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CN101810262B - Xylitol mother liquor crystallization method - Google Patents

Xylitol mother liquor crystallization method Download PDF

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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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massecuite
xylitol
mother liquor
crystallization
room temperature
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CN101810262A (en
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田强
杜瑞锋
王成福
周娟
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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 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

木糖醇母液结晶方法Xylitol mother liquor crystallization method

技术领域 technical field

本发明属于功能糖生产技术领域,涉及一种木糖醇母液的结晶方法。The invention belongs to the technical field of functional sugar production and relates to a crystallization method of xylitol mother liquor.

背景技术 Background technique

木糖醇是由木糖加氢得到,木糖醇溶液经净化、蒸发、真空结晶、离心得到木糖醇晶体。木糖醇生产中传统真空结晶方法是将糖膏预浓缩到过饱和状态,加入晶种,真空降温结晶,离心得到晶体。在晶体木糖醇生产中会产生大量的木糖醇母液,木糖醇母液由于杂质多、纯度低,采用传统的真空结晶的方法不能得到晶体,木糖醇母液只能作为液体木糖醇使用。液体木糖醇给储存和运输带来很大不方便,由于纯度低,应用范围也受到限制,附加值较低。Xylitol is obtained by hydrogenating xylose, and the xylitol solution is purified, evaporated, vacuum crystallized, and centrifuged to obtain xylitol crystals. The traditional vacuum crystallization method in xylitol production is to pre-concentrate massecuite to a supersaturated state, add seed crystals, cool down in vacuum to crystallize, and centrifuge to obtain crystals. In the production of crystal xylitol, a large amount of xylitol mother liquor will be produced. Due to the many impurities and low purity of xylitol mother liquor, crystals cannot be obtained by traditional vacuum crystallization methods. Xylitol mother liquor can only be used as liquid xylitol. . Liquid xylitol brings great inconvenience to storage and transportation. Due to its low purity, its application range is also limited and its added value is low.

发明内容 Contents of the invention

针对现有技术的不足,本发明提供一种木糖醇母液结晶方法,以解决现有技术不能得到晶体,只能作为液体木糖醇使用,由于纯度低,应用范围也受到限制,附加值较低等问题。Aiming at the deficiencies in the prior art, the present invention provides a method for crystallization of xylitol mother liquor to solve the problem that the prior art cannot obtain crystals and can only be used as liquid xylitol. Due to the low purity, the scope of application is also limited, and the added value is relatively high. Inferior question.

本发明为解决其技术问题所采用的技术方案是提供一种新的木糖醇母液的结晶方法,在传统结晶方法的基础上增加了脱水促进、室温放置、冷冻结晶三步,并且添加了脱水剂和促进剂,该结晶方法由以下工艺步骤组成:The technical scheme adopted by the present invention to solve its technical problems is to provide a new crystallization method of xylitol mother liquor, which adds three steps of dehydration promotion, room temperature placement, and freezing crystallization on the basis of the traditional crystallization method, and adds dehydration agent and accelerator, the crystallization method consists of the following process steps:

1、预浓缩:将木糖醇母液真空浓缩至浓度为75-95%。1. Pre-concentration: vacuum concentrate the xylitol mother liquor to a concentration of 75-95%.

2、脱水促进:将步骤1预浓缩后的糖膏降温冷却至温度为44-52℃时,按糖膏容重的0.1-5%加入甘油、无水乙醇中的一种或两种,按糖膏干重的0.01-0.10%加入葡萄糖酸钠、山梨酸钾中的一种或两种。2. Dehydration promotion: when the pre-concentrated massecuite in step 1 is cooled to a temperature of 44-52°C, one or both of glycerin and absolute ethanol are added according to 0.1-5% of the massecuite’s bulk density. One or both of sodium gluconate and potassium sorbate are added to 0.01-0.10% of the dry weight of the paste.

3、降温结晶:将步骤2已处理好的母液,放到超级恒温水浴,在温度45℃左右,按糖膏干重的0.2-0.8%加入木糖醇微粉,降温结晶10-36小时,适当延长降温时间。3. Cooling and crystallization: Put the mother liquor treated in step 2 into a super constant temperature water bath, add xylitol micropowder according to 0.2-0.8% of the dry weight of the massecuite at a temperature of about 45°C, cool down and crystallize for 10-36 hours, appropriate Extend cooling time.

