CN107936143B - Method for removing lignin from plant fiber raw material hydrolysate through biological treatment - Google Patents
Method for removing lignin from plant fiber raw material hydrolysate through biological treatment Download PDFInfo
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- CN107936143B CN107936143B CN201711193844.2A CN201711193844A CN107936143B CN 107936143 B CN107936143 B CN 107936143B CN 201711193844 A CN201711193844 A CN 201711193844A CN 107936143 B CN107936143 B CN 107936143B
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- JLCPHMBAVCMARE-UHFFFAOYSA-N [3-[[3-[[3-[[3-[[3-[[3-[[3-[[3-[[3-[[3-[[3-[[5-(2-amino-6-oxo-1H-purin-9-yl)-3-[[3-[[3-[[3-[[3-[[3-[[5-(2-amino-6-oxo-1H-purin-9-yl)-3-[[5-(2-amino-6-oxo-1H-purin-9-yl)-3-hydroxyoxolan-2-yl]methoxy-hydroxyphosphoryl]oxyoxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(5-methyl-2,4-dioxopyrimidin-1-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(6-aminopurin-9-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(6-aminopurin-9-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(6-aminopurin-9-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(6-aminopurin-9-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxyoxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(5-methyl-2,4-dioxopyrimidin-1-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(4-amino-2-oxopyrimidin-1-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(5-methyl-2,4-dioxopyrimidin-1-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(5-methyl-2,4-dioxopyrimidin-1-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(6-aminopurin-9-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(6-aminopurin-9-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(4-amino-2-oxopyrimidin-1-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(4-amino-2-oxopyrimidin-1-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(4-amino-2-oxopyrimidin-1-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(6-aminopurin-9-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(4-amino-2-oxopyrimidin-1-yl)oxolan-2-yl]methyl [5-(6-aminopurin-9-yl)-2-(hydroxymethyl)oxolan-3-yl] hydrogen phosphate Polymers Cc1cn(C2CC(OP(O)(=O)OCC3OC(CC3OP(O)(=O)OCC3OC(CC3O)n3cnc4c3nc(N)[nH]c4=O)n3cnc4c3nc(N)[nH]c4=O)C(COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3CO)n3cnc4c(N)ncnc34)n3ccc(N)nc3=O)n3cnc4c(N)ncnc34)n3ccc(N)nc3=O)n3ccc(N)nc3=O)n3ccc(N)nc3=O)n3cnc4c(N)ncnc34)n3cnc4c(N)ncnc34)n3cc(C)c(=O)[nH]c3=O)n3cc(C)c(=O)[nH]c3=O)n3ccc(N)nc3=O)n3cc(C)c(=O)[nH]c3=O)n3cnc4c3nc(N)[nH]c4=O)n3cnc4c(N)ncnc34)n3cnc4c(N)ncnc34)n3cnc4c(N)ncnc34)n3cnc4c(N)ncnc34)O2)c(=O)[nH]c1=O JLCPHMBAVCMARE-UHFFFAOYSA-N 0.000 description 1
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- -1 phenoxy free radical Chemical class 0.000 description 1
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- WQGWDDDVZFFDIG-UHFFFAOYSA-N pyrogallol Chemical compound OC1=CC=CC(O)=C1O WQGWDDDVZFFDIG-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- Sustainable Development (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention relates to a method for removing lignin by biological treatment of plant fiber raw material hydrolysate, which comprises the steps of treating the plant fiber raw material hydrolysate by horseradish peroxidase firstly and then flocculating by cationic polymer, wherein the horseradish peroxidase treatment can cause dissolved lignin with low molecular weight in the hydrolysate to be polymerized into high molecular weight lignin, and precipitating to remove a part of lignin; after the lignin is treated by horseradish peroxidase, even if the part which is not precipitated is polymerized, the molecular weight is increased, and the lignin is easier to remove in the subsequent cationic flocculation treatment process, and then the residual lignin is further removed by adopting cationic polymer treatment.
