WO2022247197A1 - 利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的系统及方法 - Google Patents

利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的系统及方法 Download PDF

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WO2022247197A1
WO2022247197A1 PCT/CN2021/134594 CN2021134594W WO2022247197A1 WO 2022247197 A1 WO2022247197 A1 WO 2022247197A1 CN 2021134594 W CN2021134594 W CN 2021134594W WO 2022247197 A1 WO2022247197 A1 WO 2022247197A1
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nanofiltration
erythritol
tank
glucose
dialysate
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PCT/CN2021/134594
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English (en)
French (fr)
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郑毅
吴爱娟
方顺成
廖承军
陈兰兰
罗家星
胡昌辉
曾方明
李勉
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浙江华康药业股份有限公司
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Priority to EP21942760.6A priority Critical patent/EP4186979A4/en
Priority to JP2023509724A priority patent/JP7454103B2/ja
Priority to US18/024,090 priority patent/US20230313236A1/en
Publication of WO2022247197A1 publication Critical patent/WO2022247197A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/78—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by condensation or crystallisation
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P7/00—Preparation of oxygen-containing organic compounds
    • C12P7/02—Preparation of oxygen-containing organic compounds containing a hydroxy group
    • C12P7/04—Preparation of oxygen-containing organic compounds containing a hydroxy group acyclic
    • C12P7/18—Preparation of oxygen-containing organic compounds containing a hydroxy group acyclic polyhydric
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
    • B01D61/027—Nanofiltration
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/132—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12M—APPARATUS FOR ENZYMOLOGY OR MICROBIOLOGY; APPARATUS FOR CULTURING MICROORGANISMS FOR PRODUCING BIOMASS, FOR GROWING CELLS OR FOR OBTAINING FERMENTATION OR METABOLIC PRODUCTS, i.e. BIOREACTORS OR FERMENTERS
    • C12M29/00—Means for introduction, extraction or recirculation of materials, e.g. pumps
    • C12M29/04—Filters; Permeable or porous membranes or plates, e.g. dialysis
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12M—APPARATUS FOR ENZYMOLOGY OR MICROBIOLOGY; APPARATUS FOR CULTURING MICROORGANISMS FOR PRODUCING BIOMASS, FOR GROWING CELLS OR FOR OBTAINING FERMENTATION OR METABOLIC PRODUCTS, i.e. BIOREACTORS OR FERMENTERS
    • C12M43/00—Combinations of bioreactors or fermenters with other apparatus
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00—Preparation of compounds containing saccharide radicals
    • C12P19/02—Monosaccharides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2311/00—Details relating to membrane separation process operations and control
    • B01D2311/04—Specific process operations in the feed stream; Feed pretreatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2311/00—Details relating to membrane separation process operations and control
    • B01D2311/06—Specific process operations in the permeate stream
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2311/00—Details relating to membrane separation process operations and control
    • B01D2311/08—Specific process operations in the concentrate stream
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2311/00—Details relating to membrane separation process operations and control
    • B01D2311/26—Further operations combined with membrane separation processes
    • B01D2311/2623—Ion-Exchange
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2311/00—Details relating to membrane separation process operations and control
    • B01D2311/26—Further operations combined with membrane separation processes
    • B01D2311/263—Chemical reaction
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2311/00—Details relating to membrane separation process operations and control
    • B01D2311/26—Further operations combined with membrane separation processes
    • B01D2311/2643—Crystallisation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2311/00—Details relating to membrane separation process operations and control
    • B01D2311/26—Further operations combined with membrane separation processes
    • B01D2311/2649—Filtration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2311/00—Details relating to membrane separation process operations and control
    • B01D2311/26—Further operations combined with membrane separation processes
    • B01D2311/2673—Evaporation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2311/00—Details relating to membrane separation process operations and control
    • B01D2311/26—Further operations combined with membrane separation processes
    • B01D2311/2688—Biological processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
    • B01D61/04—Feed pretreatment
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency

Definitions

  • the invention belongs to the technical field of sugar alcohol preparation, in particular to a system and method for co-producing erythritol and liquid sorbitol by using corn starch.
  • Erythritol has been widely used in food, beverage and other industries. At present, most of the methods for industrialized preparation of erythritol are obtained from glucose as raw material through microbial fermentation, and glucose is usually obtained from starch through liquefaction, saccharification, and then refining, concentration and crystallization. The integration of glucose and erythritol production processes will be more conducive to the utilization of resources and energy.
