CN103923130A - Method for separating glucose and xylose in straw fiber enzymatic hydrolysate - Google Patents
Method for separating glucose and xylose in straw fiber enzymatic hydrolysate Download PDFInfo
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Abstract
The invention relates to a method for separating glucose and xylose in straw fiber enzymatic hydrolysate. The method for separating glucose and xylose in straw fiber enzymatic hydrolysate comprises the following steps: a) blending feeding syrup, namely, adjusting the concentration of desalted, decolored and concentrated straw fiber enzymatic hydrolysate to be 40-60%; b) filtering, namely, filtering the syrup solution obtained in the step a) by using a micron-order filter so as to prepare a clear liquid in which impurities visible to the naked eyes do not exist; c) performing sequential simulated moving bed chromatographic separation, namely, performing sequential simulated moving bed chromatographic separation on the obtained syrup, wherein deionized water is adopted as an eluent, high-acidity cation exchange resin is adopted as an adsorbent, the separation temperature is 60-70 DEG C, and the sequential simulated moving bed chromatographic separation equipment comprises 9 chromatographic columns arranged in sequence, and is provided with two inlets and two outlets which are alternated sequentially; d) concentrating, namely, concentrating an obtained solution of a component A to be 70-75%, mixing an obtained component B, and further concentrating to be 70-75%. The method is low in operation cost, a product obtained from separation is high in purity, concentration and yield, and continuous and industrial production is achieved.
Description
One, technical field
What the present invention relates to is sequential simulated mobile chromatographic separation technology, and what be specifically related to is the method that separates glucose and xylose in stalk fibre enzymolysis solution.
Two, background technology
According to incompletely statistics, China produces hundred million tons of agricultural crop straw 6-8 every year, approximately has and more than 2/3 is not effectively utilized and is wasted.These unemployed agricultural crop straw major parts are directly burnt, processing like this agricultural crop straw not only causes a large amount of wastes of resource and causes environmental pollution, also can cause fire failure, the poor efficiency and the low economic benefit that have also caused on the other hand agricultural crop straw to utilize.In stalk, containing a large amount of Mierocrystalline celluloses and hemicellulose, is the fine raw material of sugaring.Along with the development of biotechnology, stalk enzymolysis sugar refining is mature on the whole at present, and 3-4 ton stalk can be produced 1 ton of 70% syrup after enzymolysis, and it has a extensive future as seen.But, main component in straw enzymolysis is glucose and xylose, but the closely similar very difficult separation of the physico-chemical property of glucose and xylose, therefore, in stalk fibre enzymolysis solution, the isolation technique of glucose and xylose becomes the key that can agricultural crop straw efficiently utilize.
Simulating mobile chromatographic bed (SMB) is a kind of advanced isolation technique efficiently, and modern functions sugar and the development of functional sugar alcohol, glucose, sucrose and herbal medicine are had to vital role.State-of-the-art simulated moving bed chromatography is sequential type simulated moving bed chromatography (SSMB) in the world at present.SSMB than traditional SMB advanced person many, be characterized in that separator column quantity reduces, reduce running cost 30%-50% than traditional chromatographic separation equipment, solvent load reduces 20%-40%.Ensureing, on highly purified basis, to there is the performances such as high separation property, high-recovery, high-level efficiency, low cost, high stability.
Chinese patent 200910039185.6 discloses a kind of method of preparing plant hemicellulose hydrolyzed solution and extraction wood sugar and extracting pectinose; Chinese patent 201010000196. 6 discloses a kind of corncob acid hydrolysis slag and stalk soda boiling slag mixing enzymolysis method; Chinese patent 201210518298.6 discloses a kind of method that improves stalk reducing sugar content.As seen from the above, the patent of the aspect of the existing stalk sugaring of China at present mainly concentrates on the pre-treatment aspect of stalk sugaring, in stalk fibre enzymolysis solution, aspect the separation of glucose and xylose, there is no achievement in research.
