CN110205412B - Method for preparing glucose by hydrolyzing and saccharifying non-enzymatic cellulose - Google Patents
Method for preparing glucose by hydrolyzing and saccharifying non-enzymatic cellulose Download PDFInfo
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Abstract
The invention provides a non-enzymatic cellulose hydrolysis saccharification technology, which specifically comprises the following steps: mixing cellulose-containing biomass and solid oxide, mechanically pulverizing, heat treating, and hydrolyzing and saccharifying. The invention has the advantages and beneficial effects that: the method has the advantages that the lignocellulose is pretreated by combining mechanical energy and heat energy, the energy consumption problem of pretreating the lignocellulose by a single mechanical method is greatly reduced, the reaction conditions are mild, the cellulose-containing biomass material is efficiently converted into monosaccharide products under the condition of low energy consumption, the energy consumption is low, the pollution is small, and the biomass sugar platform development and the industrialization process of bio-based products are effectively promoted.
Description
Technical Field
The invention belongs to the technical field of biomass energy, and particularly relates to a non-enzymatic cellulose hydrolysis and saccharification technology.
Background
Lignocellulose is an inexhaustible renewable biomass resource in nature. With the decline of petroleum and coal reserves and the growing concern of human beings about environmental pollution, the raw materials of the world chemical industry are gradually shifting from fossil resources to biomass resources, and lignocellulose is considered as a green biological resource most likely to replace fossil energy. Lignocellulosic biomass is composed of three components, cellulose, hemicellulose, and lignin). Cellulose and hemicellulose are mainly high polymers of sugars, while lignin is an aromatic polymer with phenylpropane as a basic unit. The lignocellulose biomass can be converted into monosaccharide substances through hydrolysis and saccharification, and the monosaccharide substances can be converted into bio-based fuels, fuel additives, fine chemicals and the like through chemical and biological catalytic ways by taking the monosaccharide substances as a platform; the monosaccharide crystals obtained by using the crystallization purification technology are more important industrial raw materials. Therefore, lignocellulose-derived biomass sugar is a main raw material and an important platform substance of a bio-based product, the subsequent development and industrialization process of the bio-based product must be promoted by enhancing the research and development of a biomass sugar platform, a new biomass resource efficient utilization integrated industry is established, and the sustainable development of the economic society is realized.
The process of producing carbohydrate intermediates using lignocellulosic biomass is quite challenging. At present, lignocellulose hydrolysis saccharification technology mainly focuses on two ways of acid hydrolysis and enzyme hydrolysisAlthough the saccharification process has mild conditions, the cost of the cellulase is too high, and the industrial production is difficult to realize. The hydrolysis of the liquid sulfuric acid and the hydrochloric acid not only corrodes equipment, but also generates a large amount of waste water after post-treatment; solid acid hydrolysis also has the problem of catalyst contact with lignocellulose, and the catalyst is difficult to recycle. Cellulose is difficult to reach by hydrolysis catalysts due to its stable and complex supramolecular morphological structure, resulting in inefficient reactions. To enhance the accessibility of cellulose, the macromolecular chain structure of cellulose is first destroyed, increasing the amorphous regions and contact area of cellulose. Mechanical activation can improve the reactivity of the solid, and patent CN201410787022 discloses a method for degrading cellulose by mechanical activation in cooperation with metal salt. According to the method, the mixture of cellulose and metal salt is placed into a ball mill, and ball milling activation is carried out for 10-180 minutes at the temperature of 30-90 ℃, and the result shows that the polymerization degree of the cellulose is greatly reduced, the accessibility and the reaction activity of a cellulose degradation product are effectively improved, but only a cellulose oligomer is obtained in the system, and monosaccharide cannot be obtained. CN201510278766.0 