CN112301077A - Method for producing xylooligosaccharide by continuous liquefaction coupling enzyme method of hemicellulose powder - Google Patents
Method for producing xylooligosaccharide by continuous liquefaction coupling enzyme method of hemicellulose powder Download PDFInfo
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Abstract
The invention relates to the technical field of sugar industry by utilizing natural resources, and particularly discloses a method for producing xylo-oligosaccharide by a hemicellulose powder continuous liquefaction coupling enzyme method, which comprises the following steps: size mixing → continuous liquefaction → separation of residue and liquid → primary enzymolysis → primary decolorization → primary ion exchange → primary concentration → secondary enzymolysis → secondary decolorization → secondary ion exchange → secondary concentration; the method reduces energy consumption, reduces the discharge of waste, reduces the pollution to the environment, and has great economic benefit and social benefit.
Description
Technical Field
The invention relates to the technical field of sugar industry by utilizing natural resources, in particular to a method for producing xylo-oligosaccharide by a hemicellulose powder continuous liquefaction coupling enzyme method.
Background
The xylo-oligosaccharide is also called xylo-oligosaccharide, and is a functional polysaccharide formed by combining 2-7 xylose molecules by beta-1, 4 glycosidic bonds. The preparation method of xylo-oligosaccharide generally comprises the following steps: 1. directly treating natural wood fiber material containing xylan by an enzyme method; 2. separating xylan from wood fiber material chemically, and hydrolyzing xylan to oligoxylose with enzyme; 3. the xylan is directly hydrolyzed by steam, water or dilute inorganic acid to generate xylo-oligosaccharide.
The raw materials for producing xylo-oligosaccharide in the industry at present are corncob powder or rice husk and other agricultural wastes. The purchasing of the agricultural wastes is easily limited and influenced by seasons and regions, and has a plurality of inconvenient factors for industrial production. The raw material adopted by the project is hemicellulose powder, the xylan content is more than 90%, the ash content is lower than 3.5%, the active ingredients are high, the impurity content is small, and the raw material is the best production raw material which has the advantages of highest yield, highest purity, stable source, no limitation of acquisition radius and no influence of seasons for producing xylo-oligosaccharide at present.
The prior production process for producing xylo-oligosaccharide in the industry is to pretreat corncob powder with acetic acid, then perform intermittent high-pressure cooking, and then perform enzymolysis to obtain the xylo-oligosaccharide. However, the existing production process has the following problems: the corn cob powder contains a lot of impurities, the light transmittance of the saccharified feed liquid is low (less than 2%), the conductivity is high (more than 6000 mu s/cm), and the purity of the xylo-oligosaccharide is not high (less than 75%), so that the acid and alkali consumption is high, the sewage discharge amount is large, the intermittent cooking waste heat is not easy to recover, and the steam consumption is high. If the raw material adopts hemicellulose powder, firstly adding acid and water to stir and mix into suspension, then conveying the suspension into continuous cooking equipment by a pump, carrying out enzymolysis after flash evaporation and temperature reduction, wherein the light transmittance of the saccharified feed liquid is more than 10 percent, the electric conductivity is lower than 3000 mu s/cm, the purity of the xylo-oligosaccharide is more than 80 percent, the product quality is improved, the sewage quantity is greatly reduced, the waste heat of continuous liquefaction is convenient to recover, and the energy consumption is reduced.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for producing xylo-oligosaccharide by a continuous liquefaction coupling enzyme method of hemicellulose powder, which reduces energy consumption, reduces waste discharge, reduces environmental pollution, and has great economic and social benefits.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for producing xylooligosaccharide by a hemicellulose powder continuous liquefaction coupling enzyme method comprises the following steps:
1) mixing pulp, namely putting the hemicellulose and 0.2% acetic acid aqueous solution in a mass ratio of 1:10 into a pulp mixing tank, heating to 70-80 ℃, and stirring and mixing uniformly to form a hemicellulose powder suspension;
2) continuously cooking, namely conveying the hemicellulose powder suspension obtained in the step 1 to a liquefaction ejector, ensuring that the steam pressure of the liquefaction ejector is 0.8-1.0MPa, keeping the material temperature at 180-;
3) separating slag and liquid, namely conveying the raw materials treated in the step 2 into a plate frame for separating slag and liquid;
4) carrying out primary enzymolysis, inputting the liquid obtained by separation in the step 3 into an enzymolysis tank, adding xylanase, and carrying out saccharification enzymolysis;
5) primary decolorization, namely filtering the material subjected to enzymolysis treatment in the step 4, and adding powdered activated carbon into filtrate for decolorization to obtain feed liquid with the light transmittance of more than 20%;
6) performing ion exchange on the feed liquid obtained in the step 5 for one time, wherein the conductivity after ion exchange is less than 500 mu s/cm, the PH value is 3-5, and the light transmittance is more than 90%; regenerating the ion exchange column after the ion exchange column is invalid by using hydrochloric acid with the concentration of 3-4% and liquid alkali, and finally leaching by using pure water;
7) performing primary concentration, namely filtering and concentrating the feed liquid obtained in the step 6 by using a membrane, and inputting the feed liquid into a flash tank for heating and concentrating to keep the concentration of discharged materials at 30-32%;
8) inputting the feed liquid obtained in the step (7) into an enzymolysis tank, and adding xylanase for enzymolysis;
9) performing secondary decolorization, namely adding powdered activated carbon into the feed liquid obtained in the step 8 for decolorization treatment to obtain feed liquid with the light transmittance of more than 30%;
10) performing secondary ion exchange, namely performing ion exchange on the feed liquid obtained in the step 9, wherein the conductivity after ion exchange is less than 500 mu s/cm, the pH value is 3-5, and the light transmittance is more than 90%; then putting the mixture into hydrochloric acid with the concentration of 3-4% and liquid alkali for regeneration, and finally leaching the mixture with pure water;
11) and (4) performing secondary concentration, namely performing ultrafiltration on the feed liquid obtained in the step (10) for concentration to obtain a finished xylose solution product with the concentration of 70-75%.
