CN114717278A - Agricultural and forestry biomass pretreatment method - Google Patents
Agricultural and forestry biomass pretreatment method Download PDFInfo
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- CN114717278A CN114717278A CN202110011406.XA CN202110011406A CN114717278A CN 114717278 A CN114717278 A CN 114717278A CN 202110011406 A CN202110011406 A CN 202110011406A CN 114717278 A CN114717278 A CN 114717278A
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- C—CHEMISTRY; METALLURGY
- 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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- 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
- C12P19/02—Monosaccharides
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- C12P2201/00—Pretreatment of cellulosic or lignocellulosic material for subsequent enzymatic treatment or hydrolysis
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- C12P2203/00—Fermentation products obtained from optionally pretreated or hydrolyzed cellulosic or lignocellulosic material as the carbon source
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses an agriculture and forestry biomass pretreatment method, and belongs to the fields of environmental protection and biomass development and utilization. The method comprises the steps of uniformly mixing and infiltrating crushed lignocellulose and high-boiling alcohol according to a certain proportion, and then feeding the infiltrated mixture to a screw extruder and extruding, so as to achieve the aim of pretreatment. The invention organically combines the double-screw extrusion and the high-boiling alcohol pretreatment together, has complementary advantages and can achieve the following characteristics: (1) the operation is simple, the pretreatment time is short, and the continuity is strong; (2) the glycerol consumption is less, and the glucose yield is high; (3) low energy consumption, high economic feasibility and easy realization of industrial utilization.
Description
Technical Field
The invention belongs to the fields of environmental protection and biomass development and utilization, relates to an agriculture and forestry biomass pretreatment method, and particularly relates to a method for strengthening the saccharifiability and the fermentability of agriculture and forestry biomass raw materials through high-boiling-point alcohol assisted double-screw extrusion pretreatment.
Background
Lignocellulose is mainly composed of three major parts, namely cellulose, hemicellulose and lignin, and is one of the most abundant renewable biomass resources on the earth. The raw material formed by the method contains a large amount of carbohydrate, and the carbohydrate has great potential for producing biomass sugar syrup, so that a platform is established for producing fuels and chemicals through biochemical or chemical routes. Saccharification and enzymolysis are key steps for producing monosaccharide and establishing a platform. However, plants rich in lignocellulosic biomass are composed primarily of cell walls, which are highly resistant to enzymatic degradation in their natural state. In addition, lignin in biomass has a strong irreversible inhibition of hydrolytic enzymes. For the above reasons, pretreatment of lignocellulosic feedstocks before saccharification and enzymolysis is an inevitable approach for industrial development.
At present, methods for improving the enzymatic saccharification rate of biomass mainly comprise a physical method, a chemical method, a physicochemical method and a biological method. In recent years, research on extrusion pretreatment of lignocellulosic biomass shows that the method has significant improvement on the enzymatic saccharification effect of the biomass. Compared with a batch pretreatment system, extrusion is a continuous pretreatment process, has higher treatment capacity, and is safe and environment-friendly. However, there are some disadvantages in the extrusion process of the lignocellulose material, such as poor material flow characteristics due to excessive frictional resistance, strong pressure resistance of equipment in high-temperature water phase, and easy corrosion of equipment due to the addition of acid-base catalyst.
Glycerol is a high boiling alcohol with affinity for cellulose. When the cellulose is subjected to normal-pressure glycerol cooking pretreatment, the saccharifiable property and the fermentability of the lignocellulose can be well enhanced due to the characteristics of strong lubricating property, fast heat conduction, good component selectivity and the like of the glycerol, and the pretreated raw material has low content of fermentation inhibitors and strong enzymolysis property. However, the addition of more glycerol and the high energy consumption of heating and cooking are disadvantages.
Disclosure of Invention
[ problem ] to
The invention aims to solve the technical problems that the friction resistance is large when the lignocellulose biomass is subjected to extrusion pretreatment, and the consumption of glycerol is large and the glycerol is difficult to recover when the normal pressure glycerol is adopted for cooking.