4、室温放置:将步骤3降温结晶的糖膏拿出水浴,室温放置16-32小时,糖膏变白,晶粒增多。4. Place at room temperature: Take the massecuite crystallized in step 3 out of the water bath, and place it at room temperature for 16-32 hours. The massecuite turns white and the crystal grains increase.

5、冷冻结晶:将步骤4室温放置以后的糖膏,放到4℃冰箱中,冷冻结晶8-72小时。5. Freezing and crystallization: Put the massecuite after standing at room temperature in step 4 into a refrigerator at 4°C, and freeze and crystallize for 8-72 hours.

6、离心:将冷冻结晶糖膏离心,得到晶体。6. Centrifugation: Centrifuge the frozen crystal massecuite to obtain crystals.

7、烘干包装。7. Dry the package.

采用本方法,解决了木糖醇母液结晶困难的问题,提高了收率,使原料得到充分利用,提高了木糖醇晶体的纯度和质量,提高了木糖醇母液的附加值。本发明同样适用于木糖醇结晶。By adopting the method, the problem of difficult crystallization of the xylitol mother liquor is solved, the yield is increased, the raw materials are fully utilized, the purity and quality of the xylitol crystals are improved, and the added value of the xylitol mother liquor is increased. The present invention is equally applicable to xylitol crystallization.

具体实施例specific embodiment

取木糖醇母液1000g,参照添加脱水剂和促进剂的几种不同方式,提供以下具体实施实例。Get xylitol mother liquor 1000g, refer to several different ways of adding dehydrating agent and accelerator, provide the following specific implementation examples.

实施例1Example 1

1、预浓缩:取木糖醇母液1000g,真空浓缩至浓度为75%。1. Pre-concentration: Take 1000 g of the xylitol mother liquor and concentrate it in vacuum to a concentration of 75%.

2、脱水促进:将步骤1预浓缩后的糖膏降温冷却至温度为50℃时,加入无水乙醇0.58ml,加入葡萄糖酸钠0.14g。2. Acceleration of dehydration: When the pre-concentrated massecuite in step 1 is cooled down to 50°C, add 0.58ml of absolute ethanol and 0.14g of sodium gluconate.

3、降温结晶:将步骤2已处理好的母液,放到超级恒温水浴,在温度44℃时,加入木糖醇微粉3.9g,降温结晶10小时。3. Cooling and crystallization: put the mother liquor treated in step 2 into a super constant temperature water bath, add 3.9g of xylitol micropowder at a temperature of 44°C, and cool and crystallize for 10 hours.

4、室温放置:将步骤3降温结晶的糖膏拿出水浴,室温放置24小时,糖膏变白,晶粒增多。4. Place at room temperature: Take the massecuite crystallized in step 3 out of the water bath, and place it at room temperature for 24 hours. The massecuite turns white and the crystal grains increase.

5、冷冻结晶:将步骤4室温放置结晶以后的糖膏,放到4℃冰箱中,冷冻结晶39小时。5. Freezing and crystallization: Put the massecuite after crystallization at room temperature in step 4 into a refrigerator at 4°C, and freeze and crystallize for 39 hours.

6、离心:将冷冻结晶糖膏离心,得到晶体。6. Centrifugation: Centrifuge the frozen crystal massecuite to obtain crystals.

7、烘干包装。7. Dry the package.

实施例2Example 2

1、预浓缩:取木糖醇母液1000g,真空浓缩至浓度为78%。1. Pre-concentration: Take 1000 g of the xylitol mother liquor and concentrate it in vacuum to a concentration of 78%.

2、脱水促进:将步骤1预浓缩后的糖膏降温冷却至温度为50℃时,加入无水乙醇0.4ml,加入甘油0.2ml,加入葡萄糖酸钠0.24g。2. Acceleration of dehydration: When the pre-concentrated massecuite in step 1 is cooled to 50°C, add 0.4 ml of absolute ethanol, 0.2 ml of glycerin, and 0.24 g of sodium gluconate.

3、降温结晶:将步骤2已处理好的母液,放到超级恒温水浴,在温度45℃左右,加入木糖醇微粉3g,降温结晶11小时。3. Cooling and crystallization: Put the mother liquor treated in step 2 into a super constant temperature water bath, add 3g of xylitol micropowder at a temperature of about 45°C, and cool down and crystallize for 11 hours.

4、室温放置:将步骤3降温结晶的糖膏拿出水浴,室温放置15.5小时,糖膏变白,晶粒增多。4. Place at room temperature: Take the massecuite crystallized in step 3 out of the water bath, and place it at room temperature for 15.5 hours. The massecuite turns white and the crystal grains increase.