Description
Technical Field
The invention relates to a method for separating components of hydrolysate, in particular to a method for removing lignin by biological treatment of hydrolysate of plant fiber raw material, belonging to the field of comprehensive utilization of biomass.
Background
Hemicellulose is one of the most abundant natural polymers in nature, with lignocellulosic feedstocks including wood and nonwood, such as bagasse, reed, and various grasses, containing large amounts of hemicellulosic glycans. The hemicellulose has a plurality of applications, can be used for producing chemicals such as furfural, hydroxymethyl furfural and the like, and the high molecular weight hemicellulose can be used for preparing biological materials such as food packaging films, hydrogel, surfactants, antibacterial materials and the like. In addition, the hemicellulose sugar can also be fermented to produce ethanol, methanol and other biofuels. Therefore, how to effectively utilize these hemicellulosic polysaccharides is of great significance for biomass refining. To efficiently utilize the hemicellulose in lignocellulosic feedstocks, the hemicellulose is first separated from the feedstock. At present, the hydrolysis method is a common method for separating hemicellulose from plant fiber raw materials, and comprises acid hydrolysis, self-hydrolysis and alkaline hydrolysis, wherein hemicellulose glycan enters into hydrolysis liquid after hydrolysis, in the hydrolysis process, besides hemicellulose, lignin can be partially degraded and enter into the hydrolysis liquid, and in addition, the hydrolysis liquid can also contain degradation products of the hemicellulose and cellulose, lipophilic extracts and the like. In the process of producing biofuel by hydrolysate fermentation, lignin can inhibit the hydrolysis and fermentation processes of enzyme, and is also a main source of color in hydrolysate of the wood fiber raw material. In order to obtain pure hemicellulose, the hemicellulose in the hydrolysate is purified. In the process of removing impurities from the hydrolysate to obtain sugar solution with high concentration and purity, the removal of main impurity lignin is difficult. The method for removing various impurities from the hydrolysate comprises various methods such as activated carbon adsorption, quicklime adsorption, macroporous resin adsorption, cationic or nonionic polymer flocculation, membrane filtration and the like, and the membrane can be blocked in the process of removing the small molecular impurities by adopting membrane concentration, so that the membrane flux is reduced and the membrane service life is prolonged.
There are many prior arts disclosing the removal of impurities from a lignocellulosic feedstock hydrolysate to extract oligosaccharides, for example, chinese patent document 200410023875.X discloses a method of extracting xylo-oligosaccharides from corncob meal. The invention comprises the following sequential steps: (1) mixing the corncob powder with water, adding a weak acid catalyst for cracking, and dissolving out xylan in the corncobs; (2) adjusting the pH value of the xylan aqueous solution to 5.0-6.0, adding xylanase for enzymolysis, and inactivating the xylanase at high temperature; (3) filtering corncob powder residues, and removing impurities and decolorizing xylan liquid glucose by using activated carbon and ion exchange resin; (4) intercepting macromolecular xylan by a macromolecular interception membrane, and filtering low-xylan sugar liquor; concentrating and desalting with sodium filter membrane; (5) and (3) concentrating the xylo-oligosaccharide sugar solution in vacuum to obtain light yellow viscous syrup, and performing excipient or direct spray drying on the xylo-oligosaccharide syrup to obtain xylo-oligosaccharide powder. However, the method adopts the activated carbon and the ion exchange resin to remove impurities and decolor, has poor impurity removal effect, can not effectively remove lignin, still has impurity residues, and simultaneously adopts the activated carbon and the ion exchange resin to remove impurities, and is easy to remove together with xylan, so that sugar loss is caused.