  • the Chinese patent with the publication number CN102154383A introduces a method for producing erythritol by using corn flour. Corn starch is directly used as raw material, and after liquefaction and saccharification, fermentable glucose is obtained.
  • the technical problem to be solved by the present invention is to provide a system and method for co-producing erythritol and liquid sorbitol by using cornstarch.
  • the glucose solution obtained after liquefaction and saccharification is prepared by nanofiltration. Erythritol and liquid sorbitol two products.
  • the present invention is achieved by providing a system for co-producing erythritol and liquid sorbitol using cornstarch, including a liquefaction tank, a saccharification tank, a filter and a nanofiltration assembly, and the liquefaction tank is used to liquefy cornstarch , the saccharification tank is used to saccharify the liquefied material, the filter is used to filter the impurities in the saccharified material to obtain glucose solution, and the nanofiltration component performs nanofiltration treatment on the filtered glucose solution to obtain dialysate and concentrated solution, the system also includes a fermentation and crystallization component for fermenting and crystallizing the dialysate to prepare crystalline erythritol, and a hydrogenation evaporation component for hydrogenating and evaporating the concentrated solution to prepare liquid sorbitol .
  • a system for co-producing erythritol and liquid sorbitol using cornstarch including a liquefaction tank, a saccharification tank,
  • the nanofiltration assembly includes a buffer tank, a feed pump, a pre-nanofiltration filter, a high-pressure pump, and a nanofiltration membrane assembly composed of a nanofiltration membrane and a circulation pump that are sequentially connected through pipelines, and are filtered before the nanofiltration
  • the glucose solution filtered by the filter is subjected to the nanofiltration treatment of the nanofiltration membrane module to obtain the dialysate and the concentrated solution respectively.
  • the fermentation crystallization component includes a fermenter, a membrane filter, a crystallization component and a recrystallization component
  • the fermenter is used to convert the glucose component in the dialysate into erythritol after fermentation
  • the membrane filter is used to remove the fermented Impurities in the processed material
  • the crystallization component and the recrystallization component are used to crystallize the material filtered by the membrane filter to obtain crystal erythritol.
  • the hydrogenation evaporation assembly includes a hydrogenation tank, an ion exchanger and an evaporation tank, the hydrogenation tank is used to convert the glucose component in the concentrated liquid into sorbitol after hydrogenation treatment, and the ion exchanger and the evaporation tank are used to convert the hydrogenation tank
  • the hydrotreated material is purified to obtain liquid sorbitol.
  • the present invention is achieved in this way, also provides a kind of method utilizing corn starch to co-produce erythritol and liquid sorbitol, it has used the system utilizing corn starch to co-produce erythritol and liquid sorbitol as described above , the method includes the following steps:
  • Step 1 Liquefying, saccharifying and filtering the cornstarch to obtain a glucose solution with a solids concentration of 33% to 35%. In the solids, the purity of glucose is 95.0% to 96.3%;
  • Step 2 subjecting the obtained glucose solution to nanofiltration treatment to obtain dialysate and concentrate respectively, in the dialysate, the purity of glucose is 99.0% ⁇ 99.5%, in the concentrate, the purity of glucose is 80.0% ⁇ 86.0%;
  • Step 3 Process the obtained dialysate through fermentation, membrane filtration, crystallization, recrystallization and other processes to obtain crystalline erythritol.
  • the purity of erythritol is >99.5%.
  • the obtained concentrated solution is hydrogenated, ion exchanged and evaporated. After other processes, liquid sorbitol is obtained, and the purity of sorbitol is more than 80%.
  • step one the temperature of the glucose solution is 50°C-60°C, and the pH value is 4.0-5.0.
  • the nanofiltration treatment includes entering the obtained glucose solution into the buffer tank, and then passing through the pre-nanofiltration filter through the feed pump, and then the filtered glucose solution enters the filter by the nanofiltration membrane through the high-pressure pump.
  • the nanofiltration is carried out in the nanofiltration module composed of the circulating pump and the nanofiltration treatment. After the nanofiltration treatment, the dialysate that passes through the nanofiltration membrane and the concentrated solution that does not pass through the nanofiltration membrane are respectively obtained.
