CN111334542B - Method for preparing xylo-oligosaccharide from cornstalk cores - Google Patents
Method for preparing xylo-oligosaccharide from cornstalk cores Download PDFInfo
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- HEBKCHPVOIAQTA-NGQZWQHPSA-N d-xylitol Chemical compound OC[C@H](O)C(O)[C@H](O)CO HEBKCHPVOIAQTA-NGQZWQHPSA-N 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 38
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000010902 straw Substances 0.000 claims abstract description 40
- 240000008042 Zea mays Species 0.000 claims abstract description 38
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims abstract description 38
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims abstract description 38
- 235000005822 corn Nutrition 0.000 claims abstract description 38
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 239000011347 resin Substances 0.000 claims abstract description 18
- 229920005989 resin Polymers 0.000 claims abstract description 18
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 15
- 102000004190 Enzymes Human genes 0.000 claims abstract description 6
- 108090000790 Enzymes Proteins 0.000 claims abstract description 6
- 238000000746 purification Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 27
- 229920001221 xylan Polymers 0.000 claims description 26
- 150000004823 xylans Chemical class 0.000 claims description 26
- 239000007788 liquid Substances 0.000 claims description 23
- 239000000843 powder Substances 0.000 claims description 20
- 239000003729 cation exchange resin Substances 0.000 claims description 19
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 17
- 239000003957 anion exchange resin Substances 0.000 claims description 17
- 239000002244 precipitate Substances 0.000 claims description 14
- 230000007071 enzymatic hydrolysis Effects 0.000 claims description 11
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 claims description 11
- 150000001450 anions Chemical class 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- 239000006228 supernatant Substances 0.000 claims description 10
- 239000002023 wood Substances 0.000 claims description 9
- 101710121765 Endo-1,4-beta-xylanase Proteins 0.000 claims description 8
- 238000005520 cutting process Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 8
- 238000001179 sorption measurement Methods 0.000 claims description 8
- 238000000967 suction filtration Methods 0.000 claims description 8
- 238000011033 desalting Methods 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 7
- 238000001556 precipitation Methods 0.000 claims description 7
- 238000002390 rotary evaporation Methods 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 6
- 238000004042 decolorization Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 230000009849 deactivation Effects 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 150000001768 cations Chemical class 0.000 claims 2
- 239000002994 raw material Substances 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 3
- 229920005610 lignin Polymers 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 239000000413 hydrolysate Substances 0.000 abstract description 2
- 229920001542 oligosaccharide Polymers 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 150000002482 oligosaccharides Chemical class 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 14
- 238000004128 high performance liquid chromatography Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 230000035484 reaction time Effects 0.000 description 5
- 230000008569 process Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 235000013372 meat Nutrition 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 241000609240 Ambelania acida Species 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 208000008589 Obesity Diseases 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 244000082204 Phyllostachys viridis Species 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 description 1
- 238000005903 acid hydrolysis reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000010905 bagasse Substances 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 235000005911 diet Nutrition 0.000 description 1
- 230000000378 dietary effect Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 238000012869 ethanol precipitation Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000019261 food antioxidant Nutrition 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 description 1
- 235000020824 obesity Nutrition 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000010907 stover Substances 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
- 239000000811 xylitol Substances 0.000 description 1
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 description 1
- 229960002675 xylitol Drugs 0.000 description 1
- 235000010447 xylitol Nutrition 0.000 description 1
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- 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
- C12P19/14—Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
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- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/04—Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
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Abstract
The invention relates to the field of xylo-oligosaccharide, in particular to a method for preparing xylo-oligosaccharide by utilizing cornstalk cores. The raw material adopted by the invention is corn straw pulp, alkaline hydrogen peroxide is utilized to primarily hydrolyze and remove lignin, then hydrolysate is desalted and pH environment is adjusted, and finally, enzymolysis method is adopted to further hydrolyze to obtain xylo-oligosaccharide solution. In order to further improve the purity of oligosaccharide, activated carbon is combined with decolorizing resin for purification treatment. The method of the invention has the advantages of simple preparation process, mild reaction and environmental protection, and the obtained xylo-oligosaccharide has high purity and yield, and the dosage of enzyme is less during the subsequent enzymolysis method, thereby saving the cost.