Chinese patent 201310554290.X discloses a method for extracting oligosaccharides from plant material prehydrolysis liquid, comprising the following steps: (1) adding polyelectrolyte into the plant raw material prehydrolysis liquid, wherein the polyelectrolyte is one or a combination of polyaluminium chloride, polyaluminium sulfate, polyaluminium ferric chloride, polyaluminium ferric sulfate, polyaluminium ferric silicate, polyferric chloride and polyferric sulfate, the addition amount of the polyelectrolyte is 0.01-10g/L, stirring for 5-20 minutes, standing for 80-150 minutes, and separating to obtain supernatant; (2) filtering the supernatant by membrane separation to obtain oligosaccharide concentrate; (3) evaporating to crystallize oligosaccharide concentrated solution, and drying to obtain oligosaccharide. In the method, polyelectrolyte is added to remove lignin in the hydrolysate, so that the impurity removal effect is poor and the efficiency is low.
At present, treatment with cationic flocculants is considered to be a common method for removing lignin, particularly high molecular colloidal lignin, from hydrolysate. The cationic flocculant used was: polydiallyldimethylammonium chloride (pDADMAC), Cationic Polyacrylamide (CPAM), Polyethyleneimine (PEI), and polyaluminum chloride (PAC). The lignin removal from the poplar hydrolysate of polyaluminium chloride (PAC) and polydiallyldimethylammonium chloride (PDADMAC) by Naringin and Wangmujiang et al shows that the addition of PAC and PDADMAC can remove part of the lignin in the hydrolysate, but also causes part of the loss of sugar. See Cheng Dan et al, Bioresource engineering, 2014,152:31-37(Chen Xiaoqian, Wang Zhaojian, Fu Yingjuan, Li Zongquan, Qin Menghua, specific lignin prediction for oligonucleotides recovery from hot water wood extract, Bioresource Technology, 2014,152: 31-37).
Therefore, the cationic flocculant treatment for removing lignin in the hydrolysate has the following problems: the cationic polymer flocculant is used in a large amount, the removal efficiency of dissolved lignin with lower molecular weight is low, and in addition, the loss amount of sugar is large when the lignin is removed by the treatment of the single cationic flocculant.
The problem that impurity exists is got rid of to current wood fibre raw materials hydrolysate: the impurity removal effect is poor, lignin can not be effectively removed, impurities still remain, the loss amount of sugar is large, the dosage of the cationic polymer flocculant is large, and a treatment method with high lignin removal rate and low sugar loss rate is necessary to be developed.
Disclosure of Invention
The invention provides a method for removing lignin from plant fiber raw material hydrolysate by biological treatment, aiming at the problems that when cation polymer is adopted to remove lignin from hydrolysate in the prior separation and purification process of sugar in plant fiber raw material hydrolysate, the removal efficiency of low molecular weight dissolved lignin is low, the removal selectivity of lignin is poor, and the loss rate of sugar is high.
Summary of the invention:
the method of the invention firstly treats the plant fiber raw material hydrolysate with horseradish peroxidase and then flocculates the cationic polymer. Horseradish peroxidase treatment can cause dissolved lignin with low molecular weight in hydrolysate to be polymerized into high molecular weight lignin, and a part of lignin is precipitated and removed; after the lignin is treated by horseradish peroxidase, even if the part which is not precipitated is polymerized, the molecular weight is increased, the lignin can be removed more easily in the subsequent cationic flocculation treatment process, and then the residual lignin is further removed by adopting cationic polymer treatment, so that the removal rate of the lignin can be improved under the condition of lower cationic polymer dosage, and the loss of sugar in the cationic polymer treatment process can be obviously reduced.
Description of terms:
self-hydrolysis: the plant fiber raw material is added with water or water vapor only, and is not added with any other chemical for hydrolysis reaction.
Horse radish peroxidase activity: at 20 ℃, at the pH of 6.0, the enzyme amount for catalyzing pyrogallic acid to generate 1.0mg of red gallol in 20 seconds is one enzyme activity unit: and U is adopted.
Sugar loss rate: the percentage of the amount of sugar reduction in the hydrolysate treatment process to the amount of raw sugar in the hydrolysate is expressed as a percentage.
The lignin removal rate is as follows: the percentage of lignin in the hydrolysate decreased before and after treatment.
