CN101810262B - Xylitol mother liquor crystallization method - Google Patents
Xylitol mother liquor crystallization method Download PDFInfo
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- CN101810262B CN101810262B CN200910014321A CN200910014321A CN101810262B CN 101810262 B CN101810262 B CN 101810262B CN 200910014321 A CN200910014321 A CN 200910014321A CN 200910014321 A CN200910014321 A CN 200910014321A CN 101810262 B CN101810262 B CN 101810262B
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- CN
- China
- Prior art keywords
- massecuite
- xylitol
- mother liquor
- freezing
- crystallization
- Prior art date
- Legal status (The legal status 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 status listed.)
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- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 title claims abstract description 39
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 235000010447 xylitol Nutrition 0.000 title claims abstract description 39
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 title claims abstract description 39
- 229960002675 xylitol Drugs 0.000 title claims abstract description 39
- 239000000811 xylitol Substances 0.000 title claims abstract description 39
- 239000012452 mother liquor Substances 0.000 title claims abstract description 26
- 238000002425 crystallisation Methods 0.000 title claims abstract description 24
- 239000013078 crystal Substances 0.000 claims abstract description 22
- 230000008014 freezing Effects 0.000 claims abstract description 22
- 238000007710 freezing Methods 0.000 claims abstract description 22
- 230000018044 dehydration Effects 0.000 claims abstract description 10
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000004806 packaging method and process Methods 0.000 claims abstract description 7
- 238000004094 preconcentration Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- CHHHXKFHOYLYRE-UHFFFAOYSA-M 2,4-Hexadienoic acid, potassium salt (1:1), (2E,4E)- Chemical compound [K+].CC=CC=CC([O-])=O CHHHXKFHOYLYRE-UHFFFAOYSA-M 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 235000011187 glycerol Nutrition 0.000 claims description 3
- 229940069338 potassium sorbate Drugs 0.000 claims description 3
- 235000010241 potassium sorbate Nutrition 0.000 claims description 3
- 239000004302 potassium sorbate Substances 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000012024 dehydrating agents Substances 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 3
- SRBFZHDQGSBBOR-LECHCGJUSA-N alpha-D-xylose Chemical compound O[C@@H]1CO[C@H](O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-LECHCGJUSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 229960003487 xylose Drugs 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a xylitol mother liquor crystallization method, belonging to the technical field of functional sugar production. The crystallization method adds three steps of dehydration promotion, room-temperature placement and freezing crystallization on the basis of the traditional crystallization method, adopts a dehydrating agent and a accelerator, and comprises the following specific technical steps: (1) prethickening; (2) dehydration promotion; (3) cooling crystallization; (4) displacing at room temperature; (5) freezing crystallization; (6) decentralizing; and (7) drying, packaging and the like. The crystallization method of the invention solves the problem of difficult crystallization of xylitol mother liquor, improves yield, fully utilizes raw materials, improves purity and quality of xylitol crystals, and improves the additional value of the xylitol mother liquor. The invention is also suitable for xylitol crystallization.
Description
Technical field
The invention belongs to technical field of functional sugar production, relate to a kind of crystallization method of Xylitol mother liquor.
Background technology
Xylitol is to be obtained by the wood sugar hydrogenation, and xylitol solution is through purification, evaporation, vacuum crystallization, the centrifugal xylitol crystal that obtains.The traditional vacuum crystallization method is that the massecuite pre-concentration is arrived hypersaturated state in the Xylitol production, adds crystal seed, vacuum cool-down crystallization, the centrifugal crystal that obtains.In the crystal Xylitol is produced, can produce a large amount of Xylitol mother liquors, Xylitol mother liquor is because impurity is many, purity is low, adopts the method for traditional vacuum crystallization can not obtain crystal, and Xylitol mother liquor can only use as liquid xylitol.Liquid xylitol brings very big inconvenience for storage and transportation, because purity is low, range of application also is restricted, and added value is lower.
Summary of the invention
To the deficiency of prior art, the present invention provides a kind of Xylitol mother liquor crystallization method, can not obtain crystal to solve prior art, can only use as liquid xylitol, because problem such as purity is low, and range of application also is restricted, and added value is lower.
The technical scheme that the present invention is adopted for its technical problem of solution provides a kind of crystallization method of new Xylitol mother liquor; Dehydration promotion, room temperature placement, three steps of freezing and crystallizing on the basis of conventional junction crystal method, have been increased; And added dewatering agent and promotor, this crystallization method is made up of following process step:
1, pre-concentration: with Xylitol mother liquor vacuum concentration to concentration is 75-95%.
2, dehydration promotes: the cooling of the massecuite behind step 1 pre-concentration is cooled to temperature when being 44-52 ℃; The 0.1-5% that presses massecuite unit weight adds one or both in glycerine, the absolute ethyl alcohol, press the 0.01-0.10% adding Sunmorl N 60S of massecuite dry weight, in the POTASSIUM SORBATE GRANULAR WHITE one or both.
