CN108330723B - Method for extracting cellulose by utilizing amorpha fruticosa planted in saline-alkali soil - Google Patents
Method for extracting cellulose by utilizing amorpha fruticosa planted in saline-alkali soil Download PDFInfo
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- CN108330723B CN108330723B CN201711455090.3A CN201711455090A CN108330723B CN 108330723 B CN108330723 B CN 108330723B CN 201711455090 A CN201711455090 A CN 201711455090A CN 108330723 B CN108330723 B CN 108330723B
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C3/00—Pulping cellulose-containing materials
- D21C3/20—Pulping cellulose-containing materials with organic solvents or in solvent environment
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
- D21C9/001—Modification of pulp properties
- D21C9/002—Modification of pulp properties by chemical means; preparation of dewatered pulp, e.g. in sheet or bulk form, containing special additives
- D21C9/004—Modification of pulp properties by chemical means; preparation of dewatered pulp, e.g. in sheet or bulk form, containing special additives inorganic compounds
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
- D21C9/001—Modification of pulp properties
- D21C9/007—Modification of pulp properties by mechanical or physical means
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
- D21C9/10—Bleaching ; Apparatus therefor
- D21C9/1084—Bleaching ; Apparatus therefor with reducing compounds
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- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention relates to the technical field of cellulose extraction, in particular to a method for extracting cellulose by utilizing amorpha fruticosa planted in saline-alkali soil. The extraction method of the invention improves the yield and purity of the cellulose.
Description
Technical Field
The invention relates to the technical field of chemical fibers, in particular to a method for extracting cellulose by utilizing amorpha fruticosa planted in saline-alkali soil.
Background
Amorpha fruticosa is a perennial leguminous deciduous shrub, and due to the characteristics of fast growth, strong fertility, wide adaptability, saline-alkali water humidity resistance and the like, green manure and saline-alkali soil are widely used for improving tree species in coastal and low-lying saline-alkali areas.
The amorpha fruticosa contains cellulose, hemicellulose and lignin ash as main chemical components, so that the amorpha fruticosa can be used for pulping and papermaking, fiberboards and composite boards. In the prior art, a large amount of process methods for extracting cellulose exist, but the process for extracting the cellulose from the amorpha fruticosa is not reported.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: aiming at the defects in the prior art, the method for extracting the cellulose by using the amorpha fruticosa planted in the saline-alkali soil is provided, and the yield of the cellulose can be improved by using the method.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a method for extracting cellulose by utilizing amorpha fruticosa planted in saline-alkali soil comprises the following steps:
(1) pretreatment: peeling amorpha fruticosa, pulverizing, sieving, oven drying, and cooling to obtain amorpha fruticosa wood powder;
(2) acid cooking treatment: taking the amorpha fruticosa wood flour in the step (1), adding a mixed solution of an organic solvent, an organic acid and a surfactant, stirring, heating, cooking, cooling, filtering, repeatedly washing collected filter residues with the organic solvent, and then washing with deionized water;
(3) alkali cooking treatment: adding an alkali liquor-organic solvent mixed solution into the filter residue washed by the organic solvent and the deionized water in the step (2), performing ultrasonic treatment, heating, cooking, filtering, and collecting solid filtrate;
(4) bleaching treatment: adding the solid filtrate obtained in the step (3) into an organic acid-bleaching agent mixed solution for bleaching to obtain amorpha fruticosa white pulp;
(5) microwave treatment: and (4) adding the amorpha fruticosa white pulp obtained in the step (4) into a calcium hydroxide solution, performing microwave treatment, filtering, and drying to obtain the amorpha fruticosa cellulose.
As an improved technical scheme, in the mixed solution of the organic solvent, the organic acid and the surfactant in the step (2), the organic solvent is ethanol, n-butanol or isopropanol; the organic acid is citric acid, tartaric acid or oxalic acid; the surfactant is sodium dodecyl benzene sulfonate or tween-60.
As a preferable technical solution, the mixed solution of the organic solvent, the organic acid and the surfactant is a mixed solution of ethanol/isopropanol-tartaric acid-tween-60.
As a further preferable technical scheme, the volume concentration of the ethanol is 65-80%.
As an improved technical proposal, the cooking temperature in the step (2) is 120-180 ℃, and the cooking time is 1-3 h.
As a preferable technical scheme, the temperature of the ultrasonic treatment in the step (3) is 80-120 ℃, the time is 1-4h, and the power of the ultrasonic wave is 200-400 w.
As an improved technical scheme, the mixed solution of the alkali liquor and the organic solvent in the step (3) is a mixed solution of 0.5-1mol of sodium hydroxide solution/potassium hydroxide solution-isopropanol.
As an improved technical scheme, the mixed solution of organic acid and bleaching agent in the step (4) is mixed solution of acetic acid-tetraacetylethylenediamine/sodium hypochlorite/sodium sulfite.
As a preferable technical scheme, the bleaching temperature in the step (4) is 60-100 ℃, and the bleaching time is 1-2 h.
As an improved technical scheme, the power of the microwave treatment in the step (5) is 200-300w, and the temperature is 80-120 ℃.