Description
Technical Field
The invention relates to the field of xylo-oligosaccharide, in particular to a method for preparing xylo-oligosaccharide by utilizing cornstalk cores.
Background
Agricultural and forestry biomass materials such as corn stover, wheat straw, corn cobs, bagasse, rice straw, bamboo, and the like, have potential utility values in many respects. Some countries have achieved great success in using these biomass by-products to produce high value added products. China is a big agricultural country, and corn is one of the food crops in China and has rich resources. The cornstalk bark part is widely applied to the fields of laminated wood and flakeboards, but the produced pith cannot be fully utilized. The corn straw pulp is used as a raw material to develop some new purposes, such as producing functional xylo-oligosaccharide, so that the corn straw is fully utilized, the income of farmers is increased, and the method has great prospect.
Due to the unique properties and functions, the xylo-oligosaccharide is widely applied to the fields of food and pharmacy, is a good dietary therapy additive for patients with diabetes, obesity and other rich and noble diseases, is mainly used for producing xylitol, meat processing, meat flavor, preparing food antioxidant and the like, and has great social and economic benefits.
In the aspects of research and application of xylo-oligosaccharide, China starts late, and some defects exist in the aspects of technology and equipment. Briefly, the preparation principle of xylo-oligosaccharide is as follows: taking a raw material rich in xylan, hydrolyzing the glycosidic bond of the raw material to obtain low-polymerization-degree saccharides, namely xylo-oligosaccharide. The traditional method for preparing the xylo-oligosaccharide has high requirements on equipment, complex process and even produces some byproducts by an acid hydrolysis method and a hot water extraction method, thereby reducing the yield of the xylo-oligosaccharide.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a novel method for preparing xylo-oligosaccharide from cornstalk cores. The raw material adopts cornstalk pith, firstly, the lignin is removed by oxidation pretreatment under the alkaline condition, secondly, the components of the treatment solution are adjusted, the complexity of the treatment solution is reduced, and finally, the xylo-oligosaccharide is obtained by hydrolysis by an enzymolysis method. The method has low requirements on equipment, is simple to operate, and further improves the yield and purity of the xylo-oligosaccharide.
The method for preparing xylo-oligosaccharide mainly comprises the processes of crushing cornstalk medulla, oxidation pretreatment, pretreatment liquid component adjustment, enzyme hydrolysis, enzyme inactivation, decoloration and the like.
A method for preparing xylo-oligosaccharide from corn straw cores comprises the following steps:
(1) pulverizing
The method comprises the steps of selecting dry and moldless corn straws, carrying out untwining and peeling to obtain corn straw cores, cutting the cores into small sections, and crushing the small sections by using a crusher for later use.
(2) Oxidative pretreatment
Taking corn straw pulp powder, adding a hydrogen peroxide solution with the mass fraction of 0.5-4%, controlling the solid-to-liquid ratio to be 1: 10-1: 30(g/mL), adjusting the pH value of the solution to 11-12 by using an alkali liquor with the mass fraction of 0.5-4%, reacting at the temperature of 60-85 ℃ for 2-8 h, performing suction filtration after the reaction is finished to achieve solid-liquid separation, and collecting filtrate to obtain a pretreatment solution.
(3) Pretreatment liquid composition adjustment
And (3) carrying out a desalting step by using anion and cation exchange resin, and then adjusting the pH value of the pretreatment solution to 6.
(4) Enzymatic hydrolysis
Performing rotary evaporation on the solution in the step (3) by using a rotary evaporator, then precipitating by using ethanol, and drying the solid to obtain xylan solid; the enzymatic hydrolysis of xylan is carried out in a constant temperature shaking table at 35-55 ℃ to prepare a xylan solution with the mass concentration of 10-13%, the addition amount of xylanase is 300-600 IU/g, and the enzymolysis time is 8-24 h, thus obtaining the enzymatic hydrolysate.
(5) Enzyme deactivation
And (4) preserving the temperature of the enzymolysis liquid in the step (4) for 15min at 80 ℃, then centrifuging by using a centrifuge, centrifuging for 10min at 3000rpm, and taking supernatant.