discloses a method for preparing xylose hydrolysate by pretreatment of corncobs through oxalic acid mixed ball milling. Firstly, grinding and screening corncobs, mixing the screened corncobs with an oxalic acid solution for ball milling pretreatment, adding water into the mixture after ball milling, carrying out ultrasonic treatment, and then carrying out hydrothermal pretreatment in a microwave reaction kettle, so that a xylose solution is obtained, and cellulose is not hydrolyzed. Literature referenceChem. Sci., 2016, 7, 692–696 The eucalyptus bark and the catalyst are mixed and ball-milled for two hours by adopting a planetary ball mill, and then the yield of the hydrolyzed glucose can reach 80% in the presence of 120ppm hydrochloric acid, but trace hydrochloric acid is still used and the concentration of the recovered sugar solution is very low. Patent CN201711010502.2 discloses a method for hydrolyzing and fermenting lignocellulose catalyzed by phosphorus pentoxide, wherein 80% of glucose yield can be obtained by mixing and ball-milling lignocellulose and phosphorus pentoxide for two hours and then directly hydrolyzing; however, the ball milling time in the process is too long, so that the energy consumption for treatment is too high.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention aims to provide a hydrolysis saccharification process which combines mechanical energy and heat energy to pretreat lignocellulose, reduces saccharification energy consumption and investment operation cost, and develops high efficiency and low energy consumption. The technology successfully improves the yield and efficiency of lignocellulose hydrolysis fermentation, effectively separates out lignin components in the treatment process, does not introduce excessive metal ions, realizes the maximum utilization of lignocellulose raw materials, and effectively promotes the realization of industrialization process of bio-based products.
The invention specifically provides a non-enzymatic cellulose hydrolysis saccharification technology, which specifically comprises the following steps: adding solid oxide to mix with lignocellulose raw material containing cellulose, and carrying out hydrolysis saccharification after pretreatment of the cellulose biomass raw material by combining mechanical energy and heat energy. After the reaction is finished, solid-liquid separation is carried out to respectively obtain sugar solution and lignin components, thereby realizing the maximum recycling of the lignocellulose biomass raw material.
The solid oxide includes, but is not limited to, a phosphorus-containing oxide, a vanadium-containing oxide, a copper-containing oxide, an iron-containing oxide, a cobalt-containing oxide, a nickel-containing oxide, an aluminum-containing oxide, a zinc-containing oxide, a tin-containing oxide, and the like.
The solid oxide includes, but is not limited to, phosphorus pentoxide.
The mechanical energy includes, but is not limited to, ball milling, hammer milling, grinding, extrusion.
Including but not limited to thermal radiation, optical radiation, microwaves, and electromagnetic heating.
The method for pretreating the raw material by combining mechanical energy and thermal energy comprises but is not limited to mixing the cellulose-containing biomass raw material with solid oxide, crushing the mixture by mechanical energy, and then performing mechanical energy crushing on the crushed mixture at a temperature of between 50 and 250 DEG CoC, heat treatment for 10-120 min.
The method for pretreating the raw material by combining mechanical energy and thermal energy comprises but is not limited to mixing the cellulose-containing biomass raw material with the solid oxide, and simultaneously carrying out heat treatment and mechanical crushing, wherein the heat treatment temperature is 50-250 DEG CoC。
The mass ratio of the solid oxide to the cellulose-containing biomass is 0.1-20%.
The hydrolysis saccharification is to make the solid-liquid mass ratio of the pretreated cellulose-containing raw material to water be 1.0-50%.
The hydrolysis saccharification temperature is 100-250 ℃, and the hydrolysis saccharification time is 10-120 min. The biomass raw material containing cellulose is selected from one or more biomass materials containing lignocellulose, such as microcrystalline cellulose, straws, corncobs, reed grasses, sorghum, willow branches, xylose residues, furfural residues, sweet sorghum, willow branches, bagasse, branches and leaves, waste wood, wood chips and other natural biomass and fiber pulp products including waste paper, waste cartons and the like.