[ solution ]
The invention provides an agriculture and forestry biomass pretreatment method, which comprises the following steps:
(1) preparation of lignocellulosic feedstock: crushing lignocellulose raw materials, wherein the lignocellulose raw materials comprise one or a mixture of several of bagasse, corn straw, wheat straw, rice straw and the like, and packing and storing the crushed lignocellulose raw materials by using a vacuum bag;
(2) mixing and infiltrating high-boiling alcohol and materials: uniformly mixing the crushed lignocellulose with high-boiling alcohol according to a certain proportion, and soaking for 0.25-24h, wherein the high-boiling alcohol comprises: glycerin, ethylene glycol, and the like;
(3) feeding the soaked mixture to a screw extruder and extruding the mixture so as to achieve the aim of pretreatment; the screw extruder is a twin screw extruder (extruder).
Further, the particle size of the pulverized lignocellulose in the step (1) is 0.25-10mm, and the particle size is more preferably 0.5-5 mm.
Further, the water content of the lignocellulose raw material in the step (1) is 3-15%.
Furthermore, in the step (2), no catalyst is added or no catalyst is added when the high-boiling alcohol is mixed and soaked with the material. The catalyst can be acid, alkali, metal salt catalyst, such as: hydrochloric acid, sodium hydroxide, zinc chloride, lithium bromide, and the like.
Further, when the lignocellulose crushed in the step (2) is mixed with high-boiling alcohol, the mass ratio of the lignocellulose crushed to the high-boiling alcohol is 1:1-1: 5.
Further, the pre-treatment extrusion rotating speed in the step (3) is 30-90 rpm.
Further, the pretreatment extrusion temperature in the step (3) is 160-.
Further, the number of times of extrusion in the pretreatment in the step (3) is 1-5.
[ advantageous effects ]
The invention adopts double screws, and controls the extrusion rotating speed within a certain range to obtain better pretreatment effect. Meanwhile, the function of the glycerol can be fully exerted by combining the high extrusion temperature of 160-250 ℃. In addition, in the pretreatment process, the pretreatment effect is improved by adding catalysts (alkali, acid and metal salt).
The method comprises the steps of carrying out component analysis, scanning electron microscope analysis, crystallinity analysis and Fourier infrared spectrum analysis on the lignocellulose raw material before and after pretreatment, determining the retention rate and lignin removal rate of the pretreated cellulose and hemicellulose, and determining the glucose yield and enzymolysis rate after saccharification and fermentation, wherein the results show that the double-screw extrusion pretreatment of the high-boiling-point alcohol auxiliary agriculture and forestry biomass raw material has an effect of strengthening the saccharinability and the fermentability of the lignocellulose.
Compared with the traditional cooking process (normal-pressure glycerol cooking pretreatment), the method has the advantages that the consumption of the glycerol is obviously reduced when a higher saccharification enzymolysis effect is obtained, and the method has higher cellulose and hemicellulose retention rate and lignin removal rate while using a small amount of glycerol additive.
The invention organically combines the double-screw extrusion and the high-boiling alcohol pretreatment together, has complementary advantages and can achieve the following characteristics: (1) the operation is simple, the pretreatment time is short, and the continuity is strong; (2) the glycerol consumption is less, and the glucose yield is high; (3) low energy consumption, high economic feasibility and easy realization of industrial utilization.
Detailed Description
The method for measuring the water content comprises the following steps:
the moisture content of the lignocellulose raw material was measured by a moisture meter (MB25 aohaus instruments ltd., china).
Comparative example
(1) 10g of the ready bagasse lignocellulose raw material was weighed into a 500mL three-necked flask (0.2% (w/w) NaOH was added as catalyst) and glycerol was added in a mass ratio of 1:10 (this ratio is the optimum cooking process).
(2) After the mixture is uniform, the flask is fixed above the heater, and a stirring paddle is installed. Cooking at 240 deg.C and 180rpm for 20 min.
(3) After the pretreatment is finished, after the temperature of the pretreated raw material is naturally reduced to be below 100 ℃, the pretreated raw material is filtered and washed by using about 650mL of hot water (100 ℃).
(4) Drying the washed substrate in an oven at 60 ℃, carrying out an enzymolysis experiment under the conditions of low enzyme amount (< 15FPU/g dry substrate) and high substrate concentration (> 15%), and finally determining the content of the glucose in the hydrolysate to be 100-150g/L by using a high performance liquid chromatography.
Example 1 bagasse pretreatment method (I)
(1) Preparing bagasse raw materials: crushing bagasse to 0.5-5mm, vacuum packing, and storing in a sample chamber (at room temperature and under ventilation).
(2) Mixing the vacuum-preserved bagasse powder and glycerol according to the mass ratio of 1:1-1:3, and sealing and infiltrating at room temperature for 0.5-12h after uniform mixing.