  • the nanofiltration treatment also includes using the cleaning water in the cleaning tank to regularly clean the nanofiltration membrane through a cleaning pump.
  • the operating temperature of the nanofiltration assembly is 40°C ⁇ 60°C, and the operating pressure is 15bar ⁇ 35bar.
  • Step 3 the dialysate is evaporated by heat exchange to 35% dry matter concentration before undergoing fermentation treatment.
  • the system and method for co-producing erythritol and liquid sorbitol using cornstarch of the present invention uses cornstarch as a raw material to obtain glucose liquid after liquefaction and saccharification, and then nanofiltration treatment
  • the obtained dialysate with a glucose content of more than 99% is used for fermentation to prepare erythritol.
  • the dry basis concentration of erythritol in the fermentation broth can be improved, not only can Improve the fermentation yield, and also facilitate the subsequent purification of the fermentation broth.
  • the nanofiltration concentrate obtained after the nanofiltration treatment is then subjected to hydrogenation and ion exchange treatment to obtain liquid sorbitol with a sorbitol purity > 80%.
  • the invention not only improves the purity of erythritol, but also obtains an additional product of liquid sorbitol, and improves the utilization value of cornstarch.
  • Fig. 1 is the principle schematic diagram of the system utilizing cornstarch co-production erythritol and liquid sorbitol of the present invention
  • Fig. 2 is the principle schematic diagram of the method utilizing cornstarch co-production erythritol and liquid sorbitol of the present invention
  • FIG. 3 is a schematic diagram of the principle of the nanofiltration assembly and nanofiltration treatment in FIG. 1 .
  • the system includes a liquefaction tank 1 , a saccharification tank 2 , a filter 3 and a nanofiltration assembly 4 .
  • Liquefaction tank 1 is used to liquefy corn starch A
  • saccharification tank 2 is used to saccharify the liquefied material
  • filter 3 is used to filter impurities in the saccharified material to obtain glucose solution B
  • nanofiltration Component 4 performs nanofiltration treatment on the filtered glucose solution to obtain dialysate C and concentrated solution D respectively.
  • the dialysate C contains small molecular substances such as water and most of glucose.
  • Concentrate D contains a small portion of macromolecular substances such as glucose, oligosaccharides and other miscellaneous sugars.
  • the system also includes a fermentation and crystallization component I for fermenting and crystallizing the dialysate C to produce crystalline erythritol E, and a hydrogenation evaporation unit for hydrogenating and evaporating the concentrate D to produce liquid sorbitol F Component II.
  • a fermentation and crystallization component I for fermenting and crystallizing the dialysate C to produce crystalline erythritol E
  • a hydrogenation evaporation unit for hydrogenating and evaporating the concentrate D to produce liquid sorbitol F Component II.
  • described nanofiltration module 4 comprises buffer tank 41, feed pump 42, pre-filter 43 of nanofiltration, high-pressure pump 44 and by nanofiltration membrane 45 and
  • the nanofiltration membrane assembly 47 composed of the circulating pump 46, the glucose solution B filtered by the pre-nanofiltration filter 43 is subjected to nanofiltration treatment by the nanofiltration membrane assembly 47 to obtain the dialysate C and the concentrate D respectively.
  • the water and most of the glucose and other small molecules in the glucose solution B penetrate through the surface of the nanofiltration membrane under the action of pressure to form the dialysate C.
  • a small part of macromolecular components such as glucose, oligosaccharides and other miscellaneous sugars in the glucose solution B are intercepted by the nanofiltration membrane and cannot penetrate the surface of the nanofiltration membrane to form a concentrated solution D.
  • the nanofiltration assembly 4 includes a cleaning tank 48 and a cleaning pump 49 .
  • the cleaning tank 48 and the cleaning pump 49 are used for cleaning the nanofiltration membrane 45 regularly. Washing waste water G is obtained after washing.
  • the fermentation crystallization component I includes a fermenter 5 , a membrane filter 6 , a crystallization component 7 and a recrystallization component 8 .
  • the fermenter 5 is used to convert the glucose component in the dialysate C into erythritol after fermentation treatment.
  • Membrane filter 6 is used to remove impurities in the material after fermentation treatment.
  • the crystallization component 7 and the recrystallization component 8 are used for crystallizing the material filtered by the membrane filter 6 to obtain crystal erythritol E.