Chinese patent 200710014175.8 discloses a kind of method of utilizing sequential simulated moving bed purifying xylose mother liquor, it be utilize sequential simulated moving bed to glucose, wood sugar separates with pectinose component simultaneously, wherein glucose purity and concentration are 5% and 75.6%, wood sugar purity and concentration are 90.2% and 31.5%, pectinose purity and concentration are 85.8% and 7.5%, result shows that wood sugar and pectinose purity and concentration are not high, sequential simulated moving bed advantage is not brought into play completely, a part of wood sugar and pectinose have been lost again in the extraction of glucose component, cause the yield of these two components to reduce, there is the decline of certain amplitude in whole economic efficiency, Chinese patent 200720141139.3 discloses a kind of sequential type simulation moving bed chromatogram device, Chinese patent 200920274899.0 discloses a kind of sequential type simulated moving bed chromatography purification device.As seen from the above, the patent of the existing sequential type simulated moving bed chromatography of China aspect mainly concentrates on the research and development manufacture view of device at present, application aspect sugar alcohol neither be very ripe, and the glucose and xylose that utilizes sequential type simulated moving bed chromatography to separate in stalk fibre enzymolysis solution does not have achievement in research.
Three, summary of the invention
The object of this invention is to provide the method that separates glucose and xylose in stalk fibre enzymolysis solution, in this separation stalk fibre enzymolysis solution, the method for glucose and xylose is for solving the difficult problem that glucose and xylose in prior art stalk fibre enzymolysis solution cannot high efficiency separation.
The technical solution used in the present invention is: in this separation stalk fibre enzymolysis solution, the method for glucose and xylose is as follows:
A), the allotment of charging syrup: be 40-60% by being formulated to concentration through desalination, decolouring, stalk fibre enzymolysis solution after concentrated;
B), filter: the syrup solution that step a) is obtained filters with micron order filter, make clarification without macroscopic liquid;
C), sequential type simulated moving bed chromatography separate: by syrup obtained above through sequential type simulated moving bed chromatography device separates, eluent is deionized water, sorbent material is highly acidic cation crossover resin, separation temperature is 60-70 DEG C, sequential type simulated moving bed chromatography separating device comprises 9 chromatographic columns of arranging in turn, have 2 of the opening for feeds of order conversion, 2 of discharge ports, are wherein divided into following three steps when No. 1 post position:
The first step: material can not enter, carries out systemic circulation, liquid flow path direction is to be flowed by No. 1 post to 9 post, internal circulating load is 50%～70% of chromatographic column volume;
Second step: this step is partial circulating, only enters eluent deionized water, No. 1 post enters eluent, under No. 8 posts, brings out a part of B component, and B component is glucose component, and entering amount of eluent is 3%～15% of chromatographic column volume;
The 3rd step: enter material simultaneously, enter eluent, discharging, this step claims again all-in and all-out, and No. 1 post enters eluent, brings out component A under No. 1 post, and component A is wood sugar component; No. 9 post enters raw material, brings out the B component of another part under No. 8 posts, and entering amount of eluent is 3%～15% of chromatographic column volume, and inlet amount is 5%～10% of chromatographic column volume;
After No. 1 post end of run, repeat in order above three steps, wherein, in the time repeating second step and the 3rd step, every repetition once, charging and discharging position moves to next post by No. 1 post to 9 post direction;
D), concentrated: the component A solution that all third steps are made concentrates, and component A strength of solution is concentrated into 70%～75%, and the B component that all second steps, third step are made is mixed, then concentrates, and B component strength of solution is reduced to 70%～75%.
Such scheme middle strong acidity cationic exchange type resin is any one in ZG-106Na+, UBK530 Na+, UBK550 Na+, 99 Na+-310 or 99 Na+-320.