The invention has the advantages and beneficial effects that: the method has the advantages that the lignocellulose is pretreated by combining mechanical energy and heat energy, the energy consumption problem of pretreating the lignocellulose by a single mechanical method is greatly reduced, the reaction conditions are mild, the cellulose-containing biomass material is efficiently converted into monosaccharide products under the condition of low energy consumption, the energy consumption is low, the pollution is small, and the biomass sugar platform development and the industrialization process of bio-based products are effectively promoted.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.
All the starting materials of the present invention are not particularly limited in purity, and the reagents used in the following examples are commercially available. Analytical purification is preferably used in the present invention.
Qualitative and quantitative detection instrument: high Performance Liquid Chromatography (HPLC) is Agilent 1260, liquid chromatography column is 87-H ion exchange column, column temperature is 65 ℃, parallax refraction detector is 50 ℃; mobile phase: 5Mm H2SO4The flow rate was 0.6ml/min, and the amount of sample was 25 uL.
Comparative example 1
50g of corn straw and 2.5g of phosphorus pentoxide are weighed, mixed and placed in a ball milling tank for ball milling for 120 minutes. Then weighing 4g of ball-milled sample, adding 40mL of water into the reaction kettle, and carrying out hydrolysis reaction for 40min at 215 ℃. After the reaction is finished, cooling to room temperature, and collecting a liquid product. Qualitative and quantitative analysis by HPLC gave a glucose yield of 51%.
Comparative example 2
Weighing 50g of corn straw and 2.5g of phosphorus pentoxide, uniformly mixing, and heating 180 DEGoC, treating for 60 minutes. Then weighing 4g of ball-milled sample, adding 40mL of water into the reaction kettle, and carrying out hydrolysis reaction for 40min at 215 ℃. After the reaction is finished, cooling to room temperature, and collecting a liquid product. Qualitative and quantitative analysis by HPLC gave a glucose yield of 5.5%.
Comparative example 3
50g of corn straw and 2.5g of phosphorus pentoxide are weighed, mixed and placed in a ball milling tank for ball milling for 30 minutes. Then weighing 4g of ball-milled sample, adding 40mL of water into the reaction kettle, and carrying out hydrolysis reaction for 40min at 215 ℃. After the reaction is finished, cooling to room temperature, and collecting a liquid product. Qualitative and quantitative analysis by HPLC gave a glucose yield of 20%.
Example 1
Preparation of lignocellulose hydrolysate
Weighing 50g of corn straw and 2.5g of phosphorus pentoxide, mixing, placing in a ball milling tank, ball milling for 30 minutes, and heating to 180 DEGoC, treating for 60 minutes. Then weighing 4g of ball-milled sample, adding 40mL of water into the reaction kettle, and carrying out hydrolysis reaction for 40min at 215 ℃. After the reaction is finished, cooling to room temperature, and collecting a liquid product. Qualitative and quantitative analysis by HPLC gave a glucose yield of 50.1%.
Example 2
Weighing 50g of corn straw and 5g of phosphorus pentoxide, mixing, placing in a ball milling tank, ball milling for 30 minutes, and heating to 140%oC, treating for 60 minutes. Then weighing 4g of ball-milled sample, adding 40mL of water into the reaction kettle, and carrying out hydrolysis reaction for 40min at 215 ℃. After the reaction is finished, cooling to room temperature, and collecting a liquid product. Qualitative and quantitative analysis by HPLC gave a glucose yield of 52.3%.
Example 3
Weighing 50g of corn straw and 5g of phosphorus pentoxide, mixing, placing in a ball milling tank, ball milling for 30 minutes, and heating to 80%oC, treating for 60 minutes. Then weighing 4g of ball-milled sample, adding 40mL of water into the reaction kettle, and carrying out hydrolysis reaction for 40min at 215 ℃. After the reaction is finished, cooling to room temperature, and collecting a liquid product. Qualitative and quantitative analysis by HPLC gave a glucose yield of 45.3%.