(6) Purification of
And (5) carrying out double decolorization on the supernatant obtained in the step (5) by using activated carbon and decolorizing resin to obtain a xylo-oligosaccharide solution for later use.
Preferably, the alkali used in step (2) is one of sodium hydroxide and potassium hydroxide.
Preferably, the cation exchange resin type in step (3) is a 732 type cation exchange resin, and the anion exchange resin type is a D301-FD type anion exchange resin. By adopting an anion-cation resin series connection method, the volume ratio of anion-cation resin to cation-anion resin is 2: 1, the operation temperature is 50 ℃, the pH value is 6.0, and the time is 60 min.
Preferably, in the step (4), the solution is evaporated to one third of the original volume by using a rotary evaporator, and then ethanol precipitation is carried out by adding ethanol solution with the mass fraction of 95% and 3 times of the residual volume, and the precipitate is collected.
Preferably, the double decolorization in the step (6) refers to firstly decolorizing with activated carbon, selecting wood dry carbon powder, wherein the addition amount is 0.04g/mL, the temperature is 50 ℃, and the adsorption time is 50 min; and (4) treating the xylo-oligosaccharide solution treated by the activated carbon by using anion-cation exchange resin in the same step (3).
The invention has the advantages that:
1. in the invention, the corn straw pulp core which is not fully utilized at present is utilized as the raw material, and the raw material has wide sources, is a raw material rich in xylan, and is suitable for producing xylo-oligosaccharide.
2. In the invention, the alkaline hydrogen peroxide method not only has the effects of removing lignin and bleaching, but also increases the dissolution degree of hemicellulose and improves the purity and yield of xylo-oligosaccharide.
3. Salt component treatment and pH environment adjustment are carried out before enzymolysis, so that the reaction environment of the enzyme preparation is further improved, and the yield of the product is improved. Then enzymolysis is carried out by an enzymolysis method, the operation process is simple, the reaction condition is mild, the requirement on equipment is not strict, and the method is environment-friendly and convenient for industrial production.
Drawings
FIG. 1 is a flow chart of the production process described in this application.
Detailed Description
The following examples are intended to illustrate the invention, but are not intended to limit the scope of the invention.
Example 1
1) The method comprises the steps of selecting dry and moldless corn straws, carrying out untwining and peeling to obtain corn straw cores, cutting the cores into small sections, and crushing the small sections into powder for later use by a crusher.
2) Taking the crushed corn straw pulp core powder, and mixing the crushed corn straw pulp core powder according to a solid-liquid ratio of 1:10 (g/mL) of hydrogen peroxide solution with the mass fraction of 0.5 percent is added, and the pH value is adjusted to 11 by sodium hydroxide solution with the mass fraction of 0.5 percent, the reaction temperature is 60 ℃, and the reaction time is 2 hours. And after the reaction is finished, carrying out suction filtration, and collecting filtrate to obtain a pretreatment solution.
3) Desalting the pretreatment solution in the step 2) and adjusting pH: the 732 type cation exchange resin and the D301-FD type anion exchange resin are used for a series connection method, and the volume ratio of the cation-anion resin to the cation-anion resin is 2: 1, the operation temperature is 50 ℃, the pH value is 6.0, and the time is 60 min.
4) Evaporating the solution in the step 3) to one third of the original volume by using a rotary evaporator, then adding an ethanol solution which is 3 times of the original volume and has a mass fraction of 95% for alcohol precipitation, collecting the precipitate, and drying the precipitate to obtain a xylan solid; and (3) carrying out enzymatic hydrolysis on xylan in a constant-temperature shaking table at 35 ℃ to prepare a xylan solution with the mass concentration of 10%, wherein the addition amount of xylanase is 300IU/g, and the enzymolysis time is 8 hours to obtain an enzymolysis solution.
5) Preserving the temperature of the enzymolysis liquid in the step 4) at 80 ℃ for 15min, then centrifuging by using a centrifuge at 3000rpm for 10min, and taking supernatant.
