CN105330869A - Hydrolysis method of wood fiber raw material - Google Patents
Hydrolysis method of wood fiber raw material Download PDFInfo
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Abstract
The invention provides a hydrolysis method of a wood fiber raw material. The hydrolysis method comprises the following steps: (1) adding an alkaline water solution of hydrogen peroxide into the wood fiber raw material to react; after the reaction is finished, filtering and separating to obtain filter residues (containing rich holocellulose) and filtrate; (2) after washing the filter residues with water, adding the filter residues into a high-pressure reaction kettle; adding an organic solvent, a catalyst and a catalyst auxiliary agent into the high-pressure reaction kettle to carry out a hydrolysis reaction; after the reaction is finished, filtering, wherein the filtrate contains reduced monosaccharide; (3) adding absolute ethyl alcohol into the filtrate of the step (1) and adjusting the pH value to be 5 to 6 by organic acid; after standing, filtering and separating to obtain filter residues and another kind of filtrate, wherein the filter residues are hemicellulose; taking the filtrate and carrying out rotary evaporation to remove ethanol; then adjusting the pH value to be 1 to 2; standing and then centrifuging, and separating to obtain solids, namely lignin. The wood fiber raw material, provided by the invention, has a simple and feasible process, is environmentally friendly, and has low toxin and high lignin removing and recycling rate; the separated holocellulose has high saccharifying efficiency; the industrialization is easy to realize and the hydrolysis method has a wide application prospect.
Description
Technical field
The present invention relates to agricultural fossil data and utilize technical field, specifically, relate to a kind of method for hydrolysis of lignocellulose raw material.
Background technology
Lignocellulose raw material is renewable resources the abundantest on the earth, adopts appropriate technology that lignocellulose raw material is converted into biomass fuel and biobased products, has very great meaning to the Sustainable development of China's economy and society.In lignocellulose raw material, Mierocrystalline cellulose accounts for 35 ~ 45% of dry weight, and hemicellulose accounts for 20 ~ 40%, and xylogen accounts for 20 ~ 30%.Wherein utilizing the Mierocrystalline cellulose in biomass, hemicellulose to produce the liquid fuel such as alcohol fuel, butanols through hydrolysis and saccharification is one of important research direction, and sugar is also a kind of important industrial chemicals.The hydrolysis of current lignocellulose raw material generally adopts acid hydrolysis and enzyme hydrolysis process, and acid hydrolysis needs to use a large amount of mineral acids, and the acid after using must be reclaimed, otherwise can cause serious environmental pollution.And cellulase hydrolysis process required time long (general needs several days), the production cost of biological enzyme is higher, and enzyme is mostly running stores, and secondary recovery utilizes difficulty, and hydrolysis material needs through effective pre-treatment.
Current China macromolecular material and chemical mainly rely on petroleum resources; reproducible biomass-based substitute products are less than 1%; therefore the biomass-based product of petroleum replacing base product is is urgently researched and developed; as products such as energy-saving and heat-insulating material, thermoset resin material, functional high molecule materials; reduce oil to rely on, for reply climate change and energy dilemma make positive contribution.Therefore the xylogen that can not be converted into carbohydrate in lignocellulose raw material is utilized to produce macromolecular material and chemical is also the research direction merited attention.Current xylogen generally reclaims from black liquid, and its recovery is more difficult, and easily causes environmental pollution.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of method for hydrolysis with the lignocellulose raw material of universality is provided, namely from lignocellulose raw material, high efficiency separation goes out xylogen, and can be recycled, be separated the holocellulose that obtains can under new catalyst effect effective hydrolysis and saccharification.
In order to realize the object of the invention, the method for hydrolysis of lignocellulose raw material provided by the invention, comprise the steps: 1) pre-treatment: the alkaline aqueous solution adding hydrogen peroxide in lignocellulose raw material reacts, to remove xylogen, after reaction terminates, pretreatment fluid filtering separation is obtained filter residue and filtrate, in filter residue, is rich in holocellulose; 2) hydrolysis of holocellulose: filter residue adds in autoclave after washing, adds organic solvent, catalyzer and catalyst adjuvant wherein and to be hydrolyzed reaction, and reaction terminates rear filtration, containing reducing monose in filtrate; 3) separation of xylogen: to step 1) add dehydrated alcohol in gained filtrate, then use mineral acid adjust pH 5-6, after leaving standstill, filter, be separated and obtain filter residue and filtrate; Filter residue is hemicellulose; Get its filtrate rotary evaporation and remove adjust pH 1-2 after ethanol, centrifugal after leaving standstill, be separated the solid obtained and be xylogen.