  • the hydrogenation evaporation assembly II includes a hydrogenation tank 9 , an ion exchanger 10 and an evaporation tank 11 .
  • the hydrogenation tank 9 is used to convert the glucose component in the concentrate D into sorbitol after hydrogenation treatment, and the ion exchanger 10 and the evaporation tank 11 are used to purify the hydrogenated material in the hydrogenation tank 9 to obtain liquid sorbitol F .
  • the present invention also discloses a method of utilizing cornstarch to co-produce erythritol and liquid sorbitol, which uses the aforementioned system utilizing cornstarch to co-produce erythritol and liquid sorbitol, the method comprising the following steps step:
  • Step 1 Liquefying, saccharifying and filtering the cornstarch A to obtain a glucose solution B with a solids concentration of 33%-35%.
  • the purity of glucose is 95.0%-96.3%.
  • liquefaction, saccharification and filtration treatment belong to the existing mature treatment process and will not be repeated here.
  • Step 2 The obtained glucose solution B is subjected to nanofiltration treatment to obtain dialysate C and concentrate D respectively.
  • dialysate C the purity of glucose is 99.0% to 99.5%
  • concentrate D the purity of glucose is 80.0% to 86.0% %.
  • Step 3 the obtained dialysate C is subjected to fermentation, membrane filtration, crystallization, recrystallization and other processes to obtain crystalline erythritol E, and the purity of erythritol is >99.5%, and the obtained concentrated solution D is hydrogenated, ionized Liquid sorbitol F is obtained after exchange, evaporation and other processes, and the purity of sorbitol is >80%.
  • fermentation, membrane filtration, crystallization, recrystallization and other processes belong to the existing mature treatment processes, and hydrogenation, ion exchange, evaporation and other process treatments also belong to the existing mature treatment processes, and will not be repeated here.
  • Step 1 the temperature of the glucose solution B is 50°C-60°C, and the pH value is 4.0-5.0.
  • the nanofiltration treatment includes entering the obtained glucose solution B into the buffer tank 41, then passing through the pre-nanofiltration filter 43 through the feed pump 42, and then passing the filtered glucose solution B through the high-pressure pump 44 enters the nanofiltration module 47 that is made up of nanofiltration membrane 45 and circulation pump 46 and carries out nanofiltration, obtains respectively the dialysate C that passes through nanofiltration membrane 45 and the concentrated solution D that does not pass through nanofiltration membrane 45 after nanofiltration treatment .
  • the nanofiltration treatment also includes using the cleaning water in the cleaning tank 48 to regularly clean the nanofiltration membrane 45 through a cleaning pump 49 . Washing waste water G is obtained after washing.
  • the operating temperature of the nanofiltration assembly is 40°C ⁇ 60°C, and the operating pressure is 15bar ⁇ 35bar.
  • Step 3 the dialysate is evaporated by heat exchange to a dry matter concentration of 35% before undergoing fermentation treatment.
  • the first embodiment of the method for co-producing erythritol and liquid sorbitol using cornstarch of the present invention uses 96% glucose solution to undergo nanofiltration and then ferment to prepare erythritol and hydrogenate to prepare liquid sorbitol.
  • the described method utilizing cornstarch to co-produce erythritol and liquid sorbitol comprises the following steps: taking 1 ton of glucose solution B dry basis of 96.0% purity prepared by cornstarch A after liquefaction, saccharification and filtration After filtration treatment, 0.8 tons of dialysate C with a glucose purity of 99.0% on a dry basis and 0.2 tons of a concentrated solution D with a glucose purity of 85.5% were obtained on a dry basis, and the dialysate C was subjected to fermentation, membrane filtration, crystallization, and recrystallization.
  • the specific steps include: using 0.8 tons of 96% pure glucose liquid on a dry basis to directly obtain 0.42 tons of crystals after fermentation, membrane filtration, crystallization, recrystallization and other processes Erythritol.
  • the conversion rate from glucose to erythritol is 52.50%.
  • Example 1 As can be seen from the comparison of Example 1 and Comparative Example, the same amount of glucose on a dry basis, the conversion rate of preparing erythritol by direct fermentation of glucose solution with a purity of 96% is not as good as using the dialysate obtained by nanofiltration from glucose solution The conversion rate of the erythritol prepared by utilizing the dialysate is high, because the purity of glucose in the dialysate is greater than 99%, which is higher than the purity of the glucose solution before dialysis.