Example 4
Weighing 50g of straw furfural residues and 5g of phosphorus pentoxide, mixing, placing in a ball milling tank, ball milling for 30 minutes, and heating to 140%oC, treating for 60 minutes. Then weighing 4g of ball-milled sample, adding 40mL of water into the reaction kettle, and carrying out hydrolysis reaction for 40min at 200 ℃. After the reaction is finished, cooling to room temperature, and collecting a liquid product. Qualitative and quantitative analysis by HPLC gave a glucose yield of 59.5%.
Example 5
Weighing 50g of straw furfural residues and 5g of phosphorus pentoxide, mixing, placing in a ball milling tank, ball milling for 30 minutes, and then heating to 140 ℃ for treatment for 60 minutes. Then 8g of ball-milled sample is weighed in a reaction kettle, 40mL of water is added, and hydrolysis reaction is carried out for 40min at 215 ℃. After the reaction is finished, cooling to room temperature, and collecting a liquid product. Qualitative and quantitative analysis by HPLC gave a glucose yield of 50.8%.
Example 6
Weighing 50g of rice hull furfural residues and 2.5g of phosphorus pentoxide, mixing, placing in a ball milling tank, ball milling for 10 minutes, and heating to 140 DEGoC, treating for 60 minutes. Then 8g of ball-milled sample is weighed in a reaction kettle, 40mL of water is added, and hydrolysis reaction is carried out for 30min at the temperature of 200 ℃. After the reaction is finished, cooling to room temperature, and collecting a liquid product. Qualitative and quantitative analysis by HPLC gave a glucose yield of 58.1%.
Example 7
Weighing 50g of rice hull furfural residues and 2.5g of phosphorus pentoxide, mixing, placing in a ball milling tank, ball milling for 20 minutes, and heating to 140 DEGoC, treating for 60 minutes. Then 8g of ball-milled sample is weighed in a reaction kettle, 40mL of water is added, and hydrolysis reaction is carried out for 30min at the temperature of 200 ℃. After the reaction is finished, cooling to room temperature, and collectingAnd (3) liquid products. Qualitative and quantitative analysis by HPLC gave a glucose yield of 65.1%.
Example 8
Weighing 50g of rice hull furfural residues and 2.5g of phosphorus pentoxide, mixing, placing in a ball milling tank, ball milling for 30 minutes, and heating to 140%oC, treating for 60 minutes. Then 8g of ball-milled sample is weighed in a reaction kettle, 40mL of water is added, and hydrolysis reaction is carried out for 30min at the temperature of 200 ℃. After the reaction is finished, cooling to room temperature, and collecting a liquid product. Qualitative and quantitative analysis by HPLC gave a glucose yield of 70.4%.
Example 9
Weighing 50g of rice hull furfural residues and 1.5g of phosphorus pentoxide, mixing, placing in a ball milling tank, ball milling for 40 minutes, and heating to 140 DEGoC, treating for 60 minutes. Then weighing 12g of ball-milled sample into a reaction kettle, adding 40mL of water, and carrying out hydrolysis reaction for 40min at 190 ℃. After the reaction is finished, cooling to room temperature, and collecting a liquid product. Qualitative and quantitative analysis by HPLC gave a glucose yield of 73.4%.
Example 10
Weighing 50g of rice hull furfural residues and 0.5g of phosphorus pentoxide, mixing, placing in a ball milling tank, ball milling for 60 minutes, and heating to 140 DEGoC, treating for 60 minutes. Then 16g of ball-milled sample is weighed in a reaction kettle, 40mL of water is added, and hydrolysis reaction is carried out for 40min at 190 ℃. After the reaction is finished, cooling to room temperature, and collecting a liquid product. Qualitative and quantitative analysis by HPLC gave a glucose yield of 46.4%.