6) Treating the solution in the step 4) with activated carbon, selecting wood dry carbon powder, wherein the addition amount of the activated carbon is 0.04g/mL, the temperature is 50 ℃, and the adsorption time is 50 min; and (4) treating the solution treated by the activated carbon by using anion and cation exchange resin, and obtaining the xylo-oligosaccharide solution in the same step (3).
7) The conversion rate of the xylo-oligosaccharide is 21.98 percent by the high performance liquid chromatography determination of the xylo-oligosaccharide solution.
Example 2
1) The method comprises the steps of selecting dry and moldless corn straws, carrying out untwining and peeling to obtain corn straw cores, cutting the cores into small sections, and crushing the small sections into powder for later use by a crusher.
2) Taking the crushed corn straw pulp core powder, and mixing the crushed corn straw pulp core powder according to a solid-liquid ratio of 1: 20(g/mL) of the solution is added with 1.5 percent of hydrogen peroxide solution by mass fraction, and 1.5 percent of sodium hydroxide solution by mass fraction is used for adjusting the pH value to 11.6, the reaction temperature is 70 ℃, and the reaction time is 4 hours. And after the reaction is finished, carrying out suction filtration, and collecting filtrate to obtain a pretreatment solution.
3) Desalting the pretreatment solution in the step 2) and adjusting pH: the 732 type cation exchange resin and the D301-FD type anion exchange resin are used for a series connection method, and the volume ratio of the cation-anion resin to the cation-anion resin is 2: 1, the operation temperature is 50 ℃, the pH value is 6.0, and the time is 60 min.
4) Carrying out rotary evaporation on the solution in the step 2) by using a rotary evaporator, evaporating the volume of the solution to one third of the original volume, then adding an ethanol solution which is 3 times of the original volume and has a mass fraction of 95% for alcohol precipitation, collecting the precipitate, and drying the precipitate to obtain a xylan solid; and (3) carrying out enzymatic hydrolysis on xylan in a constant-temperature shaking table at 45 ℃ to prepare a xylan solution with the mass concentration of 13%, wherein the addition amount of xylanase is 400IU/g, and the enzymolysis time is 6 hours, so as to obtain an enzymolysis liquid.
5) Preserving the temperature of the enzymolysis liquid in the step 3) at 80 ℃ for 15min, then centrifuging by using a centrifuge at 3000rpm for 10min, and taking supernatant.
6) Decoloring the solution in the step 4) by using activated carbon, selecting wood dry carbon powder, wherein the addition amount is 0.04g/mL, the temperature is 50 ℃, and the adsorption time is 50 min; and (4) treating the solution treated by the activated carbon by using anion and cation exchange resin, and obtaining the xylo-oligosaccharide solution in the same step (3).
7) The conversion rate of the xylo-oligosaccharide is 22.79 percent by the high performance liquid chromatography determination of the xylo-oligosaccharide solution.
Example 3
1) The method comprises the steps of selecting dry and moldless corn straws, carrying out untwining and peeling to obtain corn straw cores, cutting the cores into small sections, and crushing the small sections into powder for later use by a crusher.
2) Taking the crushed corn straw pulp core powder, and mixing the crushed corn straw pulp core powder according to a solid-liquid ratio of 1: adding 2 percent by mass of hydrogen peroxide solution into the mixture according to the amount of 25, and adjusting the pH value to 11.6 by using 2 percent by mass of sodium hydroxide solution, wherein the reaction temperature is 75 ℃ and the reaction time is 4 hours. And after the reaction is finished, carrying out suction filtration, and collecting filtrate to obtain a pretreatment solution.
3) Desalting the pretreatment solution in the step 2) and adjusting pH: the 732 type cation exchange resin and the D301-FD type anion exchange resin are used for a series connection method, and the volume ratio of the cation-anion resin to the cation-anion resin is 2: 1, the operation temperature is 50 ℃, the pH value is 6.0, and the time is 60 min.
4) Carrying out rotary evaporation on the solution obtained in the step 3) by using a rotary evaporator, evaporating the volume of the solution to one third of the original volume, then adding an ethanol solution which is 3 times of the volume and has the mass fraction of 95% for carrying out alcohol precipitation, collecting the precipitate, and drying the precipitate to obtain xylan solid; and (3) carrying out enzymatic hydrolysis on xylan in a constant-temperature shaking table at 52 ℃ to prepare a xylan solution with the mass concentration of 11%, wherein the addition amount of xylanase is 500IU/g, and the enzymolysis time is 8 hours to obtain an enzymolysis solution.