Aforesaid method, step 1) in the alkaline aqueous solution of lignocellulose raw material and hydrogen peroxide count 1-2:10 by g:mL, temperature of reaction is 70-100 DEG C, and the reaction times is 0.5-24h.
Wherein, in the alkaline aqueous solution of described hydrogen peroxide, the mass percent of hydrogen peroxide is 3-30%, and in alkaline aqueous solution, the concentration of sodium hydroxide or potassium hydroxide is 3-50%.
Aforesaid method, step 2) in filter residue and organic solvent count 1-1:20 by g:mL, hydrolysis temperature is 120 DEG C-200 DEG C, and hydrolysis time is 0.2-2h.
Wherein, described organic solvent is the aqueous solution of methyl alcohol, ethanol, propyl alcohol, ethylene glycol, glycerol or acetone, and concentration is 30-95v/v%.
Aforesaid method, step 2) described in catalyzer be PEG-OSO
3h and/or PS-PEG-OSO
3h; Described catalyst adjuvant is at least one in the metallic salts such as Manganous chloride tetrahydrate, iron(ic) chloride, iron protochloride, cupric chloride and zinc chloride.
Aforesaid method, step 2) middle filter residue, PEG-OSO
3h and/or PS-PEG-OSO
3the mass ratio of H and catalyst adjuvant is 100:10-400:1-40.
Aforesaid method, step 3) be the dehydrated alcohol adding filtrate 3-5 times volume in filtrate.
Aforesaid method, step 3) described in mineral acid be at least one in hydrochloric acid, nitric acid, sulfuric acid or phosphoric acid.
The lignocellulose raw material used in the present invention is timber, at least one in bamboo wood, rattan material, agricultural crop straw etc.Preferably, described raw material is in advance through pulverization process.More preferably, after pulverizing, particle diameter is less than 2mm.The bamboo wood selecting young age is that raw material effect is better.
The present invention also provides the xylogen adopting aforesaid method to obtain preparing the application in lignin oil and xylogen sizing agent.
In order to reach the object being applicable to different lignocellulose raw material, the aqueous solution of the organic solvent of different sorts and proportioning and different catalyst system can be selected to be applied to different lignocellulose raw materials.Preferably, what hydrotropy ability was strong is applicable to the lignocellulose raw material that density is large, hardness is high.
The present invention by alkaline hydrogen peroxide to the saponification of lignin component and strong oxidation, significantly to remove the xylogen hindering lignocellulosic material hydrolysis, the polymer supported catalyst of economic environmental protection is utilized to make most of holocellulose (Mierocrystalline cellulose and hemicellulose) be hydrolyzed to fermentable monose, thus improve the raw material availability of lignocellulose to greatest extent, and by reclaiming the hemicellulose in pretreatment fluid and xylogen, really achieve null resource waste.
The lignin product utilizing method of the present invention to obtain and holocellulose product can be used as organism-based raw material.Xylogen directly or indirectly can obtain bio oil by post liquefaction, also can be used for preparing sizing agent.Be separated the holocellulose that obtains effective hydrolysis and saccharification under the effect of novel hydrolyst and catalyst aid, avoid the length consuming time of cellulase hydrolysis, enzyme high in cost of production problem.
Lignocellulose raw material provided by the invention simple for process, environmental protection low toxicity, the delignification rate of recovery are high, be separated the holocellulose saccharification efficiency that obtains high, be easy to realize industrialization, have a extensive future.
Embodiment
Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.If do not specialize, the conventional means that technique means used in embodiment is well known to those skilled in the art, is raw materials usedly commercial goods.
The percentage sign " % " related in the present invention, if not specified, refers to mass percent; But the per-cent of solution, unless otherwise specified, refers to the grams containing solute in 100mL solution.
The delignification of embodiment 1 bamboo powder and hydrolysis and saccharification
Comprise the steps:
(1) bamboo is crushed to particle diameter and is less than 2mm, getting 100g bamboo powder, to join 500mL mass percent be in 10% hydrogen peroxide and 10% sodium hydroxide solution, room temperature mixes, 60min is stirred at 90 DEG C, naturally cooling final vacuum suction filtration is with solid-liquid separation, obtain solid filter residue (being rich in hemicellulose and xylogen), washing process is carried out to solid filter residue.
(2) the solid filter residue 5g that step (1) obtains is added in 100mL autoclave, add 50mL organic solvent (ethanolic soln of 75v/v%), catalyzer 0.5gPEG-OSO
3h, additive (catalyst adjuvant) 0.05g Manganous chloride tetrahydrate, stirring reaction 30min at 150 DEG C; After having reacted, gained hydrolyzed solution cools rapidly, filters, and filtrate measures reducing sugar by DNS method, reducing sugar yield 75%.