Example 11
Weighing 50g of rice hull furfural residues and 2.5g of phosphorus pentoxide, mixing, placing in a ball milling tank, ball milling for 30 minutes, and heating to 140%oC, treating for 10 minutes. Then 8g of ball-milled sample is weighed in a reaction kettle, 40mL of water is added, and hydrolysis reaction is carried out for 30min at the temperature of 200 ℃. After the reaction is finished, cooling to room temperature, and collecting a liquid product. Qualitative and quantitative analysis by HPLC gave a glucose yield of 50.4%.
Example 12
Weighing 50g of rice hull furfural residues and 2.5g of phosphorus pentoxide, mixing, placing in a ball milling tank, ball milling for 30 minutes, and heating to 140%oC, treating for 30 minutes. Then 8g of ball-milled sample is weighed in a reaction kettle, 40mL of water is added, and hydrolysis reaction is carried out for 30min at the temperature of 200 ℃. After the reaction is finished, cooling to room temperature, and collecting a liquid product. Qualitative and quantitative analysis by HPLC gave a glucose yield of 60.4%.
Example 13
Weighing 50g of rice hull furfural residues and 2.5g of phosphorus pentoxide, mixing, placing in a ball milling tank, ball milling for 30 minutes, and heating to 140%oC, treating for 60 minutes. Then 8g of ball-milled sample is weighed in a reaction kettle, 40mL of water is added, and hydrolysis reaction is carried out for 60min at the temperature of 150 ℃. After the reaction is finished, cooling to room temperature, and collecting a liquid product. Qualitative and quantitative analysis by HPLC gave a glucose yield of 45.4%.
Example 14
Weighing 50g of rice hull furfural residues and 2.5g of phosphorus pentoxide, mixing, placing in a ball milling tank, ball milling for 30 minutes, and heating to 140%oC, treating for 60 minutes. Then 8g of ball-milled sample is weighed in a reaction kettle, 40mL of water is added, and hydrolysis reaction is carried out for 120min at the temperature of 150 ℃. After the reaction is finished, cooling to room temperature, and collecting a liquid product. Qualitative and quantitative analysis by HPLC gave a glucose yield of 48.5%.
Example 15
Weighing 50g of rice hull furfural residues and 2.5g of phosphorus pentoxide, mixing, placing in a ball milling tank, ball milling for 60 minutes, and heating to 150%oC, treating for 60 minutes. Then 8g of ball-milled sample is weighed in a reaction kettle, 40mL of water is added, and hydrolysis reaction is carried out for 40min at 190 ℃. After the reaction is finished, cooling to room temperature, and collecting a liquid product. Qualitative and quantitative analysis by HPLC gave a glucose yield of 78%.
Example 16
Weighing 50g of fast-growing poplar furfural residues and 2.5g of phosphorus pentoxide, mixing, placing in a ball milling tank, ball milling for 30 minutes, and heating to 180 DEGoC, treating for 60 minutes. Then 20g of ball-milled sample is weighed in a reaction kettle, 40mL of water is added, and hydrolysis reaction is carried out for 50min at 190 ℃. After the reaction is finished, cooling to room temperature, and collecting a liquid product. Qualitative and quantitative analysis by HPLC gave a glucose yield of 65.2%.
Example 17
Weighing 50g of fast-growing poplar furfural residues and 2.5g of phosphorus pentoxide, mixing, placing in a ball milling tank, ball milling for 30 minutes, and heating to 180 DEGoC, treating for 60 minutes. Then 2g of ball-milled sample is weighed in a reaction kettle, 40mL of water is added, and hydrolysis reaction is carried out for 50min at the temperature of 150 ℃. After the reaction is finished, cooling to room temperature, and collecting a liquid product. Qualitative and quantitative analysis by HPLC gave a glucose yield of 50.2%.