Beneficial effect:
1, the present invention adopts sequential type simulated moving bed chromatography to separate glucose and xylose in stalk fibre enzymolysis solution, separation obtains component A solution and B component solution, component A concentration is 30%～40%, wood sugar purity 80%～90%, yield 80～90%, B component concentration is 30%～40%, glucose purity 80%～90%, yield 75～85%, and process operation cost is low, product purity, concentration and yield that separation obtains are high, can realize serialization, suitability for industrialized production.
2, the present invention has reduced follow-up concentrated cost, has simplified operation steps, has reduced production loss.
Four, brief description of the drawings
Fig. 1 is production method FB(flow block) of the present invention;
Fig. 2 is the schematic diagram of the first step during sequential type simulated moving bed chromatography of the present invention separates;
Fig. 3 is the schematic diagram of second step during sequential type simulated moving bed chromatography of the present invention separates;
Fig. 4 is the schematic diagram of the 3rd step during sequential type simulated moving bed chromatography of the present invention separates;
Fig. 5 is straw enzymolysis liquid-phase chromatographic analysis collection of illustrative plates;
Fig. 6 is the glucose component liquid-phase chromatographic analysis collection of illustrative plates after embodiment 3 sequential type simulated moving bed chromatographies separate;
Fig. 7 is the wood sugar component liquid-phase chromatographic analysis collection of illustrative plates after embodiment 3 sequential type simulated moving bed chromatographies separate.
Five, embodiment
Below in conjunction with accompanying drawing, the present invention is described further:
embodiment 1
As shown in Figure 1, in this separation stalk fibre enzymolysis solution, the method for glucose and xylose is as follows:
A), the allotment of charging syrup: be 60% by being formulated to concentration through desalination, decolouring, stalk fibre enzymolysis solution after concentrated;
B), filter: the syrup solution that step a) is obtained filters with micron order filter, makes the liquid without the visible impurity of naked eyes of clarification;
C), sequential type simulated moving bed chromatography separates: syrup obtained above is separated through sequential simulated mobile chromatographic equipment.Eluent is water, and sorbent material is resin ZG-106 Na
+, separation temperature is 60-70 DEG C, and sequential type simulated moving bed chromatography separating device comprises 9 chromatographic columns of arranging in turn, has 2 of the opening for feeds of order conversion, and 2 of discharge ports are wherein divided into following three steps when No. 1 post position:
The first step: material can not enter, carries out systemic circulation, liquid flow path direction is to be flowed by No. 1 post to 9 post, internal circulating load is 60% of chromatographic column volume, consults Fig. 2;
Second step: this step is partial circulating, only enters eluent deionized water, No. 1 post enters eluent, brings out a part of B component (glucose component) under No. 8 posts, and entering amount of eluent is 5% of chromatographic column volume, consults Fig. 3, and in figure, D is water;
The 3rd step: enter material simultaneously, enter eluent, discharging, this step claims again all-in and all-out.No. 1 post enters eluent, brings out component A(wood sugar component under No. 1 post); No. 6 post enters raw material, brings out the B component (glucose component) of another part under No. 8 posts.Entering amount of eluent is 5% of chromatographic column volume, and inlet amount is 5% of chromatographic column volume, consults Fig. 4, and in figure, D is water;
After No. 1 post end of run, repeat successively above three steps by the order of No. 2 post-No. 9 posts, wherein, in the time repeating second step and the 3rd step, every repetition once, charging and discharging position moves to next post by No. 1 post to 9 post direction.
D), concentrated: concentrated: the component A solution that all third steps are made concentrates, component A strength of solution is concentrated into 70%～75%, the B component that all second steps, third step are made is mixed, then concentrates, and B component strength of solution is reduced to 70%～75%.