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Abstract

一种利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的系统和方法。系统包括液化罐、糖化罐、过滤器以及纳滤组件，液化罐用于将玉米淀粉进行液化处理，糖化罐用于将液化处理后的物料进行糖化处理，过滤器用于过滤糖化处理后的物料中的杂质以得到葡萄糖液，纳滤组件对过滤处理后的葡萄糖液进行纳滤处理分别得到透析液和浓缩液，该系统还包括用于将透析液发酵及结晶处理以制备晶体赤藓糖醇的发酵结晶组件，以及用于将浓缩液进行氢化及蒸发处理以制备液体山梨糖醇的氢化蒸发组件。

Description

利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的系统及方法 技术领域
本发明属于糖醇制备技术领域，特别涉及一种利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的系统及方法。
 背景技术
赤藓糖醇已广泛应用于食品、饮料等行业中。目前，工业化制备赤藓糖醇的方法大多是以葡萄糖为原料经过微生物发酵制得，而葡萄糖通常是以淀粉为原料，经液化、糖化，然后经过精制、浓缩和结晶等工艺得到，如果可以把葡萄糖和赤藓糖醇生产工艺进行整合，将更有利于资源和能源的利用。公开号CN102154383A的中国专利介绍了一种利用玉米粉生产赤藓糖醇的方法，直接以玉米淀粉为原料，经过液化和糖化后，得到可发酵的葡萄糖，其中配料、酶水解和发酵培养在同一发酵罐中进行，省去了现有技术中的淀粉和葡萄糖的生产过程和装置。但是由于液化和糖化后得到的葡萄糖液中葡萄糖含量在96.0%左右，相比结晶葡萄糖中含量＞99.0%以上，葡萄糖的干基量减少了，另一方面，葡萄糖液中存在的其他杂质，进入发酵后，需要在后续赤藓糖醇提纯过程去除，增加了提纯工艺难度，影响整体收率。
 技术问题
本发明所要解决的技术问题在于，提供一种利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的系统及方法，从淀粉出发，将液化、糖化后得到的葡萄糖液经过纳滤处理后制备出赤藓糖醇和液体山梨糖醇两种产品。
 技术解决方案
本发明是这样实现的，提供一种利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的系统，包括液化罐、糖化罐、过滤器以及纳滤组件，液化罐用于将玉米淀粉进行液化处理，糖化罐用于将液化处理后的物料进行糖化处理，过滤器用于过滤糖化处理后的物料中的杂质以得到葡萄糖液，纳滤组件对过滤处理后的葡萄糖液进行纳滤处理分别得到透析液和浓缩液，该系统还包括用于将透析液发酵及结晶处理以制备晶体赤藓糖醇的发酵结晶组件，以及用于将浓缩液进行氢化及蒸发处理以制备液体山梨糖醇的氢化蒸发组件。
进一步地，所述纳滤组件包括依次通过管路连通的缓冲罐、进料泵、纳滤前过滤器、高压泵以及由纳滤膜和循环泵组成的纳滤膜组件，被纳滤前过滤器过滤处理后的葡萄糖液经过纳滤膜组件纳滤处理后分别得到透析液和浓缩液。
进一步地，所述发酵结晶组件包括发酵罐、膜过滤器、结晶组件和重结晶组件，发酵罐用于将透析液中的葡萄糖成份发酵处理后转化为赤藓糖醇，膜过滤器用于去除发酵处理后的物料中的杂质，结晶组件和重结晶组件用于将膜过滤器过滤处理后的物料进行结晶处理以得到晶体赤藓糖醇。
进一步地，所述氢化蒸发组件包括氢化罐、离子交换器和蒸发罐，氢化罐用于将浓缩液中的葡萄糖成份氢化处理后转化为山梨糖醇，离子交换器和蒸发罐用于将氢化罐氢化处理后的物料进行提纯以得到液体山梨糖醇。
本发明是这样实现的，还提供一种利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的方法，其使用了如前所述的利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的系统，该方法包括如下步骤：
步骤一、将玉米淀粉进行液化、糖化及过滤处理后得到固形物浓度33%~35%的葡萄糖液，在固形物中，葡萄糖纯度95.0%~96.3%；