Example 18
Weighing 50g of fast-growing poplar and 10g of phosphorus pentoxide, mixing, placing in a ball milling tank, ball milling for 30 minutes, and heating to 150%oC, treating for 60 minutes. Then 0.4g of ball-milled sample is weighed in a reaction kettle, 40mL of water is added, and hydrolysis reaction is carried out for 30min at 190 ℃. After the reaction is finished, cooling to room temperature, and collecting a liquid product. Qualitative and quantitative analysis by HPLC gave a glucose yield of 55.2%.
Example 19
Weighing 50g of fast-growing poplar and 5g of phosphorus pentoxide, mixing, placing in a ball milling tank, ball milling for 30 minutes, and heating to 150%oC, treating for 60 minutes. Then weighing 4g of ball-milled sample, putting the ball-milled sample into a reaction kettle, adding 40mL of water, and carrying out hydrolysis reaction for 30min at 190 ℃. After the reaction is finished, cooling to room temperature, and collecting a liquid product. Qualitative and quantitative analysis by HPLC gave a glucose yield of 48.2%.
Example 20
Weighing 50g of fast-growing poplar and 2.5g of phosphorus pentoxide, mixing, placing in a ball milling tank, ball milling for 30 minutes, and heating to 140 DEGoC, treating for 120 minutes. Then weighing 4g of ball-milled sample, adding 40mL of water into the reaction kettle, and carrying out hydrolysis reaction for 40min at 190 ℃. After the reaction is finished, cooling to room temperature, and collecting a liquid product. Qualitative and quantitative analysis by HPLC gave a glucose yield of 75.2%.
The preparation data of the lignocellulose hydrolysates in the examples 1 to 20 are shown in table 1, 50g of different types of lignocellulose biomass is weighed, the mass ratio of phosphorus pentoxide to the lignocellulose biomass, the ball milling time, the heat treatment temperature, the heat treatment time, the hydrolysis temperature, the hydrolysis time and other conditions are carried out according to the scheme in table 1, after the hydrolysis reaction is finished, the lignocellulose hydrolysate is cooled to the room temperature, and the liquid product is collected. Qualitative and quantitative analysis by HPLC gave the glucose yields shown in table 1.
TABLE 1 preparation of lignocellulosic Hydrosaccharification liquid
Claims (4)
1. A method for preparing glucose by hydrolyzing and saccharifying non-enzymatic cellulose is characterized in that solid oxide is mixed with a biomass raw material containing cellulose, and the hydrolysis and saccharification are carried out after the cellulose biomass raw material is pretreated by combining mechanical energy and heat energy;
the raw material pretreatment method combining mechanical energy and heat energy comprises the steps of mixing cellulose-containing biomass raw material and solid oxide, crushing by using mechanical energy, and then carrying out heat treatment at 50-250 ℃ for 10-120 min; the solid oxide comprises phosphorus pentoxide;
the raw material pretreatment method combining mechanical energy and heat energy comprises the steps of mixing a cellulose-containing biomass raw material with a solid oxide, and performing heat treatment and mechanical crushing simultaneously, wherein the heat treatment is 50-250 ℃;
the mass ratio of the solid oxide to the cellulose-containing biomass is 0.1-20: 100, respectively; the hydrolysis saccharification is to mix the pretreated cellulose-containing raw material and water in a solid-liquid mass ratio of 1.0-50: 100, and hydrolyzing and saccharifying the mixture at 100-250 ℃ for 10-120 min.
2. The method of claim 1, wherein the mechanical energy comprises ball milling, hammer milling, grinding and extrusion.
3. The method of claim 1, wherein said thermal energy comprises light radiation, microwaves and electromagnetic heating.
4. The process of claim 1, wherein the cellulose-containing biomass feedstock is selected from the group consisting of one or more of microcrystalline cellulose, straw, corn cobs, reed grass, sorghum, switchgrass, xylose residues, furfural residues, sugar cane bagasse, wood waste, wood chips, and lignocellulose-containing biomass materials including waste paper, waste paper boxes, and other fibrous pulp products.
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