CN102249855A - Process for preparing erythritol - Google Patents
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Abstract
一种赤藓糖醇制备工艺,属于功能糖生产技术领域该工艺使用活性炭脱色技术,脱蛋白、脱小分子物质的专用活性炭和阴阳离子交换树脂对发酵液进行精制提纯,其工艺步骤包括:(1)透析液制备、(2)脱色、(3)除味、(4)净化、(5)蒸发、(6)结晶、(7)结晶、分离、烘干得到结晶赤藓糖醇。本发明缩短了生产周期,提高了工作效率;较少了生产中蒸汽、电的消耗,降低了生产成本;发酵液经精制提纯后再浓缩结晶,减少了料液中的杂质,有利于提高结晶收率和产品质量,可以提高分离后的母液质量及再利用性,降低生产成本。A process for preparing erythritol, which belongs to the technical field of functional sugar production. The process uses activated carbon decolorization technology, special activated carbon for deproteinization and small molecule removal, and anion and cation exchange resins to refine and purify the fermentation broth. The process steps include: ( 1) Dialysate preparation, (2) decolorization, (3) deodorization, (4) purification, (5) evaporation, (6) crystallization, (7) crystallization, separation, and drying to obtain crystalline erythritol. The invention shortens the production cycle, improves the work efficiency; reduces the consumption of steam and electricity in the production, and reduces the production cost; Yield and product quality can improve the quality and reusability of the mother liquor after separation, and reduce production costs.
Description
技术领域 technical field
本发明属于功能糖生产技术领域,具体涉及到一种赤藓糖醇发酵液的精制、结晶工艺。 The invention belongs to the technical field of functional sugar production, and in particular relates to a process for refining and crystallizing erythritol fermentation liquid.
背景技术 Background technique
赤藓糖醇是一种甜度为蔗糖的60~80%的无热量四碳多元糖。由于赤藓糖醇具有低能量值、高耐受量、无毒副作用、糖尿病人可食用及非致龋齿性等优越特性,近年来被应用在低糖、保健等功能性食品中。目前,赤藓糖醇的工业制备方法主要为微生物发酵法,它的生产方法是以葡萄糖为原料,由高渗酵母经发酵得到赤藓糖醇发酵液,发酵液经陶瓷膜或板式过滤机过滤除去酵母,再经过蒸发浓缩、结晶得到赤藓糖醇粗晶体,然后将粗晶体用淡水溶解,经活性炭脱色、离子交换树脂精制提纯、蒸发、结晶、分离得到成品赤藓糖醇。目前这种生产方法,要经过两次结晶才能得到成品赤藓糖醇,生产周期长、蒸汽消耗量大;且赤藓糖醇发酵液除去酵母后不经过精制提纯直接蒸发浓缩,结晶,结晶收率低,结晶母液颜色深、粘度大,不能再次利用,导致整体收率低,不超过75%。 Erythritol is a non-caloric four-carbon polysaccharide with a sweetness of 60-80% of sucrose. Erythritol has been used in low-sugar, health-care and other functional foods in recent years due to its superior characteristics such as low energy value, high tolerance, no toxic side effects, edible for diabetics and non-cariogenic properties. At present, the industrial preparation method of erythritol is mainly microbial fermentation method. Its production method uses glucose as raw material to obtain erythritol fermentation liquid by fermentation of hyperosmotic yeast, and the fermentation liquid is filtered by ceramic membrane or plate filter. Yeast is removed, then concentrated by evaporation and crystallized to obtain crude crystals of erythritol, and then the crude crystals are dissolved in fresh water, decolorized by activated carbon, purified by ion exchange resin, evaporated, crystallized, and separated to obtain finished erythritol. At present, this production method requires two crystallizations to obtain the finished erythritol, which has a long production cycle and large steam consumption; and the erythritol fermentation liquid is directly evaporated and concentrated without refining and purifying after the yeast is removed, crystallized, and crystallized. The yield is low, the crystallization mother liquor is dark in color and high in viscosity, and cannot be reused, resulting in a low overall yield of no more than 75%.
发明内容 Contents of the invention
本发明旨在提供一种赤藓糖醇制备工艺,以解决现有技术制备工艺复杂,生产周期长、蒸汽消耗量大、收率低结晶母液颜色深、粘度大,不能再次利用等问题。 The present invention aims to provide a preparation process of erythritol to solve the problems of complex preparation process, long production cycle, large steam consumption, low yield and low crystallization mother liquor in the prior art, which has deep color, high viscosity and cannot be reused.