5、冷冻结晶:将步骤4室温放置以后的糖膏,放到4℃冰箱中,冷冻结晶16小时。5. Freezing and crystallization: Put the massecuite after standing at room temperature in step 4 into a refrigerator at 4°C, and freeze and crystallize for 16 hours.

6、离心:将冷冻结晶糖膏离心,得到晶体。6. Centrifugation: Centrifuge the frozen crystal massecuite to obtain crystals.

7、烘干包装。7. Dry the package.

实施例3Example 3

1、预浓缩:取木糖醇母液1000g,真空浓缩至浓度为78%。1. Pre-concentration: Take 1000 g of the xylitol mother liquor and concentrate it in vacuum to a concentration of 78%.

2、脱水促进:将步骤1预浓缩后的糖膏降温冷却至温度为45℃时,加入无水乙醇44ml,加入葡萄糖酸钠0.1g。2. Acceleration of dehydration: When the pre-concentrated massecuite in step 1 is cooled to a temperature of 45°C, add 44ml of absolute ethanol and 0.1g of sodium gluconate.

3、降温结晶:将步骤2已处理好的母液,放到超级恒温水浴,在温度44℃时,加入木糖醇微粉2.34g,降温结晶10小时。3. Cooling and crystallization: Put the mother liquor treated in step 2 into a super constant temperature water bath, add 2.34g of xylitol micropowder at a temperature of 44°C, and cool down and crystallize for 10 hours.

4、室温放置:将步骤3降温结晶的糖膏拿出水浴,室温放置16小时,糖膏变白,晶粒增多。4. Place at room temperature: Take the massecuite crystallized in step 3 out of the water bath, and place it at room temperature for 16 hours. The massecuite turns white and the crystal grains increase.

5、冷冻结晶:将步骤4室温放置以后的糖膏,放到4℃冰箱中,冷冻结晶56小时。5. Freezing and crystallization: Put the massecuite after standing at room temperature in step 4 into a refrigerator at 4°C, and freeze and crystallize for 56 hours.

6、离心:将冷冻结晶糖膏离心,得到晶体。6. Centrifugation: Centrifuge the frozen crystal massecuite to obtain crystals.

7、烘干包装。7. Dry the package.

实施例4Example 4

1、预浓缩:取木糖醇母液1000g,真空浓缩至浓度为80%。1. Pre-concentration: Take 1000 g of the xylitol mother liquor and concentrate it in vacuum to a concentration of 80%.

2、脱水促进:将步骤1预浓缩后的糖膏降温冷却至温度为46℃时,加入无水乙醇4ml,加入葡萄糖酸钠0.2g,加入山梨酸钾0.07g。2. Acceleration of dehydration: When the pre-concentrated massecuite in step 1 is cooled to 46°C, add 4ml of absolute ethanol, 0.2g of sodium gluconate, and 0.07g of potassium sorbate.

3、降温结晶:将步骤2已处理好的母液,放到超级恒温水浴,在温度46℃时,加入木糖醇微粉4.44g,降温结晶26小时。3. Cooling and crystallization: put the mother liquor treated in step 2 into a super constant temperature water bath, add 4.44g of xylitol micropowder at a temperature of 46°C, and cool down and crystallize for 26 hours.

4、室温放置:将步骤3降温结晶的糖膏拿出水浴,室温放置32小时,糖膏变白,晶粒增多。4. Place at room temperature: Take the massecuite crystallized in step 3 out of the water bath, and place it at room temperature for 32 hours. The massecuite turns white and the crystal grains increase.

5、冷冻结晶:将步骤4室温放置以后的糖膏,放到4℃冰箱中,冷冻结晶38小时。5. Freezing and crystallization: Put the massecuite after standing at room temperature in step 4 into a refrigerator at 4°C, and freeze and crystallize for 38 hours.

6、离心:将冷冻结晶糖膏离心,得到晶体。6. Centrifugation: Centrifuge the frozen crystal massecuite to obtain crystals.

7、烘干包装。7. Dry the package.

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.
CN200910014321A 2009-02-20 2009-02-20 Xylitol mother liquor crystallization method Active CN101810262B (en)

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MX342980B (en) * 2011-03-31 2016-10-20 Mondelez Japan Ltd Flowable food composition and confection.
JP6774494B2 (en) 2016-02-19 2020-10-21 インターコンチネンタル グレート ブランズ エルエルシー Process for forming multiple useful streams 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

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