The present embodiment separates and obtains component A solution and B component solution, and component A concentration is 36.5%, wood sugar purity 85.3%, yield 82.1%, and B component concentration is 32.0%, glucose purity 86.7%, yield 79.4%.
embodiment 2
In this separation stalk fibre enzymolysis solution, the method for glucose and xylose is as follows:
A), the allotment of charging syrup: be 60% by being formulated to concentration through desalination, decolouring, stalk fibre enzymolysis solution after concentrated;
B), filter: the syrup solution that step a) is obtained filters with micron order filter, make clarification without macroscopic liquid;
C), sequential type simulated moving bed chromatography separates: syrup obtained above is separated through sequential simulated mobile chromatographic equipment.Eluent is water, and sorbent material is resin 99 Na+-310, and separation temperature is 60-70 DEG C, sequential type simulated moving bed chromatography separating device comprises 9 chromatographic columns of arranging in turn, have 2 of the opening for feeds of order conversion, 2 of discharge ports, are wherein divided into following three steps when No. 1 post position:
The first step: material can not enter, carries out systemic circulation, liquid flow path direction is to be flowed by No. 1 post to 9 post, internal circulating load is 55% of chromatographic column volume;
Second step: this step is partial circulating, only enters eluent deionized water, No. 1 post enters eluent, brings out a part of B component (glucose component) under No. 8 posts, and entering amount of eluent is 7.5% of chromatographic column volume;
The 3rd step: enter material simultaneously, enter eluent, discharging, this step claims again all-in and all-out.No. 1 post enters eluent, brings out component A(wood sugar component under No. 1 post); No. 6 post enters raw material, brings out the B component (glucose component) of another part under No. 8 posts.Entering amount of eluent is 7.5% of chromatographic column volume, and inlet amount is 10% of chromatographic column volume;
After No. 1 post end of run, repeat successively above three steps by the order of No. 2 post-No. 9 posts, wherein, in the time repeating second step and the 3rd step, every repetition once, charging and discharging position moves to next post by No. 1 post to 9 post direction.
D), concentrated: the component A solution that all third steps are made concentrates, and component A strength of solution is concentrated into 70%～75%, and the B component that all second steps, third step are made is mixed, then concentrates, and B component strength of solution is reduced to 70%～75%.
The present embodiment separates and obtains component A solution and B component solution, and component A concentration is 39.5%, wood sugar purity 82.6%, yield 88.2%, and B component concentration is 35.0%, glucose purity 83.5%, yield 75.8%.
embodiment 3
In this separation stalk fibre enzymolysis solution, the method for glucose and xylose is as follows:
A), the allotment of charging syrup: be 40% by being formulated to concentration through desalination, decolouring, stalk fibre enzymolysis solution after concentrated;
B), filter: the syrup solution that step a) is obtained filters with micron order filter, make clarification without macroscopic liquid;
C), sequential type simulated moving bed chromatography separates: syrup obtained above is separated through sequential simulated mobile chromatographic equipment.Eluent is water, and sorbent material is resin 99 Na+-310, and separation temperature is 60-70 DEG C, sequential type simulated moving bed chromatography separating device comprises 9 chromatographic columns of arranging in turn, have 2 of the opening for feeds of order conversion, 2 of discharge ports, are wherein divided into following three steps when No. 1 post position:
The first step: material can not enter, carries out systemic circulation, liquid flow path direction is to be flowed by No. 1 post to 9 post, internal circulating load is 55% of chromatographic column volume;
Second step: this step is partial circulating, only enters eluent deionized water, No. 1 post enters eluent, brings out a part of B component (glucose component) under No. 8 posts, and entering amount of eluent is 5% of chromatographic column volume;
The 3rd step: enter material simultaneously, enter eluent, discharging, this step claims again all-in and all-out.No. 1 post enters eluent, brings out component A(wood sugar component under No. 1 post); No. 6 post enters raw material, brings out the B component (glucose component) of another part under No. 8 posts.Entering amount of eluent is 5% of chromatographic column volume, and inlet amount is 10% of chromatographic column volume;
After No. 1 post end of run, repeat successively above three steps by the order of No. 2 post-No. 9 posts, wherein, in the time repeating second step and the 3rd step, every repetition once, charging and discharging position moves to next post by No. 1 post to 9 post direction.