(3) after step (1) is rich in the dehydrated alcohol adding 3 times of volumes in the filtrate of hemicellulose and xylogen, with sulfuric acid, its pH value is adjusted to 6, has solid to separate out after leaving standstill, filter, filter residue is hemicellulose; Filtrate removes ethanol with rotatory evaporator at 50 DEG C, and then is adjusted to pH value 1 with sulfuric acid, and leave standstill and have solid to separate out, centrifugation goes out gained solid and is xylogen.Xylogen yield is 87.5%.
The delignification of embodiment 2 bamboo powder and hydrolysis and saccharification
Except step (1) is slightly different from embodiment 1, all the other operations are with the description of embodiment 1.
In step (1), 100g bamboo powder is joined 500mL mass percent be 20% hydrogen peroxide and 20% aqueous sodium hydroxide solution in.
The delignification of embodiment 3 bamboo powder and hydrolysis and saccharification
Except step (2) is slightly different from embodiment 1, all the other operations are with the description of embodiment 1.
The organic solvent added in step (2) is the acetone soln of 75v/v%.
The delignification of embodiment 4 bamboo powder and hydrolysis and saccharification
Except step (2) is slightly different from embodiment 1, all the other operations are with the description of embodiment 1.
The catalyst adjuvant added in step (2) is 0.05g iron(ic) chloride.
The delignification of embodiment 5 maize straw and hydrolysis and saccharification
Comprise the steps:
(1) pulverize after maize straw being removed root defoliation, getting 50g, to join 200mL mass percent be in 5% hydrogen peroxide and 5% sodium hydroxide solution, room temperature mixes, 60min is stirred at 85 DEG C, naturally cooling final vacuum suction filtration is with solid-liquid separation, obtain solid filter residue (being rich in hemicellulose and xylogen), washing process is carried out to solid filter residue.
(2) the solid filter residue 5g that step (1) obtains is added in 100mL autoclave, add 50mL organic solvent (ethanolic soln of 75v/v%), catalyzer 0.5gPS-PEG-OSO
3h, additive (catalyst adjuvant) 0.05g zinc chloride, stirring reaction 30min at 120 DEG C; After having reacted, gained hydrolyzed solution cools rapidly, filters, and filtrate measures reducing sugar by DNS method, reducing sugar yield 80%.
(3) above-mentioned be rich in the dehydrated alcohol adding 3 times of volumes in the filtrate of hemicellulose and xylogen after with sulfuric acid, its pH value is adjusted to 6, leave standstill after have solid to separate out, filtration, filter residue is hemicellulose; Filtrate removes ethanol with rotatory evaporator at 50 DEG C, and then is adjusted to pH value 1 with sulfuric acid, and leave standstill and have solid to separate out, centrifugation goes out gained solid and is xylogen.Xylogen yield is 82%.
Embodiment 6 is rich in the recovery energy of the filter residue of holocellulose
Hydrolyzed solution 40mL in Example 1 step (2) joins in 100mL Plastic Bottle, then adds following component (g/L): peptone 5.0; Potassium primary phosphate 2.0; Magnesium sulfate 1.0; Calcium chloride 0.25.Then solution is put into stainless steel steam sterilization pan, sterilising treatment 20min at 121 DEG C.After taking-up, solution 0.6M sodium hydroxide or 6% sulfuric acid adjust ph are 5.5 ± 0.1.The yeast fermentation broth activated is inoculated in above-mentioned solution.The inoculum size of yeast fermentation broth is 2% of glucose content.Postvaccinal solution is placed in shaking table and starts ethanol fermentation, control temperature is 37 DEG C, rotating speed is 150rpm.After fermentation 24h, sampling and measuring ethanol content, calculating ethanol yield is 88.7%.
The preparation of embodiment 7 xylogen sizing agent
In the xylogen that embodiment 1 obtains, add phenol by a certain percentage, the sodium hydroxide solution of mass percent 40%, S-WAT and calcium sulfite, and mix through mechanical stirring.Mixture, under the stirring velocity of 500rpm, is warming up to 95 DEG C, is down to room temperature, then adds a certain proportion of formaldehyde solution, be slowly warming up to 95 DEG C, insulation reaction 40min under mechanical stirring after insulation 1h.The temperature of reactant is slowly down to 70 DEG C, adds sodium hydroxide solution and urea that certain proportion concentration is 40% simultaneously, stir, be cooled to room temperature, discharging, obtain Vandyke brown liquid sizing agent, modest viscosity, have less insolubles.This sizing agent can be further used for Wood-based Panel Production.