Detailed description of the invention:
the invention is realized by the following technical scheme:
a method for removing lignin by biological treatment of plant fiber raw material hydrolysate comprises the following steps:
treating the plant fiber raw material hydrolysate with horseradish peroxidase;
and (3) treating hydrolysate flocculant after enzyme treatment.
According to the invention, the preferable steps of the horseradish peroxidase enzyme treatment on the plant fiber raw material hydrolysate are as follows: adding horseradish peroxidase and hydrogen peroxide into the plant fiber raw material hydrolysate for enzyme treatment, wherein the dosage of the horseradish peroxidase is 3000-30000U/L hydrolysate, and the dosage of the hydrogen peroxide is 2.0-20g/L hydrolysate, and removing precipitates to obtain the hydrolysate after the enzyme treatment.
According to the invention, the dosage of horseradish peroxidase is 5000-.
According to the invention, the enzyme treatment temperature is 10-60 ℃, the treatment time is 1-24 h, and the pH is 3.0-8.0; further preferably, the enzyme treatment temperature is 15-45 ℃, the treatment time is 4-12 h, and the pH is 3.5-6.5.
According to a preferred embodiment of the present invention, the removal of the precipitate is: standing the mixture after the enzyme treatment for 2-24 hours, removing the sediment at the bottom, and taking the supernatant as hydrolysate after the enzyme treatment; or centrifuging the mixture after enzyme treatment, and removing the precipitate to obtain the treated hydrolysate.
Preferably, the plant fiber raw material hydrolysate is a hydrolysate obtained by acid hydrolysis or self-hydrolysis treatment of the plant fiber raw material with water.
According to the invention, the plant fiber raw material is selected from one of needle-leaved wood, broad-leaved wood, bamboo, wheat straw, bagasse and reed non-wood raw material.
More preferably, the softwood is selected from one of masson pine, larch, red pine or spruce, and the hardwood is selected from one or more of poplar, birch, maple or eucalyptus.
Further preferably, the self-hydrolysis treatment temperature is 140-200 ℃, the hydrolysis time is 15-240min, and the mass ratio of the water to the plant fiber raw material is as follows: 3:1-20: 1;
further preferably, the acid hydrolysis temperature is 120-180 ℃, the hydrolysis time is 10-180min, and the mass ratio of the water to the plant fiber raw material is as follows: 3:1-20:1, wherein the acid used for acid hydrolysis is hydrochloric acid or sulfuric acid, and the dosage of the acid is 2-30 kg per ton of air-dried raw material.
The particular operative process of autohydrolysis or acid hydrolysis of the invention can be carried out using known techniques.
The horseradish peroxidase can oxidize phenolic hydroxyl of lignin to generate phenoxy free radicals in the presence of hydrogen peroxide, then transfer free radical electrons or directly perform cross-linking to generate polymerization, so that the molecular weight of lignin is increased to catalyze lignin polymerization, and further, hydrogen peroxide reacts with Fe (III) in the horseradish peroxidase to generate a high-oxidation-state intermediate HRP I; then adding lignin (reducing substrate) containing phenolic hydroxyl to enable HRP I to generate another intermediate HRP II, and simultaneously enabling the lignin containing phenolic hydroxyl to generate phenoxy radical; thirdly, lignin containing phenolic hydroxyl continues to reduce HRP II into original horse radish peroxidase, and simultaneously generates phenoxy free radical. The free radicals generated in the first two steps of reaction are used for transferring free radical electrons or directly used for crosslinking to generate polymerization, so that the molecular weight of the lignin is increased.
According to the invention, a part of low molecular weight dissolved lignin is polymerized into insoluble high molecular weight lignin by horseradish peroxidase, and a part of lignin is removed by removing precipitates, even if the part of lignin which is not precipitated is polymerized under the action of horseradish peroxidase, the molecular weight is increased, the lignin with high molecular weight further removes residual lignin by subsequent cationic flocculation, and the increase of the molecular weight is beneficial to the improvement of the cationic flocculation efficiency, so that the total removal rate of the lignin is greatly improved by combining horseradish peroxidase treatment with cationic polymer treatment.