5) Preserving the temperature of the enzymolysis liquid in the step 4) at 80 ℃ for 15min, then centrifuging by using a centrifuge at 3000rpm for 10min, and taking supernatant.
6) Decoloring the solution in the step 4) by using activated carbon, selecting wood dry carbon powder, wherein the addition amount is 0.04g/mL, the temperature is 50 ℃, and the adsorption time is 50 min; and (4) treating the solution treated by the activated carbon by using anion and cation exchange resin, and obtaining the xylo-oligosaccharide solution in the same step (3).
7) The conversion rate of the xylo-oligosaccharide is 24.83 percent by the determination of the high performance liquid chromatography of the xylo-oligosaccharide solution.
Comparative example 1
The operation of this comparative example is that the straw pulp core is not treated with alkali in step (2).
1) The method comprises the steps of selecting dry and moldless corn straws, carrying out untwining and peeling to obtain corn straw cores, cutting the cores into small sections, and crushing the small sections into powder for later use by a crusher.
2) Taking the crushed corn straw pulp core powder, and mixing the crushed corn straw pulp core powder according to a solid-liquid ratio of 1: 25(g/mL) of a hydrogen peroxide solution with the mass fraction of 2 percent is added, the reaction temperature is 75 ℃, and the reaction time is 4 hours. And after the reaction is finished, carrying out suction filtration, and collecting filtrate to obtain a pretreatment solution.
3) Desalting the pretreatment solution in the step 2) and adjusting pH: the 732 type cation exchange resin and the D301-FD type anion exchange resin are used for a series connection method, and the volume ratio of the cation-anion resin to the cation-anion resin is 2: 1, the operation temperature is 50 ℃, the pH value is 6.0, and the time is 60 min.
4) Carrying out rotary evaporation on the solution in the step 3) by using a rotary evaporator, evaporating the volume of the solution to one third of the original volume, then adding an ethanol solution which is 3 times of the volume and has the mass fraction of 95% for alcohol precipitation, collecting the precipitate, and drying the precipitate to obtain a xylan solid; and (3) carrying out enzymatic hydrolysis on xylan in a constant-temperature shaking table at 52 ℃ to prepare a xylan solution with the mass concentration of 11%, wherein the addition amount of xylanase is 500IU/g, and the enzymolysis time is 8 hours to obtain an enzymolysis solution.
5) Preserving the temperature of the enzymolysis liquid in the step 4) for 15min at 80 ℃, and then separating by using a centrifugal machine to obtain supernatant.
6) Decoloring the solution in the step 4) by using activated carbon, selecting wood dry carbon powder, wherein the addition amount is 0.04g/mL, the temperature is 50 ℃, and the adsorption time is 50 min; and (4) treating the solution treated by the activated carbon by using anion and cation exchange resin, and obtaining the xylo-oligosaccharide solution in the same step (3).
7) The conversion rate of the xylo-oligosaccharide is 19.23 percent by the high performance liquid chromatography determination of the xylo-oligosaccharide solution.
Comparative example 2
The operation of the comparative example is that the straw pulp core is not treated by adding hydrogen peroxide in the step (2), namely single alkali pretreatment.
1) The method comprises the steps of selecting dry and moldless corn straws, carrying out untwining and peeling to obtain corn straw cores, cutting the cores into small sections, and crushing the small sections into powder for later use by a crusher.
2) Taking the crushed corn straw pulp core powder, and mixing the crushed corn straw pulp core powder according to a solid-liquid ratio of 1: 25(g/mL) of sodium hydroxide solution with the mass fraction of 4 percent is added, the reaction temperature is 75 ℃, and the reaction time is 4 hours. And after the reaction is finished, carrying out suction filtration, and collecting filtrate to obtain a pretreatment solution.