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (10)
1. the method for hydrolysis of a lignocellulose raw material, it is characterized in that, comprise the steps: 1) alkaline aqueous solution that adds hydrogen peroxide in lignocellulose raw material reacts, after reaction terminates, filtering separation obtains filter residue and filtrate, is rich in holocellulose in filter residue; 2) filter residue adds in autoclave after washing, adds organic solvent, catalyzer and catalyst adjuvant wherein and to be hydrolyzed reaction, and reaction terminates rear filtration, containing reducing monose in filtrate; 3) to step 1) add dehydrated alcohol in gained filtrate, then use mineral acid adjust pH 5-6, after leaving standstill, filter, be separated and obtain filter residue and filtrate; Filter residue is hemicellulose; Get its filtrate rotary evaporation and remove adjust pH 1-2 after ethanol, centrifugal after leaving standstill, be separated the solid obtained and be xylogen.
2. method according to claim 1, is characterized in that, step 1) in the alkaline aqueous solution of lignocellulose raw material and hydrogen peroxide count 1-2:10 by g:mL, temperature of reaction is 70-100 DEG C, and the reaction times is 0.5-24h.
3. method according to claim 2, is characterized in that, step 1) described in hydrogen peroxide alkaline aqueous solution in the mass percent of hydrogen peroxide be 3-30%, in alkaline aqueous solution, the concentration of sodium hydroxide or potassium hydroxide is 3-50%.
4. method according to claim 1, is characterized in that, step 2) in filter residue and organic solvent count 1-1:20 by g:mL, hydrolysis temperature is 120 DEG C-200 DEG C, and hydrolysis time is 0.2-2h;
Wherein, described organic solvent is the aqueous solution of methyl alcohol, ethanol, propyl alcohol, ethylene glycol, glycerol or acetone, and concentration is 30-95v/v%.
5. method according to claim 4, is characterized in that, step 2) described in catalyzer be PEG-OSO
3h and/or PS-PEG-OSO
3h, described catalyst adjuvant is at least one in Manganous chloride tetrahydrate, iron(ic) chloride, iron protochloride, cupric chloride and zinc chloride.
6. method according to claim 5, is characterized in that, step 2) middle filter residue, PEG-OSO
3h and/or PS-PEG-OSO
3the mass ratio of H and catalyst adjuvant is 100:10-400:1-40.
7. method according to claim 1, is characterized in that, step 3) in be the dehydrated alcohol adding filtrate 3-5 times volume in filtrate.
8. method according to claim 1, is characterized in that, step 3) described in mineral acid be at least one in hydrochloric acid, nitric acid, sulfuric acid or phosphoric acid.
9. the method according to any one of claim 1-8, is characterized in that, described lignocellulose raw material is at least one in timber, bamboo wood, rattan material, agricultural crop straw; Described raw material is in advance through pulverization process, and after preferably pulverizing, particle diameter is less than 2mm.
10. adopt the xylogen that described in any one of claim 1-9, method obtains preparing the application in lignin oil and xylogen sizing agent.
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| CN106824992A (en) * | 2017-02-13 | 2017-06-13 | 广东工业大学 | A kind of method of water plant of degrading |
| CN108162120A (en) * | 2017-12-07 | 2018-06-15 | 常州市日臣艺术装饰材料有限公司 | A kind of preparation method of formaldehydeless high strength moistureproof particieboard |
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| CN114378912A (en) * | 2022-01-29 | 2022-04-22 | 兰州农之品生态科技有限公司 | Preparation method of bamboo cellulose |
| CN115717007A (en) * | 2022-05-13 | 2023-02-28 | 北京林业大学 | Method for separating and extracting pseudolignin from biomass |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106824992A (en) * | 2017-02-13 | 2017-06-13 | 广东工业大学 | A kind of method of water plant of degrading |
| CN108162120A (en) * | 2017-12-07 | 2018-06-15 | 常州市日臣艺术装饰材料有限公司 | A kind of preparation method of formaldehydeless high strength moistureproof particieboard |
| CN109135665A (en) * | 2018-09-08 | 2019-01-04 | 佛山朝鸿新材料科技有限公司 | A kind of preparation method of weather-proof high stable type packaging binder |
| CN112778539A (en) * | 2021-01-04 | 2021-05-11 | 中国林业科学研究院林产化学工业研究所 | Method for preparing oxidized lignin with high carboxyl content from fiber raw material |
| CN114378912A (en) * | 2022-01-29 | 2022-04-22 | 兰州农之品生态科技有限公司 | Preparation method of bamboo cellulose |
| CN115717007A (en) * | 2022-05-13 | 2023-02-28 | 北京林业大学 | Method for separating and extracting pseudolignin from biomass |
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