D), concentrated: the component A solution that all third steps are made concentrates, and component A strength of solution is concentrated into 70%～75%, and the B component that all second steps, third step are made is mixed, then concentrates, and B component strength of solution is reduced to 70%～75%.
The present embodiment separates and obtains component A solution and B component solution, and component A concentration is 38.2%, wood sugar purity 88.7%, yield 85.4%, and B component concentration is 30.4%, glucose purity 82.6%, yield 83.7%.
embodiment 4
In this separation stalk fibre enzymolysis solution, the method for glucose and xylose is as follows:
A), the allotment of charging syrup: be 50% by being formulated to concentration through desalination, decolouring, stalk fibre enzymolysis solution after concentrated;
B), filter: the syrup solution that step a) is obtained filters with micron order filter, make clarification without macroscopic liquid;
C), sequential type simulated moving bed chromatography separates: syrup obtained above is separated through sequential simulated mobile chromatographic equipment.Eluent is water, and sorbent material is resin 99 Na+-310, and separation temperature is 60-70 DEG C, sequential type simulated moving bed chromatography separating device comprises 9 chromatographic columns of arranging in turn, have 2 of the opening for feeds of order conversion, 2 of discharge ports, are wherein divided into following three steps when No. 1 post position:
The first step: material can not enter, carries out systemic circulation, liquid flow path direction is to be flowed by No. 1 post to 9 post, internal circulating load is 60% of chromatographic column volume;
Second step: this step is partial circulating, only enters eluent deionized water, No. 1 post enters eluent, brings out a part of B component (glucose component) under No. 8 posts, and entering amount of eluent is 5% of chromatographic column volume;
The 3rd step: enter material simultaneously, enter eluent, discharging, this step claims again all-in and all-out.No. 1 post enters eluent, brings out component A(wood sugar component under No. 1 post); No. 6 post enters raw material, brings out the B component (glucose component) of another part under No. 8 posts.Entering amount of eluent is 5% of chromatographic column volume, and inlet amount is 5% of chromatographic column volume;
After No. 1 post end of run, repeat successively above three steps by the order of No. 2 post-No. 9 posts, wherein, in the time repeating second step and the 3rd step, every repetition once, charging and discharging position moves to next post by No. 1 post to 9 post direction.
D), concentrated: the component A solution that all third steps are made concentrates, and component A strength of solution is concentrated into 70%～75%, and the B component that all second steps, third step are made is mixed, then concentrates, and B component strength of solution is reduced to 70%～75%.
The present embodiment separates and obtains component A solution and B component solution, and component A concentration is 34.8%, wood sugar purity 89.5%, yield 81.3%, and B component concentration is 30.3%, glucose purity 80.5%, yield 82.3%.
Core technology of the present invention is that sequential type simulated moving bed chromatography separates glucose and xylose technology in stalk fibre enzymolysis solution, obtain all higher dextrose syrup and wood sugar syrup of purity and yield, this technique has not only ensured high purity and the high yield of glucose and xylose, also in the cost savings of whole technique, process is easy etc., and aspect has distinct characteristic.