本发明解决其技术问题所采用的技术方案是使用活性炭脱色技术,脱蛋白、脱小分子物质的专用活性炭和阴阳离子交换树脂对发酵液进行精制提纯,可以去除赤藓糖醇发酵液的色素、蛋白、胶体及阴、阳离子等杂质,使得藓糖醇发酵液可以通过一次结晶就得到成品赤藓糖醇。其工艺步骤如下: The technical solution adopted by the present invention to solve its technical problems is to use activated carbon decolorization technology, special activated carbon and anion-cation exchange resin for deproteinization and removal of small molecular substances to refine and purify the fermented liquid, which can remove the pigment, erythritol fermented liquid, Impurities such as proteins, colloids, anions, and cations make it possible to obtain finished erythritol through one-time crystallization of the thiritol fermentation broth. Its process steps are as follows:
1、透析液制备:以葡萄糖为原料,经高渗酵母发酵得到的发酵液,经过陶瓷膜过滤去除酵母,得到透析液; 1. Preparation of dialysate: use glucose as raw material, ferment the fermented liquid with hyperosmotic yeast, filter through ceramic membrane to remove yeast, and obtain dialysate;
2、脱色:透析液在40℃~75℃下,按0.1%~1%(w/v)加入普通糖醇用活性炭进行脱色,脱色时间20min~80min,过滤分离得到一次脱色液; 2. Decolorization: the dialysate is decolorized by adding ordinary sugar alcohols at 0.1%~1% (w/v) and activated carbon at 40°C~75°C. The decolorization time is 20min~80min, and the decolorization solution is obtained by filtration and separation;
3、除味:一次脱色液在40℃~75℃下,按0.02%~0.1%(w/v)加入脱蛋白、脱小分子物质的专用活性炭进行蛋白质、颜色前提等小分子物质的脱除,脱色时间20min~80min,过滤分离得到二次脱色液; 3. Deodorization: Add 0.02%~0.1% (w/v) special activated carbon for deproteinization and removal of small molecular substances to the primary decolorization solution at 40°C~75°C to remove small molecular substances such as protein and color prerequisites , the decolorization time is 20min~80min, and the secondary decolorization solution is obtained by filtration and separation;
4、净化:二次脱色液按照阴—阳—阴的工艺流程进行离子交换,进一步对赤藓糖醇料液进行精制提纯,要求经过离子交换的料液透光率≥99.8%,电导率≤10μs/cm; 4. Purification: The secondary decolorization solution is ion-exchanged according to the process flow of Yin-Yang-Yin, and the erythritol feed liquid is further refined and purified. It is required that the light transmittance of the feed liquid after ion exchange is ≥99.8%, and the conductivity is ≤ 10μs/cm;
5、蒸发:将赤藓糖醇料液蒸发浓缩至折光浓度55%~75%; 5. Evaporation: Evaporate and concentrate the erythritol feed solution to a refractive concentration of 55%~75%;
6、结晶:赤藓糖醇结晶采用梯度降温结晶,起始温度为65℃~75℃,降温速度为0.5℃~10℃/hr; 6. Crystallization: Erythritol crystallization adopts gradient cooling crystallization, the initial temperature is 65°C~75°C, and the cooling rate is 0.5°C~10°C/hr;
7、分离烘干:结晶糖膏经离心机分离、烘干得到结晶赤藓糖醇。 7. Separation and drying: the crystalline massecuite is separated and dried by a centrifuge to obtain crystalline erythritol.
上述4中所指的阴、阳离子树脂可用所有离子交换树脂。 All ion exchange resins can be used for the anion and cation resins referred to in the above 4.
本发明的有益效果是:缩短了生产周期,有利于提高工作效率;较少了生产中蒸汽、电的消耗,有利于降低生产成本;发酵液经精制提纯再在浓缩结晶,减少了料液中的杂质,有利于提高结晶收率,更有利于提高产品质量,另外可以提高分离后的母液质量,提高其可再利用性,对降低生产成本有很大帮助。 The beneficial effects of the present invention are: the production cycle is shortened, which is conducive to improving work efficiency; the consumption of steam and electricity in production is reduced, which is conducive to reducing production costs; The impurities are beneficial to increase the crystallization yield and product quality. In addition, it can improve the quality of the separated mother liquor and improve its reusability, which is of great help to reduce production costs.