Further, the vapor-liquid separator in the step 3 is provided with waste heat recovery, and the obtained steam is used in the flash tank in the step 7 for material heating and concentration.
Furthermore, in the step 4, the ratio of the xylanase to the material is that 3-5kg of xylanase is added to each ton of dry matter.
Further, the enzymolysis condition in the step 4 is that the temperature is 48-50 ℃, and the enzymolysis time is 16 h.
Further, in step 4, the solution after enzymolysis is heated to more than 80 ℃ for enzyme deactivation, and the solution enters the next step of treatment after being kept warm for half an hour.
Further, in the step 8, the ratio of the xylanase to the material is that 3-5kg of xylanase is added to each ton of dry matter, the temperature is controlled at 48-50 ℃ during enzymolysis, and the temperature is raised to more than 80 ℃ for enzyme deactivation after enzymolysis is carried out for 8-10 h.
The invention has the beneficial effects that:
the method firstly expands the raw material source of the xylo-oligosaccharide and verifies the effectiveness of the process for producing the xylo-oligosaccharide from the hemicellulose; secondly, the waste heat utilization problem of cooking is solved; in the prior art, waste heat after intermittent cooking has no utilization value and can only be directly discharged and treated, and the waste heat continuously liquefied by the technology is used for concentrating materials subjected to primary ion exchange, so that the energy consumption is reduced, the pollution of the energy consumption to the surrounding environment is reduced, and great economic benefit and social benefit are generated; thirdly, improving the quality of the xylo-oligosaccharide liquid glucose; the raw material is corncob powder, the content of the xylo-oligosaccharide produced by the corncob powder can only reach about 70 percent, and the content of the xylo-oligosaccharide syrup produced by the hemicellulose can reach more than 80 percent; fourthly, acid and alkali consumption and sewage discharge are reduced. As the corncob powder used as the raw material in the prior art contains a large amount of impurities, the syrup pigment and ions after enzymolysis are more, the impurities contained in the semi-fiber powder are less, the sugar liquid after enzymolysis has better quality, and the acid and alkali consumption and the sewage discharge can be reduced by about 30 percent.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A method for producing xylooligosaccharide by continuous cooking and coupling enzyme method of hemicellulose powder comprises the following steps:
1) mixing the slurry, firstly, the total volume is 2m3The syrup tank is added with pure water of 1m30.2kg of glacial acetic acid, then 100kg of hemicellulose powder with water content of 8-10 percent is added, the temperature is raised to 70-80 ℃, and the mixture is stirred and mixed evenly.
2) And (3) continuously liquefying, starting a primary injection pump (before starting the primary injection pump, confirming that all pipeline valves from the size mixing tank to the saccharification tank are opened), conveying the hemicellulose powder suspension obtained in the step (1) to a liquefaction ejector, simultaneously opening a steam valve of the liquefaction ejector, carrying out steam heating on the material, ensuring that the steam pressure of the liquefaction ejector is 0.8-1.0MPa, keeping the temperature of the material at about 180-200 ℃, and then injecting the material to a steam-liquid separator.
3) And (3) separating residues and liquid, namely feeding the raw materials treated in the step (2) into a gas-liquid separator for separation, setting waste heat recovery in the gas-liquid separator, and using the obtained steam in a flash tank in the step (7) for concentrating materials in a waste heat evaporator after primary ion exchange. And the material subjected to vapor-liquid separation enters a plate frame for slag-liquid separation, and the filtrate is pumped into a saccharification tank.