According to the invention, the hydrolysate flocculant after enzyme treatment comprises the following steps: adding a cationic polymer flocculant into the hydrolysate after the enzyme treatment for flocculation treatment, and standing or centrifuging the treated hydrolysate to remove precipitates to obtain the purified hydrolysate.
Preferably, according to the invention, the cationic flocculant is a low molecular weight, high charge density cationic polymer.
More preferably, the cationic flocculant is one or a mixture of more than two selected from polydiallyl dimethyl ammonium chloride, polyethyleneimine or polyamine.
More preferably, the polydiallyldimethylammonium chloride, polyethyleneimine, polyamine have a molecular weight of 8 to 30 ten thousand, and a charge density of 5.0meq/g or more at pH 7.
According to the invention, the dosage of the cationic flocculant is 200-800 mg/L of hydrolysate after enzyme treatment, the treatment time is 10-30 min, and the pH value is 3.0-8.0.
The invention preferably adopts a technical scheme that the method for removing lignin by biological treatment of the hydrolysate of the plant fiber raw material comprises the following steps:
(1) adding horseradish peroxidase into the plant fiber hydrolysate for enzyme treatment, wherein the dosage of the horseradish peroxidase is 5000-;
(2) adding one or a mixture of two of cationic flocculants poly diallyl dimethyl ammonium chloride, polyethyleneimine and polyamine into the hydrolysate after enzyme treatment for treatment, wherein the molecular weight of the cationic flocculant is 8-30 ten thousand; the dosage of the cationic flocculant is 200-800 mg/L of hydrolysate after enzyme treatment, the treatment time is 10-30 min, the pH value is 3.5-8.0, and the hydrolysate is obtained after purification by standing or centrifugation.
The invention has the following technical characteristics and excellent effects:
according to the invention, horseradish peroxidase is adopted for treatment before flocculation treatment of the cationic polymer of the hydrolysate of the plant fiber raw material, and the horseradish peroxidase treatment can cause polymerization of lignin in the hydrolysate and increase molecular weight, so that part of dissolved lignin is converted into insoluble lignin after polymerization so as to precipitate and separate out; although no precipitation exists in part of lignin, the molecular weight is increased, and the lignin is easier to flocculate and remove when being further treated by cationic polymers after enzyme treatment, so that the residual lignin can be flocculated and removed at a lower dosage of the cationic polymers after horse radish peroxidase treatment. Under the action of the cationic polymer with lower molecular weight and high charge density, the loss of sugar in the hydrolysate in the flocculation process of the cationic polymer is reduced while lignin is removed, and the yield and the purity of the sugar in the hydrolysate are improved.
Detailed Description
The present invention will be further described with reference to the following examples, but is not limited thereto. The amount of cationic polymer used in the control tests in the examples is the preferred amount.
Example 1
A biological enzyme treatment method for plant fiber raw material hydrolysate comprises the following steps:
(1) the sugar content of hydrolyzed poplar is 10.2g/L, the lignin content is 4.7g/L, the hydrolyzed liquid is treated by horseradish peroxidase, and the treatment conditions are as follows: the enzyme dosage is 10000U/L hydrolysate, the hydrogen peroxide dosage is 8g/L hydrolysate, the temperature is 30 ℃, the time is 6h, and the pH is 4.0.
(2) Standing the hydrolysate treated by the horseradish peroxidase for 8 hours, decanting to remove precipitates, and treating the obtained upper-layer hydrolysate with cationic polymer, wherein the cationic polymer is cationic polymer polyallyl dimethyl ammonium chloride with the molecular weight of 25 ten thousand and the positive charge density of 7.0meq/L, the dosage of the cationic polymer is 200mg/L, and the treatment temperature is room temperature, the pH value is 4.0, and the time is 10 minutes. Standing for 8 hours after the cationic polymer is treated, and decanting to remove precipitate to obtain upper layer purified hydrolysate.