步骤二、将得到的葡萄糖液进行纳滤处理，分别得到透析液和浓缩液，在透析液中，葡萄糖纯度99.0%~99.5%，在浓缩液中，葡萄糖纯度80.0%~86.0%；
步骤三、将得到的透析液经过发酵、膜过滤、结晶、重结晶等工艺处理后得到晶体赤藓糖醇，赤藓糖醇纯度＞99.5%，将得到的浓缩液经过氢化、离子交换、蒸发等工艺处理后得到液体山梨糖醇，山梨糖醇纯度＞80%。
进一步地，在步骤一中，所述葡萄糖液的温度50℃~60℃，pH值4.0~5.0。
进一步地，在步骤二中，所述纳滤处理包括将得到的葡萄糖液进入缓冲罐，再通过进料泵经过纳滤前过滤器，过滤处理后的葡萄糖液再通过高压泵进入由纳滤膜和循环泵组成的纳滤组件中进行纳滤，纳滤处理后分别得到透过纳滤膜的透析液和未透过纳滤膜的浓缩液。
进一步地，所述纳滤处理还包括使用清洗罐中的清洗水通过清洗泵对纳滤膜进行定期清洗。
进一步地，在纳滤处理时，纳滤组件的运行温度40℃~60℃，运行压力15bar~35bar。
进一步地，在步骤三中，所述透析液先换热蒸发至35%干物浓度后才进行发酵处理。
 有益效果
与现有技术相比，本发明的利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的系统及方法，以玉米淀粉为原料，经过液化和糖化处理后得到葡萄糖液，再经过纳滤处理后得到的葡萄糖含量在99%以上的透析液，用于发酵处理制备赤藓糖醇，相比于直接用葡萄糖含量96%的葡萄糖液，可以提升发酵液中赤藓糖醇干基浓度，不仅可提升发酵收率，而且也有利于发酵液后续的提纯。而经过纳滤处理后得到的纳滤浓缩液，再经过氢化及离子交换处理后得到山梨糖醇纯度＞80%的液体山梨醇。本发明不仅提高了赤藓糖醇的纯度，而且还得到液体山梨醇附加产品，提高了玉米淀粉的利用价值。
 附图说明
图1为本发明的利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的系统的原理示意图；
图2为本发明的利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的方法的原理示意图；
图3为图1中纳滤组件及纳滤处理的原理示意图。
 本发明的最佳实施方式
为了使本发明所要解决的技术问题、技术方案及有益效果更加清楚明白，以下结合附图及实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。
请同时参照图1以及图2所示，本发明利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的系统的较佳实施例，图中的带箭头的线条表示的是本发明中物料的流动方向。该系统包括液化罐1、糖化罐2、过滤器3以及纳滤组件4。
液化罐1用于将玉米淀粉A进行液化处理，糖化罐2用于将液化处理后的物料进行糖化处理，过滤器3用于过滤糖化处理后的物料中的杂质以得到葡萄糖液B，纳滤组件4对过滤处理后的葡萄糖液进行纳滤处理分别得到透析液C和浓缩液D。
在透析液C中含有水及大部分葡萄糖等小分子物质。在浓缩液D中含有小部分葡萄糖、低聚糖及其他杂糖等大分子物质。
该系统还包括用于将透析液C发酵及结晶处理以制备晶体赤藓糖醇E的发酵结晶组件Ⅰ，以及用于将浓缩液D进行氢化及蒸发处理以制备液体山梨糖醇F的氢化蒸发组件Ⅱ。
请同时参照图1以及图3所示，所述纳滤组件4包括依次通过管路连通的缓冲罐41、进料泵42、纳滤前过滤器43、高压泵44以及由纳滤膜45和循环泵46组成的纳滤膜组件47，被纳滤前过滤器43过滤处理后的葡萄糖液B经过纳滤膜组件47纳滤处理后分别得到透析液C和浓缩液D。葡萄糖液B中的水及大部分葡萄糖等小分子成份在压力的作用下，穿透过纳滤膜表面，形成了透析液C。葡萄糖液B中的小部分葡萄糖、低聚糖及其他杂糖等大分子成份被纳滤膜截留，无法穿透过纳滤膜表面，形成浓缩液D。
所述纳滤组件4包括清洗罐48和清洗泵49。清洗罐48和清洗泵49用于定期地对纳滤膜45进行清洗。清洗后得到清洗废水G。
所述发酵结晶组件Ⅰ包括发酵罐5、膜过滤器6、结晶组件7和重结晶组件8。发酵罐5用于将透析液C中的葡萄糖成份发酵处理后转化为赤藓糖醇。膜过滤器6用于去除发酵处理后的物料中的杂质。结晶组件7和重结晶组件8用于将膜过滤器6过滤处理后的物料进行结晶处理以得到晶体赤藓糖醇E。