3, decrease temperature crystalline: the mother liquor with step 2 has been handled well, be put into thermostatic water-circulator bath, about 45 ℃ of temperature, the 0.2-0.8% that presses the massecuite dry weight adds xylitol micro powders, decrease temperature crystalline 10-36 hour, proper extension temperature fall time.
4, room temperature is placed: the massecuite of step 3 decrease temperature crystalline is taken out water-bath, and room temperature was placed 16-32 hour, and massecuite bleaches, and crystal grain increases.
5, freezing and crystallizing: step 4 room temperature is placed later massecuite, be put in 4 ℃ of refrigerators freezing and crystallizing 8-72 hour.
6, centrifugal: the freezing and crystallizing massecuite is centrifugal, obtain crystal.
7, drying and packaging.
Adopt present method, solved the problem of Xylitol mother liquor crystallization difficulty, improved yield, raw material is fully used, improved the purity and the quality of xylitol crystal, improved the added value of Xylitol mother liquor.The present invention is equally applicable to the Xylitol crystallization.
Specific embodiment
Get Xylitol mother liquor 1000g, several kinds of different modes with reference to adding dewatering agent and promotor provide following practical implementation instance.
Embodiment 1
1, pre-concentration: get Xylitol mother liquor 1000g, vacuum concentration to concentration is 75%.
2, dehydration promotes: the cooling of the massecuite behind step 1 pre-concentration is cooled to temperature when being 50 ℃, adds absolute ethyl alcohol 0.58ml, add Sunmorl N 60S 0.14g.
3, decrease temperature crystalline: the mother liquor with step 2 has been handled well, be put into thermostatic water-circulator bath, when 44 ℃ of temperature, add xylitol micro powders 3.9g, decrease temperature crystalline 10 hours.
4, room temperature is placed: the massecuite of step 3 decrease temperature crystalline is taken out water-bath, and room temperature was placed 24 hours, and massecuite bleaches, and crystal grain increases.
5, freezing and crystallizing: step 4 room temperature is placed the later massecuite of crystallization, be put in 4 ℃ of refrigerators freezing and crystallizing 39 hours.
6, centrifugal: the freezing and crystallizing massecuite is centrifugal, obtain crystal.
7, drying and packaging.
Embodiment 2
1, pre-concentration: get Xylitol mother liquor 1000g, vacuum concentration to concentration is 78%.
2, dehydration promotes: the cooling of the massecuite behind step 1 pre-concentration is cooled to temperature when being 50 ℃, adds absolute ethyl alcohol 0.4ml, add glycerine 0.2ml, add Sunmorl N 60S 0.24g.
3, decrease temperature crystalline: the mother liquor with step 2 has been handled well, be put into thermostatic water-circulator bath, about 45 ℃ of temperature, add xylitol micro powders 3g, decrease temperature crystalline 11 hours.
4, room temperature is placed: the massecuite of step 3 decrease temperature crystalline is taken out water-bath, and room temperature was placed 15.5 hours, and massecuite bleaches, and crystal grain increases.
5, freezing and crystallizing: step 4 room temperature is placed later massecuite, be put in 4 ℃ of refrigerators freezing and crystallizing 16 hours.
6, centrifugal: the freezing and crystallizing massecuite is centrifugal, obtain crystal.
7, drying and packaging.
Embodiment 3
1, pre-concentration: get Xylitol mother liquor 1000g, vacuum concentration to concentration is 78%.
2, dehydration promotes: the cooling of the massecuite behind step 1 pre-concentration is cooled to temperature when being 45 ℃, adds absolute ethyl alcohol 44ml, add Sunmorl N 60S 0.1g.
3, decrease temperature crystalline: the mother liquor with step 2 has been handled well, be put into thermostatic water-circulator bath, when 44 ℃ of temperature, add xylitol micro powders 2.34g, decrease temperature crystalline 10 hours.
4, room temperature is placed: the massecuite of step 3 decrease temperature crystalline is taken out water-bath, and room temperature was placed 16 hours, and massecuite bleaches, and crystal grain increases.
5, freezing and crystallizing: step 4 room temperature is placed later massecuite, be put in 4 ℃ of refrigerators freezing and crystallizing 56 hours.
6, centrifugal: the freezing and crystallizing massecuite is centrifugal, obtain crystal.
7, drying and packaging.
Embodiment 4
1, pre-concentration: get Xylitol mother liquor 1000g, vacuum concentration to concentration is 80%.
2, dehydration promotes: the cooling of the massecuite behind step 1 pre-concentration is cooled to temperature when being 46 ℃, adds absolute ethyl alcohol 4ml, add Sunmorl N 60S 0.2g, add POTASSIUM SORBATE GRANULAR WHITE 0.07g.