In the example, after the treatment of horseradish peroxidase and the treatment of cationic polymer, the lignin removal rate is 71%, and the sugar loss rate is 8.6%.
Comparative example 1: the method is the same as the method of the example 1, except that the method directly carries out the step (2) treatment on the hydrolysate after the self-hydrolysis without the step (1) horse radish peroxidase treatment, and the consumption of the poly diallyl dimethyl ammonium chloride is 280mg/L of the hydrolysate, so as to obtain the purified hydrolysate. After the treatment of comparative example 1, the lignin removal rate was 45%, while the sugar loss rate in the hydrolysate was 14.2%.
Comparative example: the method directly treats horse radish peroxidase without flocculation treatment. The lignin removal rate was 55% and the sugar loss rate in the hydrolysate was 4.5%.
Example 2
A biological treatment method of plant fiber raw material hydrolysate comprises the following steps:
(1) the hydrolysate after hydrolysis of the maple acid has the sugar content of 18.2g/L and the lignin content of 8.6g/L, and is firstly treated by horseradish peroxidase under the following treatment conditions: the dosage of the enzyme is 15000U/L hydrolysate, the dosage of the hydrogen peroxide is 10g/L hydrolysate, the temperature is 25 ℃, the time is 10h, and the pH value is 4.0.
(2) After horse radish peroxidase treatment, polyethyleneimine with the molecular weight of 15 ten thousand and the positive charge density of 6.5meq/g is adopted for treatment, the amount of hydrolysate is 150mg/L, the treatment temperature is room temperature, the pH value is 4.0, and the treatment time is 15 minutes. And (4) centrifuging for 15 minutes after the cationic polymer is treated, and removing precipitates to obtain hydrolysate after the upper layer is purified. After being treated by horseradish peroxidase-cationic polymer, the lignin removal rate is 58 percent, and the sugar loss rate is 7.6 percent.
Comparative example 2: the method is the same as the method of the embodiment 2, except that the method directly carries out the step (2) treatment on the hydrolysate after acid hydrolysis without the step (1) horse radish peroxidase treatment, and the consumption of the polyethyleneimine is 220mg/L hydrolysate, so as to obtain the purified hydrolysate. After the treatment of comparative example 2, the lignin removal was 38% and the sugar loss was 13.8%.
Example 3
A biological treatment method of plant fiber raw material hydrolysate comprises the following steps:
(1) the wheat straw hydrolysate after self-hydrolysis has sugar content of 8.7g/L and lignin content of 3.7g/L, and is first treated with horseradish peroxidase under the conditions: the dosage of the enzyme is 15000U/L hydrolysate, the dosage of the hydrogen peroxide is 10g/L hydrolysate, the temperature is 30 ℃, the time is 12h, and the pH is 5.0.
(2) After being treated by horse radish peroxidase, polyamine with the molecular weight of 12 ten thousand and the positive charge density of 6.6meq/g is adopted for treatment, the dosage is 160mg/L hydrolysate, the treatment temperature is room temperature, the pH value is 5.0, and the treatment time is 20 minutes. Standing for 6 hours after the cationic polymer is treated, and decanting to remove precipitate to obtain upper layer purified hydrolysate. After being treated by horseradish peroxidase-cationic polymer, the lignin removal rate is 67%, and the sugar loss rate is 7.1%.
Comparative example 3: the method is the same as the method of example 3, except that the method does not use the horseradish peroxidase treatment in the step (1), and directly uses the hydrolyzed hydrolysate for the treatment in the step (2), and the dosage of the cationic polymer polyamine is 220mg/L hydrolysate, so as to obtain the purified hydrolysate. After the treatment of comparative example 3, the lignin removal was 38% and the sugar loss was 16.0%.
Example 4:
the biological treatment method of the plant fiber raw material hydrolysate as described in example 1 is different from the following steps:
step (1), the treatment temperature of the horseradish peroxidase is 20 ℃.
Example 5:
the biological treatment method of the plant fiber raw material hydrolysate as described in example 1 is different from the following steps:
and (1) adding hydrogen peroxide into the hydrolysate in an amount of 6g/L during enzyme treatment.