(3) Pretreating the soaked raw materials on a double-screw extruder, wherein the extrusion speed is 50-90rpm, the extrusion temperature is 220-240 ℃, and the extrusion times are 1-3.
(4) After the pretreatment is finished, after the temperature of the pretreated raw material is naturally reduced to be below 100 ℃, the pretreated raw material is filtered and washed by 100mL of hot water (100 ℃) per 1g of dry basis.
(5) Drying the washed substrate in an oven at 60 ℃, performing an enzymolysis experiment under the conditions of low enzyme amount (less than 15FPU/g dry substrate) and high substrate concentration (more than 15%), and finally determining the content of glucose in the hydrolysate to be 80-130g/L by using a high performance liquid chromatography.
Example 2 corn stover pretreatment method
(1) Preparing a corn straw raw material: pulverizing corn stalk into 5-10mm, vacuum packaging, and storing in a sample chamber (room temperature and ventilation).
(2) Mixing the vacuum-preserved bagasse powder with glycerol according to the mass ratio of 1:1-1:4, uniformly mixing, and sealing and infiltrating at room temperature for 1-12 h.
(3) Pretreating the soaked raw materials on a double-screw extruder, wherein the extrusion speed is 50-90rpm, the extrusion temperature is 200-240 ℃, and the extrusion times are 1-2.
(4) After the pretreatment is finished, after the temperature of the pretreated raw material is naturally reduced to be below 100 ℃, the pretreated raw material is filtered and washed by 100mL of hot water (100 ℃) per 1g of dry basis.
(5) Drying the washed substrate in an oven at 60 ℃, performing an enzymolysis experiment under the conditions of low enzyme amount (less than 15FPU/g dry substrate) and high substrate concentration (more than 15%), and finally determining the content of glucose in the hydrolysate to be 80-150g/L by using a high performance liquid chromatography.
Example 3 bagasse pretreatment process with base catalyst
(1) Preparing bagasse raw materials: crushing bagasse to 0.5-5mm, vacuum packing, and storing in sample chamber (at room temperature and under ventilation).
(2) Mixing the vacuum-preserved bagasse powder with glycerol according to the mass ratio of 1:1-1:3 (adding 0.2% (w/w) NaOH as a catalyst), uniformly mixing, and sealing and infiltrating at room temperature for 0.5-12 h.
(3) Pretreating the soaked raw materials on a double-screw extruder, wherein the extrusion speed is 50-90rpm, the extrusion temperature is 220-240 ℃, and the extrusion times are 1-3.
(4) After the pretreatment is finished, after the temperature of the pretreated raw material is naturally reduced to be below 100 ℃, the pretreated raw material is filtered and washed by 100mL of hot water (100 ℃) per 1g of dry basis.
(5) Drying the washed substrate in an oven at 60 ℃, carrying out an enzymolysis experiment under the conditions of low enzyme amount (< 15FPU/g dry substrate) and high substrate concentration (> 15%), and finally determining the content of glucose in the hydrolysate to be 140-180g/L by using a high performance liquid chromatography.
Example 4 bagasse pretreatment Process (II)
(1) Preparing bagasse raw materials: crushing bagasse to 0.5-5mm, vacuum packing, and storing in a sample chamber (at room temperature and under ventilation).
(2) Mixing the vacuum-preserved bagasse powder and ethylene glycol according to the mass ratio of 1:1-1:2, and sealing and soaking at room temperature for 0.25-6h after uniform mixing.
(3) Pretreating the soaked raw materials on a double-screw extruder, wherein the extrusion speed is 50-90rpm, the extrusion temperature is 130-150 ℃, and the extrusion times are 1-2.
(4) After the pretreatment is finished, after the temperature of the pretreated raw material is naturally reduced to be below 100 ℃, the pretreated raw material is filtered and washed by 100mL of hot water (100 ℃) per 1g of dry basis.
(5) Drying the washed substrate in an oven at 60 ℃, performing an enzymolysis experiment under the conditions of low enzyme amount (less than 15FPU/g dry substrate) and high substrate concentration (more than 15%), and finally determining the content of glucose in the hydrolysate to be 80-150g/L by using a high performance liquid chromatography.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. An agriculture and forestry biomass pretreatment method is characterized by comprising the following steps:
step (1) preparation of a lignocellulose raw material: smashing the lignocellulose raw material, and packaging and storing the smashed lignocellulose raw material by using a vacuum bag; the lignocellulose raw material is one or a mixture of several of bagasse, corn straw, wheat straw, rice straw and the like;
step (2), mixing and infiltrating high-boiling alcohol and materials: uniformly mixing the crushed lignocellulose with high-boiling alcohol and soaking for 0.25-24 h; the high boiling alcohol includes: glycerin, ethylene glycol, and the like;
and (3) feeding the soaked mixture to a screw extruder and extruding.