3) Desalting the pretreatment solution in the step 2) and adjusting pH: the 732 type cation exchange resin and the D301-FD type anion exchange resin are used for a series connection method, and the volume ratio of the cation-anion resin to the cation-anion resin is 2: 1, the operation temperature is 50 ℃, the pH value is 6.0, and the time is 60 min.
4) Carrying out rotary evaporation on the solution in the step 3) by using a rotary evaporator, evaporating the volume of the solution to one third of the original volume, then adding an ethanol solution which is 3 times of the volume and has the mass fraction of 95% for alcohol precipitation, collecting the precipitate, and drying the precipitate to obtain a xylan solid; and (3) carrying out enzymatic hydrolysis on xylan in a constant-temperature shaking table at 52 ℃ to prepare a xylan solution with the mass concentration of 11%, wherein the addition amount of xylanase is 500IU/g, and the enzymolysis time is 8 hours to obtain an enzymolysis solution.
5) Preserving the temperature of the enzymolysis liquid in the step 4) at 80 ℃ for 15min, then centrifuging by using a centrifuge at 3000rpm for 10min, and taking supernatant.
6) Decoloring the solution in the step 5) by using activated carbon, selecting wood dry carbon powder, wherein the addition amount is 0.04g/mL, the temperature is 50 ℃, and the adsorption time is 50 min; and (4) treating the solution treated by the activated carbon by using anion and cation exchange resin, and obtaining the xylo-oligosaccharide solution in the same step (3).
7) The conversion rate of xylo-oligosaccharide is 19.84 percent by high performance liquid chromatography.
Comparative example 3
The operation of this comparative example was such that the straw cores were not subjected to the prehydrolysis liquid component treatment of step (3).
1) The method comprises the steps of selecting dry and moldless corn straws, carrying out untwining and peeling to obtain corn straw cores, cutting the cores into small sections, and crushing the small sections into powder for later use by a crusher.
2) Taking the crushed corn straw pulp core powder, and mixing the crushed corn straw pulp core powder according to a solid-liquid ratio of 1: adding 2% hydrogen peroxide solution by mass fraction into 25(g/mL), adjusting the pH value to 11.6 by using 2% sodium hydroxide solution by mass fraction, reacting at 75 ℃ for 4 h. And after the reaction is finished, carrying out suction filtration, and collecting filtrate to obtain a pretreatment solution.
3) Carrying out rotary evaporation on the solution obtained in the step 2) by using a rotary evaporator, evaporating the volume of the solution to one third of the original volume, then adding an ethanol solution which is 3 times of the original volume and has a mass fraction of 95% for alcohol precipitation, collecting the precipitate, and drying the precipitate to obtain a xylan solid; and (3) carrying out enzymatic hydrolysis on xylan in a constant-temperature shaking table at 52 ℃ to prepare a xylan solution with the mass concentration of 11%, wherein the addition amount of xylanase is 500IU/g, and the enzymolysis time is 8 hours to obtain an enzymolysis solution.
4) Preserving the temperature of the enzymolysis liquid in the step 3) at 80 ℃ for 15min, then centrifuging by using a centrifuge at 3000rpm for 10min, and taking supernatant.
5) Decoloring the solution in the step 4) by using activated carbon, selecting wood dry carbon powder, wherein the addition amount is 0.04g/mL, the temperature is 50 ℃, and the adsorption time is 50 min; and (4) treating the solution treated by the activated carbon by using anion and cation exchange resin, and obtaining the xylo-oligosaccharide solution in the same step (3).
6) The conversion rate of xylo-oligosaccharide is 17.84% by high performance liquid chromatography.
The yield and purity of xylo-oligosaccharide obtained from examples 1-3 and comparative examples 1-3 are shown in Table 1:
TABLE 1
| Conversion rate% | Purity% | |
| Example 1 | 21.98％ | 87.12％ |
| Example 2 | 22.79％ | 86.79％ |
| Example 3 | 22.83％ | 86.15％ |
| Comparative example 1 | 19.23％ | 84.66％ |
| Comparative example 2 | 19.84％ | 73.26％ |
| Comparative example 3 | 17.84％ | 70.54％ |
As can be seen from Table 1, by comparing the comparative example with the examples, the method of the present invention not only improves the yield of xylo-oligosaccharide, but also improves the purity of the product; example 3 compared to comparative example 1, the addition of base during pretreatment affects the conversion of xylo-oligosaccharides; example 3 compared to comparative example 2, the addition of hydrogen peroxide has a great influence on the purity of xylo-oligosaccharide; example 3 compared to comparative example 3, salt component treatment and pH environment adjustment prior to enzymatic hydrolysis not only improved purity but also significantly improved conversion.