Claims (2)
1. a method that separates glucose and xylose in stalk fibre enzymolysis solution, is characterized in that: in this separation stalk fibre enzymolysis solution, the method for glucose and xylose is as follows:
A), the allotment of charging syrup: be 40-60% by being formulated to concentration through desalination, decolouring, stalk fibre enzymolysis solution after concentrated;
B), filter: the syrup solution that step a) is obtained filters with micron order filter, make clarification without macroscopic liquid;
C), sequential type simulated moving bed chromatography separate: by syrup obtained above through sequential type simulated moving bed chromatography device separates, eluent is deionized water, sorbent material is highly acidic cation crossover resin, separation temperature is 60-70 DEG C, sequential type simulated moving bed chromatography separating device comprises 9 chromatographic columns of arranging in turn, have 2 of the opening for feeds of order conversion, 2 of discharge ports, are wherein divided into following three steps when No. 1 post position:
The first step: material can not enter, carries out systemic circulation, liquid flow path direction is to be flowed by No. 1 post to 9 post, internal circulating load is 50%～70% of chromatographic column volume;
Second step: this step is partial circulating, only enters eluent deionized water, No. 1 post enters eluent, under No. 8 posts, brings out a part of B component, and B component is glucose component, and entering amount of eluent is 3%～15% of chromatographic column volume;
The 3rd step: enter material simultaneously, enter eluent, discharging, this step claims again all-in and all-out, and No. 1 post enters eluent, brings out component A under No. 1 post, and component A is wood sugar component; No. 9 post enters raw material, brings out the B component of another part under No. 8 posts, and entering amount of eluent is 3%～15% of chromatographic column volume, and inlet amount is 5%～10% of chromatographic column volume;
After No. 1 post end of run, repeat in order above three steps, wherein, in the time repeating second step and the 3rd step, every repetition once, charging and discharging position moves to next post by No. 1 post to 9 post direction;
D), concentrated: the component A solution that all third steps are made concentrates, and component A strength of solution is concentrated into 70%～75%, and the B component that all second steps, third step are made is mixed, then concentrates, and B component strength of solution is reduced to 70%～75%.
2. the method for glucose and xylose in separation stalk fibre enzymolysis solution according to claim 1, is characterized in that: described highly acidic cation crossover resin is any one in ZG-106Na+, UBK530 Na+, UBK550 Na+, 99 Na+-310 or 99 Na+-320.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111285132A (en) * | 2020-03-18 | 2020-06-16 | 华润电力技术研究院有限公司 | Thermal power equipment and control method and system for material piling and taking of circular coal yard of thermal power equipment |
| WO2020260028A1 (en) * | 2019-06-28 | 2020-12-30 | IFP Energies Nouvelles | Liquid phase separation of second-generation sugars by adsorption on fau zeolite having a si/al atomic ratio of less than 1.5 |
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| US20040173533A1 (en) * | 2001-07-24 | 2004-09-09 | Farone William A. | Separation of xylose and glucose |
| CN102850408A (en) * | 2012-09-12 | 2013-01-02 | 黑龙江八一农垦大学 | Method for preparing xylose and arabinose by using simulated moving chromatography |
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| US5730877A (en) * | 1994-04-21 | 1998-03-24 | Xyrofin Oy | Method for fractionating a solution |
| US20040173533A1 (en) * | 2001-07-24 | 2004-09-09 | Farone William A. | Separation of xylose and glucose |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020260028A1 (en) * | 2019-06-28 | 2020-12-30 | IFP Energies Nouvelles | Liquid phase separation of second-generation sugars by adsorption on fau zeolite having a si/al atomic ratio of less than 1.5 |
| FR3097855A1 (en) * | 2019-06-28 | 2021-01-01 | IFP Energies Nouvelles | Liquid phase separation of second generation sugars by adsorption on FAU-type zeolite with Si / Al atomic ratio less than 1.5 |
| CN114008222A (en) * | 2019-06-28 | 2022-02-01 | Ifp 新能源公司 | By phase separation of the dibasic sugar solution adsorbed on FAU zeolite having an Si/Al atomic ratio of less than 1.5 |
| CN114008222B (en) * | 2019-06-28 | 2024-03-08 | Ifp 新能源公司 | Liquid phase separation of disaccharides by adsorption onto FAU zeolites having Si/Al atomic ratios less than 1.5 |
| CN111285132A (en) * | 2020-03-18 | 2020-06-16 | 华润电力技术研究院有限公司 | Thermal power equipment and control method and system for material piling and taking of circular coal yard of thermal power equipment |
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