2. The method for pretreating agricultural and forestry biomass according to claim 1, wherein the size of the pulverized lignocellulose in the step (1) is 0.25-10 mm.
3. The method for pretreating agricultural and forestry biomass according to claim 1 or 2, wherein the water content of the lignocellulosic raw material in the step (1) is 3-15%.
4. The method for pretreating agricultural and forestry biomass according to claim 1, wherein no catalyst is added or no catalyst is added when the high-boiling alcohol is mixed and soaked with the material in the step (2).
5. The method of claim 4, wherein the catalyst comprises: acid, base, metal salt catalysts, for example: hydrochloric acid, sodium hydroxide, zinc chloride, lithium bromide, and the like.
6. The method for pretreating agricultural and forestry biomass according to claim 1, wherein the mass ratio of the ground lignocellulose in the step (2) to the high-boiling alcohol is 1:1-1: 5.
7. The method for pretreating agricultural and forestry biomass according to any one of claims 1 to 6, wherein the pretreatment extrusion rotating speed in the step (3) is 30 to 90 rpm.
8. The method for pretreating agricultural and forestry biomass according to claim 7, wherein the pretreatment extrusion temperature in the step (3) is 160-250 ℃, more preferably 220-240 ℃.
9. The method for pretreating agricultural and forestry biomass according to claim 1, wherein the number of times of pretreatment extrusion in the step (3) is 1-5.
10. The method of any one of claims 1 to 9, wherein the screw extruder is a twin screw extruder.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101323871A (en) * | 2007-06-13 | 2008-12-17 | 中国科学院过程工程研究所 | Industry glycerol normal pressure pretreatment method of eco-efficient conversion of agricultural straw cellosugar |
| CN101434977A (en) * | 2008-12-23 | 2009-05-20 | 中国石油化工股份有限公司 | Novel method for saccharification of ligno-cellulose |
| CN103711017A (en) * | 2014-01-06 | 2014-04-09 | 海宁朗赛纤维科技有限公司 | Normal pressure ultrasonic-assisted method for preparing cellulose and lignin by using high boiling alcohol as solvent |
| CN105295070A (en) * | 2015-12-03 | 2016-02-03 | 南京林业大学 | Dissolution method for lignocellulose raw material |
| CN105779511A (en) * | 2014-12-26 | 2016-07-20 | 中粮集团有限公司 | Lignocellulose pre-processing method |
| CN109563271A (en) * | 2016-07-18 | 2019-04-02 | Ifp 新能源公司 | By impregnating the method with vapor explosion treatment lignocellulose biomass |
| CN109722932A (en) * | 2019-02-21 | 2019-05-07 | 南京农业大学 | A method of extracting agricultural stalk class waste cellulose |
-
2021
- 2021-01-06 CN CN202110011406.XA patent/CN114717278A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101323871A (en) * | 2007-06-13 | 2008-12-17 | 中国科学院过程工程研究所 | Industry glycerol normal pressure pretreatment method of eco-efficient conversion of agricultural straw cellosugar |
| CN101434977A (en) * | 2008-12-23 | 2009-05-20 | 中国石油化工股份有限公司 | Novel method for saccharification of ligno-cellulose |
| CN103711017A (en) * | 2014-01-06 | 2014-04-09 | 海宁朗赛纤维科技有限公司 | Normal pressure ultrasonic-assisted method for preparing cellulose and lignin by using high boiling alcohol as solvent |
| CN105779511A (en) * | 2014-12-26 | 2016-07-20 | 中粮集团有限公司 | Lignocellulose pre-processing method |
| CN105295070A (en) * | 2015-12-03 | 2016-02-03 | 南京林业大学 | Dissolution method for lignocellulose raw material |
| CN109563271A (en) * | 2016-07-18 | 2019-04-02 | Ifp 新能源公司 | By impregnating the method with vapor explosion treatment lignocellulose biomass |
| CN109722932A (en) * | 2019-02-21 | 2019-05-07 | 南京农业大学 | A method of extracting agricultural stalk class waste cellulose |
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