Example 6:
the biological treatment method of the plant fiber raw material hydrolysate as described in example 1 is different from the following steps:
and (1) replacing the hydrolyzed liquid of the poplar by the hydrolyzed liquid of the reed.
Example 7:
the biological treatment method of the plant fiber raw material hydrolysate as described in example 1 is different from the following steps:
and (1) replacing the hydrolyzed liquid of the poplar after the eucalyptus is hydrolyzed by the hydrolyzed liquid of the eucalyptus.
Example 8:
the biological treatment method of the plant fiber raw material hydrolysate as described in example 1 is different from the following steps:
the cationic polymer in the step (2) is a mixture of polydiallyldimethylammonium chloride with a molecular weight of 12 ten thousand and a positive charge density of 7.2meq/g and polyethyleneimine with a molecular weight of 18 ten thousand and a positive charge density of 6.8 meq/g.
Example 9:
the biological treatment method of the plant fiber raw material hydrolysate as described in example 1 is different from the following steps:
and (1) replacing the hydrolyzed liquid obtained after the poplar self-hydrolyzes with the hydrolyzed liquid obtained after the bamboo self-hydrolyzes.
Claims (2)
1. A method for removing lignin by biological treatment of plant fiber raw material hydrolysate comprises the following steps:
(1) the horseradish peroxidase treatment step of the plant fiber raw material hydrolysate with enzyme: adding horseradish peroxidase and hydrogen peroxide into the plant fiber raw material hydrolysate for enzyme treatment; standing the mixture after the enzyme treatment for 2-24 hours, removing the sediment at the bottom, wherein the supernatant is the hydrolysate after the enzyme treatment, or centrifuging the mixture after the enzyme treatment to remove the sediment to obtain the hydrolysate after the enzyme treatment;
the plant fiber raw material hydrolysate is obtained by performing acid hydrolysis or self-hydrolysis treatment on a plant fiber raw material by using water; the plant fiber raw material is selected from one of coniferous wood, broad-leaved wood, bamboo, wheat straw, bagasse and reed; the softwood is selected from one of Chinese red pine, larch, red pine or spruce, and the hardwood is selected from one or more of poplar, birch, maple or eucalyptus; the self-hydrolysis conditions are as follows: the self-hydrolysis treatment temperature is 140-; the acid hydrolysis conditions are as follows: the acid hydrolysis temperature is 120-180 ℃, the hydrolysis time is 10-180min, the mass ratio of water to the plant fiber raw material is 3:1-20:1, the acid used for acid hydrolysis is hydrochloric acid or sulfuric acid, and the acid dosage is 2-30 kg per ton of air-dried raw material;
the enzyme treatment conditions are as follows: the dosage of horseradish peroxidase is 5000-;
(2) and (3) treating the hydrolysate flocculant after enzyme treatment: adding a cationic polymer flocculant into the hydrolysate after the enzyme treatment for flocculation treatment, and standing or centrifuging the treated hydrolysate to remove precipitates to obtain purified hydrolysate; the cationic polymer flocculant is one or a mixture of more than two of poly-diallyl dimethyl ammonium chloride, polyethyleneimine or polyamine; the molecular weight of the polydiallyldimethylammonium chloride, the polyethyleneimine and the polyamine is 8-30 ten thousand, the charge density is more than or equal to 5.0meq/g at the pH value of 7, the dosage of the cationic polymer flocculant is 200-800 mg/L of hydrolysate after enzyme treatment, the treatment time is 10-30 min, and the pH value is 3.0-8.0.
2. The method of claim 1 for the biological treatment of a plant fiber feedstock hydrolysate for lignin removal, wherein: the enzyme treatment conditions in the step (1) are as follows: the amount of the hydrogen peroxide is 4.0-12g/L, the enzyme treatment temperature is 15-45 ℃, the time is 4-12 h, and the pH is 3.5-7.0;
the pH value in the step (2) is 3.5-8.0.
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