4) Performing primary enzymolysis, and inputting the liquid obtained by separation in the step 3 into a total volume of 2m3After the saccharification tank is finished, when the liquid level reaches 80 percent, the tank is closedClosing a feeding valve, cooling to 48-50 ℃, adding 0.4kg of xylanase, and carrying out enzymolysis for 16 h.
5) And (4) primary decolorization, namely detecting the content of xylo-oligosaccharide in sugar liquor in the enzymolysis tank after the enzymolysis in the step (4) is finished, confirming the purity of the xylo-oligosaccharide, and then heating to more than 80 ℃ for enzyme deactivation. Keeping the enzyme deactivation temperature for more than half an hour, then conveying the materials to a plate frame for filtration, adding powdered activated carbon into filtrate for decolorization and removal treatment, wherein the light transmittance is more than 20%.
6) Performing primary ion exchange, namely performing ion exchange on the feed liquid obtained in the step 5, wherein the cation resin in the ion exchange column is 001 x 7, and the anion resin in the ion exchange column is D301; the metal cations in the feed liquid are replaced by hydrogen ions in the resin, acid radical ions and hydroxide ions, the conductivity after ion exchange is less than 500 mu s/cm, the PH value is 3-5, and the light transmittance is more than 90 percent; after the ion exchange is failed, the positive column is put into hydrochloric acid with the concentration of 3-4% for regeneration, the negative column is put into liquid alkali with the concentration of 3-4% for regeneration, and finally, the pure water is used for leaching.
7) And (3) primary concentration, namely performing membrane concentration on the sugar solution subjected to ion exchange in the step (6), and then performing concentration by using a waste heat evaporator (heating by using secondary steam of continuous cooking flash evaporation), wherein the discharge concentration is 20-25%.
8) Secondary enzymolysis, the concentrated material in step 7 is fed into a secondary enzymolysis tank (2 m)3) When the liquid level reaches 0.5kg, xylanase is added, the temperature is reduced to 48-50 ℃, secondary enzymolysis is carried out, and the enzymolysis lasts for 16 hours.
9) And (3) secondary decolorization, namely adding powdered activated carbon into the feed liquid obtained in the step (8) for decolorization, so that the light transmittance of the feed liquid after decolorization and filtration is more than 30%.
10) Performing secondary ion exchange, namely performing secondary ion exchange on the material subjected to secondary decolorization in the step 9, wherein the conductivity after ion exchange is less than 20 mu s/cm, the pH value is 4-7, the light transmittance is more than 90%, and the feeding flow is controlled to be 2 times of the volume of the resin; after the exchange is finished, water is used for jacking until the refraction is less than 1%, then regeneration is carried out, hydrochloric acid is used for the positive column, liquid alkali is used for the negative column, waste acid and alkali are discharged after the negative column is soaked for 3 hours, then washing is carried out by pure water, the washing end point of the positive column is 3-3.5, the washing end point of the negative column is 9.5-10, and the washing is reserved; hydrochloric acid and liquid alkali are used for regeneration, the concentration is 3-4%, and the conductivity of the eluted pure water is less than 50 mu s/cm.
11) And (3) performing secondary concentration, namely performing ultrafiltration on the sugar solution subjected to ion exchange in the step (10), returning the concentrated solution to a secondary decoloring tank, performing secondary concentration on the permeate, wherein the discharge concentration is 70-75%, and filling the concentrated material into a finished product.
Finally, the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting, and other modifications or equivalent substitutions made by the technical solutions of the present invention by those of ordinary skill in the art should be covered within the scope of the claims of the present invention as long as they do not depart from the spirit and scope of the technical solutions of the present invention.