所述氢化蒸发组件Ⅱ包括氢化罐9、离子交换器10和蒸发罐11。氢化罐9用于将浓缩液D中的葡萄糖成份氢化处理后转化为山梨糖醇，离子交换器10和蒸发罐11用于将氢化罐9氢化处理后的物料进行提纯以得到液体山梨糖醇F。
本发明还公开一种利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的方法，其使用了如前所述的利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的系统，该方法包括如下步骤：
步骤一、将玉米淀粉A进行液化、糖化及过滤处理后得到固形物浓度33%~35%的葡萄糖液B，在固形物中，葡萄糖纯度95.0%~96.3%。其中，液化、糖化及过滤处理属于现有成熟的处理工艺，不再赘述。
步骤二、将得到的葡萄糖液B进行纳滤处理，分别得到透析液C和浓缩液D，在透析液C中，葡萄糖纯度99.0%~99.5%，在浓缩液D中，葡萄糖纯度80.0%~86.0%。
步骤三、将得到的透析液C经过发酵、膜过滤、结晶、重结晶等工艺处理后得到晶体赤藓糖醇E，赤藓糖醇纯度＞99.5%，将得到的浓缩液D经过氢化、离子交换、蒸发等工艺处理后得到液体山梨糖醇F，山梨糖醇纯度＞80%。其中，发酵、膜过滤、结晶、重结晶等工艺处理属于现有成熟的处理工艺，氢化、离子交换、蒸发等工艺处理也属于现有成熟的处理工艺，不再赘述。
具体地，在步骤一中，所述葡萄糖液B的温度50℃~60℃，pH值4.0~5.0。
具体地，在步骤二中，所述纳滤处理包括将得到的葡萄糖液B进入缓冲罐41，再通过进料泵42经过纳滤前过滤器43，过滤处理后的葡萄糖液B再通过高压泵44进入由纳滤膜45和循环泵46组成的纳滤组件47中进行纳滤，纳滤处理后分别得到透过纳滤膜45的透析液C和未透过纳滤膜45的浓缩液D。
所述纳滤处理还包括使用清洗罐48中的清洗水通过清洗泵49对纳滤膜45进行定期清洗。清洗后得到清洗废水G。
在纳滤处理时，纳滤组件的运行温度40℃~60℃，运行压力15bar~35bar。
具体地，在步骤三中，所述透析液先换热蒸发至35%干物浓度后才进行发酵处理。
 本发明的实施方式
下面通过具体实施例进一步说明本发明的利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的方法。
实施例1
本发明的利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的方法第一种实施例，采用96%葡萄糖液先经纳滤后再发酵制备赤藓糖醇及氢化制备液体山梨糖醇。
所述的利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的方法包括如下步骤：取由玉米淀粉A进行液化、糖化及过滤处理后制备的96.0%纯度的葡萄糖液B干基1吨进行纳滤处理，分别得到葡萄糖纯度99.0%的透析液C干基0.8吨和葡萄糖纯度85.5%的浓缩液D干基0.2吨，将透析液C进行发酵、膜过滤、结晶、重结晶等工艺处理后最终得到0.43吨的晶体赤藓糖醇E，由葡萄糖到赤藓糖醇的转化率为53.75%；另外，将浓缩液D经过氢化、离子交换、蒸发等工艺处理后得到液体山梨糖醇F干基0.2吨。
对比例
采用96%葡萄糖液直接用于发酵制备赤藓糖醇，具体步骤包括：使用96%纯度的葡萄糖液干基0.8吨直接经过发酵、膜过滤、结晶、重结晶等工艺处理后得到0.42吨的晶体赤藓糖醇。由葡萄糖到赤藓糖醇的转化率52.50%。
从实施例1与对比例的对比可以看出，同样干基的葡萄糖量，其由纯度96%的葡萄糖液直接发酵制备赤藓糖醇的转化率不如使用由葡萄糖液经过纳滤得到的透析液后再利用该透析液制备的赤藓糖醇的转化率高，因为，在透析液中葡萄糖的纯度大于99%，比透析前的葡萄糖液的纯度高。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。
 工业实用性
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Claims (10)