具体实施方式 Detailed ways
本发明的优选实施方案是使用活性炭脱色技术,脱蛋白、脱小分子物质的专用活性炭和阴阳离子交换树脂对发酵液进行精制提纯,具体工艺步骤如下: The preferred embodiment of the present invention is to use active carbon decolorization technology, special active carbon and anion and cation exchange resin for deproteinization and removal of small molecular substances to refine and purify the fermented liquid, and the specific process steps are as follows:
1、以葡萄糖为原料,经高渗酵母发酵得到的发酵液,经过陶瓷膜过滤去除酵母,得到透析液,透析液折光16%; 1. Using glucose as raw material, the fermented liquid obtained by fermenting hyperosmotic yeast is filtered through a ceramic membrane to remove yeast to obtain dialysate, which has a refractive index of 16%;
2、脱色:透析液在62℃下,按0.5%(w/v)加入普通糖醇用活性炭进行脱色,脱色时间45min,过滤分离得到一次脱色液,脱色液透光率79.8%; 2. Decolorization: The dialysate is decolorized by adding ordinary sugar alcohol at 0.5% (w/v) with activated carbon at 62°C. The decolorization time is 45 minutes, and the decolorization solution is obtained by filtration and separation. The light transmittance of the decolorization solution is 79.8%;
3、除味:一次脱色液在55℃下,按0.05%(w/v)加入脱蛋白、脱小分子物质的专用活性炭进行蛋白质、颜色前提等小分子物质的脱除,脱色时间40min,过滤分离得到二次脱色液; 3. Deodorization: Add 0.05% (w/v) special activated carbon for deproteinization and removal of small molecular substances to the primary decolorization solution at 55°C to remove small molecular substances such as protein and color prerequisites. The decolorization time is 40 minutes and filtered Separation obtains secondary decolorization liquid;
4、净化:二次脱色液按照D301——001*7——D301的工艺流程进行离子交换,进一步对赤藓糖醇料液进行精制提纯,交换液透光率100%,电导率5μs/cm; 4. Purification: The secondary decolorization liquid is ion-exchanged according to the process flow of D301——001*7——D301, and the erythritol feed liquid is further refined and purified. The light transmittance of the exchange liquid is 100%, and the conductivity is 5 μs/cm ;
5、蒸发:将赤藓糖醇料液蒸发浓缩至折光浓度63%; 5. Evaporation: Evaporate and concentrate the erythritol feed solution to a refractive concentration of 63%;
6、结晶:赤藓糖醇结晶采用梯度降温结晶,起始温度为68℃,降温速度为8℃/hr; 6. Crystallization: Erythritol crystallization adopts gradient cooling crystallization, the initial temperature is 68°C, and the cooling rate is 8°C/hr;
7、分离烘干:结晶糖膏经离心机分离、烘干得到结晶赤藓糖醇。结晶收率86.7%。 7. Separation and drying: the crystalline massecuite is separated and dried by a centrifuge to obtain crystalline erythritol. The crystallization yield was 86.7%.
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102826959A (en) * | 2012-09-26 | 2012-12-19 | 山东福田药业有限公司 | Method for extracting erythritol from erythritol mother liquor |
CN102826958A (en) * | 2012-09-26 | 2012-12-19 | 山东福田药业有限公司 | Treatment method of erythritol mother liquor |
CN102839202A (en) * | 2012-09-26 | 2012-12-26 | 山东福田药业有限公司 | Method for processing erythritol fermentation liquor |
CN103373901A (en) * | 2013-07-05 | 2013-10-30 | 上海交通大学 | Method for extracting erythritol from erythritol mother liquor and special barm strain for erythritol |
CN103524303A (en) * | 2013-10-28 | 2014-01-22 | 武汉科技大学 | Method of auxiliary judging seed crystal adding time in erythritol crystallizing process based on specific gravity |
CN104086365A (en) * | 2014-06-30 | 2014-10-08 | 山东省食品发酵工业研究设计院 | Method for preparing mixed sugar alcohol product by reutilizing erythritol production mother solution |
CN106748657A (en) * | 2016-11-30 | 2017-05-31 | 山东福田药业有限公司 | A kind of processing method of fermented erythritol liquor |
WO2023124396A1 (en) * | 2021-12-29 | 2023-07-06 | 浙江华康药业股份有限公司 | Refinement system for xylitol fermented liquid, and method therefor |
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CN101085720A (en) * | 2007-06-15 | 2007-12-12 | 淄博中舜生物技术有限公司 | Purification method for erythritol fermentation liquor |
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Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102826959A (en) * | 2012-09-26 | 2012-12-19 | 山东福田药业有限公司 | Method for extracting erythritol from erythritol mother liquor |
CN102826958A (en) * | 2012-09-26 | 2012-12-19 | 山东福田药业有限公司 | Treatment method of erythritol mother liquor |
CN102839202A (en) * | 2012-09-26 | 2012-12-26 | 山东福田药业有限公司 | Method for processing erythritol fermentation liquor |
CN102826958B (en) * | 2012-09-26 | 2014-07-30 | 山东福田药业有限公司 | Treatment method of erythritol mother liquor |
CN103373901A (en) * | 2013-07-05 | 2013-10-30 | 上海交通大学 | Method for extracting erythritol from erythritol mother liquor and special barm strain for erythritol |
CN103524303A (en) * | 2013-10-28 | 2014-01-22 | 武汉科技大学 | Method of auxiliary judging seed crystal adding time in erythritol crystallizing process based on specific gravity |
CN104086365A (en) * | 2014-06-30 | 2014-10-08 | 山东省食品发酵工业研究设计院 | Method for preparing mixed sugar alcohol product by reutilizing erythritol production mother solution |
CN104086365B (en) * | 2014-06-30 | 2016-05-18 | 山东省食品发酵工业研究设计院 | A kind of method of being prepared by antierythrite production mother liquor recycling to mixing sugar alcohol product |
CN106748657A (en) * | 2016-11-30 | 2017-05-31 | 山东福田药业有限公司 | A kind of processing method of fermented erythritol liquor |
WO2023124396A1 (en) * | 2021-12-29 | 2023-07-06 | 浙江华康药业股份有限公司 | Refinement system for xylitol fermented liquid, and method therefor |
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