100,000 dalton and molecular weight cut-off are 300,000 daltonian two kinds of films that molecular weight cut-off is arranged; Xylose mother liquid fermented liquid in the pectinose production technique is handled, and its production craft step is following:
(1) fermentation: xylose mother liquid is added water be assigned to Brix value 16%-20%; Add urea and phosphoric acid and regulate pH to 4.6-5.0; Add yeast, keep leavening temperature, whenever measured the fermented liquid glucose content at a distance from two hours at 33-36 ℃; To glucose content reduce to stop below 1% the fermentation, the centrifugal yeast of removing of fermented liquid;
(2) the fermented liquid clarification removes albumen: centrifugate is passed through the film system; What the film core of its film system adopted is ultra-filtration membrane, and the liquid concentrator of film system and the volume flow ratio of dialyzate are 1:12-1:30, pressure 2.7-3.1Mpa before the film; Feed temperature is between 30 ℃-50 ℃; The Brix value of dialyzate and liquid concentrator is consistent basically with stoste, changes lessly, and liquid concentrator can return in the step (1) fermentation once more;
(3) decolouring: the 4-6% that in the dialyzate of step (2) gained, presses amount of dry matter adds powdered active carbon, and 75 ℃-80 ℃ are incubated about 25-35 minute, filters and obtains destainer;
(4) IX: the destainer that step (3) obtains carries out desalting treatment through ion exchange resin and obtains ion exchange liquid;
(5) multiple-effect concentrates: ion exchange liquid is concentrated into the liquid glucose of Brix value for 40-48% through multiple-effect evaporator;
(6) decolouring: the liquid glucose that step (5) is obtained gets into 75 ℃-80 ℃ insulations of powdered active carbon about 25-35 minute according to the 4-6% of amount of dry matter, filters to obtain two and take off liquid;
(7) chromatographic separation: two of step (6) is taken off liquid separate, collect chromatographic separation liquid through chromatogram;
(8) IX: the pectinose component liquid of collecting in the step (7) is carried out IX;
(9) vacuum concentration: the ion exchange liquid with step (8) obtains, obtain the vacuum concentration liquid glucose that Brix is 80%-86% through vacuum concentration, vacuum tightness is 9.7*10 4Pa;
(10) crystallization is centrifugal: the vacuum concentration liquid glucose that step (9) is obtained goes to crystallizer tank, 70-80 ℃ of insulation 1-1.5 hour, then with the speed decrease temperature crystalline of 1-2 ℃/h, reduces to 38-42 ℃ and carries out spinning, obtains crystal pectinose and mother liquor;
(11) dry, screening and packing: the crystal pectinose is dry, screening, packing back warehouse-in are preserved.
2. xylose mother liquid fermented liquid clarification impurity removal process according to claim 1 is characterized in that ultra-filtration membrane described in the present invention can be a rolled film, also can be tubular membrane or hollow cellulose film, and ultra-filtration membrane does not exist monose basically to be held back.
CN2012101684555A 2012-05-28 2012-05-28 Process for clarifying and removing impurities from fermentation liquor of xylose mother liquid Pending CN102676606A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102943131A (en) * 2012-11-30 2013-02-27 安徽丰原发酵技术工程研究有限公司 Xylose preparation method
CN103409565A (en) * 2013-07-26 2013-11-27 山东福田药业有限公司 Preparation technology of xylose
CN106755613A (en) * 2016-12-16 2017-05-31 广州双桥股份有限公司 A kind of purification process of starch sugar
CN107778333A (en) * 2017-12-08 2018-03-09 山东福田药业有限公司 A kind of combination decoloration process of fermentation liquor of xylose mother liquid
CN109384819A (en) * 2018-11-14 2019-02-26 浙江华康药业股份有限公司 The minimizing technology of xylose mother liquid impurity
CN112029914A (en) * 2020-09-22 2020-12-04 焦作市华康糖醇科技有限公司 Pretreatment method of xylose mother liquor
CN112225762A (en) * 2020-11-09 2021-01-15 安阳市豫鑫木糖醇科技有限公司 Process for extracting xylose
CN114478191A (en) * 2021-12-29 2022-05-13 浙江华康药业股份有限公司 Refining treatment system and method for xylitol fermentation liquor

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002053783A1 (en) * 2000-12-28 2002-07-11 Danisco Sweeteners Oy Recovery of xylose
CN101372700A (en) * 2008-07-24 2009-02-25 上海交通大学 Method for extracting L-arabinose from xylose mother liquor and biomass acid hydrolysis solution
CN101643752A (en) * 2009-06-26 2010-02-10 安徽丰原发酵技术工程研究有限公司 Method for producing xylitol and L-arabinose by xylose mother liquor

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002053783A1 (en) * 2000-12-28 2002-07-11 Danisco Sweeteners Oy Recovery of xylose
CN101372700A (en) * 2008-07-24 2009-02-25 上海交通大学 Method for extracting L-arabinose from xylose mother liquor and biomass acid hydrolysis solution
CN101643752A (en) * 2009-06-26 2010-02-10 安徽丰原发酵技术工程研究有限公司 Method for producing xylitol and L-arabinose by xylose mother liquor

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102943131A (en) * 2012-11-30 2013-02-27 安徽丰原发酵技术工程研究有限公司 Xylose preparation method
CN103409565A (en) * 2013-07-26 2013-11-27 山东福田药业有限公司 Preparation technology of xylose
CN103409565B (en) * 2013-07-26 2015-04-22 山东福田药业有限公司 Preparation technology of xylose
CN106755613A (en) * 2016-12-16 2017-05-31 广州双桥股份有限公司 A kind of purification process of starch sugar
CN107778333A (en) * 2017-12-08 2018-03-09 山东福田药业有限公司 A kind of combination decoloration process of fermentation liquor of xylose mother liquid
CN109384819A (en) * 2018-11-14 2019-02-26 浙江华康药业股份有限公司 The minimizing technology of xylose mother liquid impurity
CN112029914A (en) * 2020-09-22 2020-12-04 焦作市华康糖醇科技有限公司 Pretreatment method of xylose mother liquor
CN112225762A (en) * 2020-11-09 2021-01-15 安阳市豫鑫木糖醇科技有限公司 Process for extracting xylose
CN114478191A (en) * 2021-12-29 2022-05-13 浙江华康药业股份有限公司 Refining treatment system and method for xylitol fermentation liquor

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Application publication date: 20120919