Claims (6)
1. A method for producing xylooligosaccharide by a hemicellulose powder continuous liquefaction coupling enzyme method is characterized by comprising the following steps:
1) mixing pulp, namely putting the hemicellulose and 0.2% acetic acid aqueous solution in a mass ratio of 1:10 into a pulp mixing tank, heating to 90-100 ℃, and stirring and mixing uniformly to form a hemicellulose powder suspension;
2) continuously liquefying, namely conveying the hemicellulose powder suspension liquid obtained in the step (1) to a liquefying ejector, ensuring that the steam pressure of the liquefying ejector is 0.8-1.0MPa, keeping the temperature of the materials at 180-;
3) separating slag and liquid, namely conveying the raw materials treated in the step 2 into a plate frame for separating slag and liquid;
4) carrying out primary enzymolysis, inputting the liquid obtained by separation in the step 3 into an enzymolysis tank, adding xylanase, and carrying out enzymolysis;
5) primary decolorization, namely filtering the material subjected to enzymolysis treatment in the step 4, and adding powdered activated carbon into filtrate for decolorization to obtain feed liquid with the light transmittance of more than 20%;
6) performing primary ion exchange, wherein the feed liquid obtained in the step 5 is subjected to ion exchange, the conductivity of the feed liquid after ion exchange is less than 500 mu s/cm, the pH value is 3-5, and the light transmittance is more than 90%; regenerating the ion exchange column after the ion exchange column is invalid by using hydrochloric acid with the concentration of 3-4% and liquid alkali, and finally leaching by using pure water;
7) performing primary concentration, namely filtering and concentrating the feed liquid obtained in the step 6 by using a membrane, and inputting the feed liquid into an evaporator for heating and concentrating to keep the concentration of discharged materials at 30-32%;
8) inputting the feed liquid obtained in the step (7) into an enzymolysis tank, and adding xylanase for enzymolysis;
9) secondary decolorization, namely adding powdered activated carbon into the filtrate obtained in the step 8 for decolorization treatment to obtain feed liquid with the light transmittance of more than 30%;
10) performing secondary ion exchange, namely performing ion exchange on the feed liquid obtained in the step 9, wherein the conductivity of the feed liquid after ion exchange is less than 50 mu s/cm, the pH value is 5-7, and the light transmittance is more than 90%; regenerating the ion exchange column after the ion exchange column is invalid by using hydrochloric acid with the concentration of 3-4% and liquid alkali, and finally leaching by using pure water;
11) and (4) performing secondary concentration, namely performing ultrafiltration on the feed liquid obtained in the step (10) for concentration to obtain a finished xylose solution product with the concentration of 70-75%.
2. The method for producing xylooligosaccharide by using the hemicellulose powder continuous liquefaction coupled enzyme method according to claim 1, wherein the method comprises the following steps: and (4) setting waste heat recovery for the steam-liquid separator in the step (3), and using the obtained steam in the flash tank in the step (7) for material heating and concentration.
3. The method for producing xylooligosaccharide by using the hemicellulose powder continuous liquefaction coupled enzyme method according to claim 1, wherein the method comprises the following steps: in the step 4, the ratio of the xylanase to the material is that 3-5kg of xylanase is added to each ton of the material.
4. The method for producing xylooligosaccharide by using the hemicellulose powder continuous liquefaction coupled enzyme method according to claim 1, wherein the method comprises the following steps: the enzymolysis condition in the step 4 is 48-50 ℃, and the enzymolysis time is 16 h.
5. The method for producing xylooligosaccharide by using the hemicellulose powder continuous liquefaction coupled enzyme method according to claim 1, wherein the method comprises the following steps: in step 4, the solution after enzymolysis is heated to more than 80 ℃ for enzyme deactivation, and the next step of treatment is carried out after the solution is kept warm for half an hour.
6. The method for producing xylooligosaccharide by using the hemicellulose powder continuous liquefaction coupled enzyme method according to claim 1, wherein the method comprises the following steps: in the step 8, the ratio of the xylanase to the material is that 3-5kg of xylanase is added to each ton of the material, the temperature is controlled at 48-50 ℃ during enzymolysis, the temperature is raised to more than 80 ℃ after enzymolysis is carried out for 8-10h, and enzyme deactivation is carried out.
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Citations (3)
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|---|---|---|---|---|
| KR20050097878A (en) * | 2004-04-05 | 2005-10-10 | 산동 롱라이브 바이오-테크놀로지 컴퍼니 리미티드 | Method for preparing xylooligosaccharide |
| JP2008136376A (en) * | 2006-11-30 | 2008-06-19 | Oji Paper Co Ltd | Method for producing acidic xylooligosaccharide |
| CN103589761A (en) * | 2013-11-08 | 2014-02-19 | 无锡群硕谷唐生物科技有限公司 | Method for preparing xylooligosaccharide by wheat bran and product obtained by method |
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- 2020-11-09 CN CN202011238721.8A patent/CN112301077A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20050097878A (en) * | 2004-04-05 | 2005-10-10 | 산동 롱라이브 바이오-테크놀로지 컴퍼니 리미티드 | Method for preparing xylooligosaccharide |
| JP2008136376A (en) * | 2006-11-30 | 2008-06-19 | Oji Paper Co Ltd | Method for producing acidic xylooligosaccharide |
| CN103589761A (en) * | 2013-11-08 | 2014-02-19 | 无锡群硕谷唐生物科技有限公司 | Method for preparing xylooligosaccharide by wheat bran and product obtained by method |
Non-Patent Citations (1)
| Title |
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| 王灿: "低聚木糖对纤维素原料酶解影响和机制的研究", 万方数据库, pages 1 - 91 * |
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