The foregoing is only an embodiment of the present invention, and it should be noted that some modifications or improvements may be made on the basis of the present invention. Thus, it is intended that all such modifications and variations be included within the scope of the invention as claimed and protected by the accompanying claims.
Claims (1)
1. A method for preparing xylo-oligosaccharide from cornstalk medulla, which is characterized by comprising the following steps:
(1) pulverizing
Selecting dry and moldless corn straws, untwining and peeling to obtain corn straw cores, cutting the cores into small sections, and crushing the small sections by using a crusher for later use;
(2) oxidative pretreatment
Taking corn straw pulp powder, adding a hydrogen peroxide solution with the mass fraction of 0.5-4%, controlling the solid-to-liquid ratio to be 1: 10-1: 30g/mL, adjusting the pH value of the solution to 11-12 by using an alkali liquor with the mass fraction of 0.5-4%, performing suction filtration after the reaction is finished to achieve solid-liquid separation, and collecting filtrate to obtain a pretreatment solution;
(3) pretreatment liquid composition adjustment
Desalting with anion and cation exchange resin, and adjusting pH to 6;
(4) enzymatic hydrolysis
Performing rotary evaporation on the solution in the step (3) by using a rotary evaporator, then precipitating by using ethanol, and drying the solid to obtain xylan solid; performing enzymatic hydrolysis on xylan in a constant-temperature shaking table at 35-55 ℃ to prepare a xylan solution with the mass concentration of 10-13%, wherein the addition amount of xylanase is 300-600 IU/g, and the enzymolysis time is 8-24 h to obtain an enzymolysis solution;
(5) enzyme deactivation
Preserving the temperature of the enzymolysis liquid in the step (4) at 80 ℃ for 15min, then centrifuging by using a centrifuge at 3000rpm for 10min, and taking supernatant;
(6) purification of
Double decoloring the supernatant in the step (5) by using activated carbon and decoloring resin to obtain a xylo-oligosaccharide solution for later use;
in the step (2), potassium hydroxide is used as alkali;
in the step (3), the type of the cation exchange resin is 732 type cation exchange resin, the type of the anion exchange resin is D301-FD type anion exchange resin, an anion and cation resin series connection method is adopted, and the volume ratio of the anion and cation resin is 2: 1, the operation temperature is 50 ℃, the pH value is 6.0, and the time is 60 min;
in the step (4), evaporating the solution to one third of the original volume by using a rotary evaporator, then adding an ethanol solution which is 3 times of the residual volume and has the mass fraction of 95% for alcohol precipitation, and collecting the precipitate;
in the step (6), the double decolorization means that activated carbon is used for decolorization firstly, wood dry carbon powder is selected, the adding amount of the activated carbon is 0.04g/mL, the temperature is 50 ℃, and the adsorption time is 50 min; and (4) treating the xylo-oligosaccharide solution treated by the activated carbon by using anion-cation exchange resin in the same step (3).
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| CN102261007A (en) * | 2010-05-26 | 2011-11-30 | 漳州伯能生物能源有限公司 | Method for grading and separating all components of forestry cellulose biomass and preparing fuel alcohol and xylo-oligosaccharide by utilizing separated components |
| CN102559808A (en) * | 2012-02-20 | 2012-07-11 | 淮阴师范学院 | Method for preparing xylo-oligosaccharide by using corn stalk cores |
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| CN102559808A (en) * | 2012-02-20 | 2012-07-11 | 淮阴师范学院 | Method for preparing xylo-oligosaccharide by using corn stalk cores |
| CN105624337A (en) * | 2016-01-07 | 2016-06-01 | 江苏振宇环保科技有限公司 | Method for preparing xylose functional sugar by hemicellulose polysaccharide in hydrolyzed agricultural wastes |
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