3, decrease temperature crystalline: the mother liquor with step 2 has been handled well, be put into thermostatic water-circulator bath, when 46 ℃ of temperature, add xylitol micro powders 4.44g, decrease temperature crystalline 26 hours.
4, room temperature is placed: the massecuite of step 3 decrease temperature crystalline is taken out water-bath, and room temperature was placed 32 hours, and massecuite bleaches, and crystal grain increases.
5, freezing and crystallizing: step 4 room temperature is placed later massecuite, be put in 4 ℃ of refrigerators freezing and crystallizing 38 hours.
6, centrifugal: the freezing and crystallizing massecuite is centrifugal, obtain crystal.
7, drying and packaging.
Claims (1)
1. an Xylitol mother liquor crystallization method is characterized in that on the basis of conventional junction crystal method, having increased dehydration promotion, room temperature placement, three steps of freezing and crystallizing, and has added dewatering agent and promotor, and this crystallization method is made up of following process step:
(1) pre-concentration: with Xylitol mother liquor vacuum concentration to concentration is 75-95%;
(2) dehydration promotes: the cooling of the massecuite behind step 1 pre-concentration is cooled to temperature when being 44-52 ℃; The 0.1-5% that presses massecuite unit weight adds one or both in glycerine, the absolute ethyl alcohol, press the 0.01-0.10% adding Sunmorl N 60S of massecuite dry weight, in the POTASSIUM SORBATE GRANULAR WHITE one or both;
(3) decrease temperature crystalline: the mother liquor with step 2 has been handled well, be put into thermostatic water-circulator bath, 45 ℃ of temperature, the 0.2-0.8% that presses the massecuite dry weight adds xylitol micro powders, decrease temperature crystalline 10-36 hour;
(4) room temperature is placed: the massecuite of step 3 decrease temperature crystalline is taken out water-bath, and room temperature was placed 16-32 hour, and massecuite bleaches, and crystal grain increases;
(5) freezing and crystallizing: step 4 room temperature is placed later massecuite, be put in 4 ℃ of refrigerators freezing and crystallizing 8-72 hour;
(6) centrifugal: the freezing and crystallizing massecuite is centrifugal, obtain crystal;
(7) drying and packaging.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910014321A CN101810262B (en) | 2009-02-20 | 2009-02-20 | Xylitol mother liquor crystallization method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910014321A CN101810262B (en) | 2009-02-20 | 2009-02-20 | Xylitol mother liquor crystallization method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101810262A CN101810262A (en) | 2010-08-25 |
| CN101810262B true CN101810262B (en) | 2012-09-19 |
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| CN200910014321A Active CN101810262B (en) | 2009-02-20 | 2009-02-20 | Xylitol mother liquor crystallization method |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012133757A1 (en) * | 2011-03-31 | 2012-10-04 | 日本クラフトフーズ株式会社 | Flowable food composition and confection |
| CN108883400B (en) | 2016-02-19 | 2021-09-17 | 洲际大品牌有限责任公司 | Method for forming a multi-value stream from a biomass source |
| CN111777493B (en) * | 2020-08-29 | 2024-05-10 | 浙江华康药业股份有限公司 | Xylitol mother liquor utilization system and method |
| CN116063158B (en) * | 2022-12-17 | 2024-05-10 | 浙江华康药业股份有限公司 | Induction nucleation crystallization method for improving anti-caking performance of xylitol |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1733668A (en) * | 2005-07-20 | 2006-02-15 | 天津市圭谷科技发展有限公司 | Method for extracting xylitol from xylitol mother liquor |
| CN1736970A (en) * | 2005-07-25 | 2006-02-22 | 天津大学 | Xylitol refining crystallization process |
| CN101200407A (en) * | 2007-12-07 | 2008-06-18 | 胡学仁 | Method for abstracting xylitol from by-product liquid of xylitol production |
-
2009
- 2009-02-20 CN CN200910014321A patent/CN101810262B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1733668A (en) * | 2005-07-20 | 2006-02-15 | 天津市圭谷科技发展有限公司 | Method for extracting xylitol from xylitol mother liquor |
| CN1736970A (en) * | 2005-07-25 | 2006-02-22 | 天津大学 | Xylitol refining crystallization process |
| CN101200407A (en) * | 2007-12-07 | 2008-06-18 | 胡学仁 | Method for abstracting xylitol from by-product liquid of xylitol production |
Non-Patent Citations (2)
| Title |
|---|
| 侯宝红等.木糖醇结晶的热力学特性.《天津大学学报》.2006,第39卷(第4期),404-407. * |
| 靳冠娴等.从低木糖醇含量母液中提取晶体木糖醇的实验研究.《食品科技》.2008,(第6期),113-114. * |
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| CN101810262A (en) | 2010-08-25 |
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Effective date of registration: 20231114 Granted publication date: 20120919 |
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