  1. 一种利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的系统，其特征在于，包括液化罐、糖化罐、过滤器以及纳滤组件，液化罐用于将玉米淀粉进行液化处理，糖化罐用于将液化处理后的物料进行糖化处理，过滤器用于过滤糖化处理后的物料中的杂质以得到葡萄糖液，纳滤组件对过滤处理后的葡萄糖液进行纳滤处理分别得到透析液和浓缩液，该系统还包括用于将透析液发酵及结晶处理以制备晶体赤藓糖醇的发酵结晶组件，以及用于将浓缩液进行氢化及蒸发处理以制备液体山梨糖醇的氢化蒸发组件。
  2. 如权利要求1所述的利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的系统，其特征在于，所述纳滤组件包括依次通过管路连通的缓冲罐、进料泵、纳滤前过滤器、高压泵以及由纳滤膜和循环泵组成的纳滤膜组件，被纳滤前过滤器过滤处理后的葡萄糖液经过纳滤膜组件纳滤处理后分别得到透析液和浓缩液。
  3. 如权利要求2所述的利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的系统，其特征在于，所述发酵结晶组件包括发酵罐、膜过滤器、结晶组件和重结晶组件，发酵罐用于将透析液中的葡萄糖成份发酵处理后转化为赤藓糖醇，膜过滤器用于去除发酵处理后的物料中的杂质，结晶组件和重结晶组件用于将膜过滤器过滤处理后的物料进行结晶处理以得到晶体赤藓糖醇。
  4. 如权利要求3所述的利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的系统，其特征在于，所述氢化蒸发组件包括氢化罐、离子交换器和蒸发罐，氢化罐用于将浓缩液中的葡萄糖成份氢化处理后转化为山梨糖醇，离子交换器和蒸发罐用于将氢化罐氢化处理后的物料进行提纯以得到液体山梨糖醇。
  5. 一种利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的方法，其特征在于，其使用了如权利要求4所述的利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的系统，该方法包括如下步骤：
    步骤一、将玉米淀粉进行液化、糖化及过滤处理后得到固形物浓度33%~35%的葡萄糖液，在固形物中，葡萄糖纯度95.0%~96.3%；
    步骤二、将得到的葡萄糖液进行纳滤处理，分别得到透析液和浓缩液，在透析液中，葡萄糖纯度99.0%~99.5%，在浓缩液中，葡萄糖纯度80.0%~86.0%；
    步骤三、将得到的透析液经过发酵、膜过滤、结晶及重结晶处理后得到晶体赤藓糖醇，赤藓糖醇纯度＞99.5%，将得到的浓缩液经过氢化、离子交换及蒸发处理后得到液体山梨糖醇，山梨糖醇纯度＞80%。
  6. 如权利要求5所述的利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的方法，其特征在于，在步骤一中，所述葡萄糖液的温度50℃~60℃，pH值4.0~5.0。
  7. 如权利要求5所述的利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的方法，其特征在于，在步骤二中，所述纳滤处理包括将得到的葡萄糖液进入缓冲罐，再通过进料泵经过纳滤前过滤器，过滤处理后的葡萄糖液再通过高压泵进入由纳滤膜和循环泵组成的纳滤组件中进行纳滤，纳滤处理后分别得到透过纳滤膜的透析液和未透过纳滤膜的浓缩液。
  8. 如权利要求7所述的利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的方法，其特征在于，所述纳滤处理还包括使用清洗罐中的清洗水通过清洗泵对纳滤膜进行定期清洗。
  9. 如权利要求7所述的利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的方法，其特征在于，在纳滤处理时，纳滤组件的运行温度40℃~60℃，运行压力15bar~35bar。
  10. 如权利要求5所述的利用玉米淀粉联产赤藓糖醇和液体山梨糖醇的方法，其特征在于，在步骤三中，所述透析液先换热蒸发至35%干物浓度后才进行发酵处理。
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