After the technical scheme is adopted, the invention has the beneficial effects that:
compared with the prior art, the invention mainly has the following advantages:
(1) the method takes amorpha fruticosa planted in saline-alkali soil as a raw material, the amorpha fruticosa is crushed and subjected to acid boiling treatment, an ethanol-tartaric acid-tween-60 mixed solution is added, and after high-temperature boiling, the ethanol-tartaric acid-tween-60 enters cells and fully contacts with cell tissues, so that the contact area of lignin and the mixed solution is increased, a large amount of lignin is degraded and dissolved in ethanol, and meanwhile, part of hemicellulose is also degraded; adding mixed solution of sodium hydroxide solution/potassium hydroxide solution-isopropanol, and performing ultrasonic treatment and cooking treatment to break the cross-linking structure between cellulose and hemicellulose and degrade a large amount of hemicellulose and dissolve the hemicellulose in the isopropanol; the lignin and hemicellulose are further removed through bleaching treatment and microwave treatment, and the yield of cellulose products is greatly improved.
(2) The invention adopts microwave and ultrasonic assisted solvent method, can effectively remove lignin and hemicellulose, reduces the using amount of solvent and lightens the pollution to the environment.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A method for extracting cellulose by utilizing amorpha fruticosa planted in saline-alkali soil comprises the following steps:
(1) pretreatment: peeling amorpha fruticosa, pulverizing, sieving, oven drying, and cooling to obtain amorpha fruticosa wood powder;
(2) acid cooking treatment: taking the amorpha fruticosa wood flour in the step (1), adding an organic solvent-organic acid-surfactant mixed solution (65% ethanol-tartaric acid-tween-60 mixed solution in a volume concentration of 1:1:0.5) with a volume 8 times of the weight of the amorpha fruticosa wood flour, stirring, heating to 120 ℃, cooking for 1h, cooling, filtering, repeatedly washing the collected filter residue with an organic solvent, and washing with deionized water;
(3) alkali cooking treatment: adding an alkali liquor-organic solvent mixed solution (0.5mol of a sodium hydroxide solution/potassium hydroxide solution-isopropanol mixed solution with the volume ratio of 1:1) with the weight of 5 times of the filter residue in the filter residue washed by the organic solvent and the deionized water in the step (2), heating to 80 ℃, carrying out ultrasonic treatment for 1h under the condition that the power of ultrasonic wave is 200w, heating to 130 ℃, cooking for 1h, filtering, and collecting a solid filtrate;
(4) bleaching treatment: taking the solid filtrate obtained in the step (3), adding an organic acid-bleaching agent (acetic acid-tetraacetylethylenediamine mixed solution) mixed solution with the volume 5 times of the weight of the solid filtrate, heating to 60 ℃, and bleaching for 1h to obtain amorpha fruticosa white pulp;
(5) microwave treatment: and (4) adding the amorpha fruticosa white pulp obtained in the step (4) into a calcium hydroxide solution according to the volume ratio of 1:2, treating under the conditions of the power of 200w and the temperature of 80 ℃, filtering, and drying to obtain the amorpha fruticosa cellulose.
The yield of amorpha fruticosa cellulose under the process condition is 78.56%.
Example 2
A method for extracting cellulose by utilizing amorpha fruticosa planted in saline-alkali soil comprises the following steps:
(1) pretreatment: peeling amorpha fruticosa, pulverizing, sieving, oven drying, and cooling to obtain amorpha fruticosa wood powder;
(2) acid cooking treatment: taking the amorpha fruticosa wood flour in the step (1), adding an organic solvent-organic acid-surfactant mixed solution (70% ethanol-tartaric acid-tween-60 mixed solution in a volume concentration of 2:1:1) in an amount which is 10 times the weight of the amorpha fruticosa wood flour, stirring, heating to 135 ℃, cooking for 1.8h, cooling, filtering, repeatedly washing the collected filter residues with an organic solvent, and washing with deionized water;
(3) alkali cooking treatment: adding an alkali liquor-organic solvent mixed solution (0.6mol of a sodium hydroxide solution-isopropanol mixed solution, wherein the volume ratio of the alkali liquor to the isopropanol is 2:1) with the volume of 8 times of the weight of the filter residue into the filter residue washed by the organic solvent and the deionized water in the step (2), heating to 90 ℃, carrying out ultrasonic treatment for 2 hours under the condition that the ultrasonic power is 280w, heating to 138 ℃, cooking for 1.5 hours, filtering, and collecting a solid filtrate;
(4) bleaching treatment: taking the solid filtrate obtained in the step (3), adding an organic acid-bleaching agent (acetic acid-sodium hypochlorite mixed solution) mixed solution with the volume 8 times of the weight of the solid filtrate, heating to 80 ℃, and bleaching for 1.5 hours to obtain amorpha fruticosa white pulp;
(5) microwave treatment: and (4) adding the amorpha fruticosa white pulp obtained in the step (4) into a calcium hydroxide solution according to the volume ratio of 1:5, treating under the conditions of power of 260w and temperature of 90 ℃, filtering and drying to obtain the amorpha fruticosa cellulose.
The yield of the amorpha fruticosa cellulose under the process conditions is 79.25 percent
Example 3
A method for extracting cellulose by utilizing amorpha fruticosa planted in saline-alkali soil comprises the following steps:
(1) pretreatment: peeling amorpha fruticosa, pulverizing, sieving, oven drying, and cooling to obtain amorpha fruticosa wood powder;
(2) acid cooking treatment: taking the amorpha fruticosa wood flour in the step (1), adding an organic solvent-organic acid-surfactant mixed solution (isopropanol-tartaric acid-tween-60 mixed solution, wherein the volume ratio of ethanol to tartaric acid to tween-60 is 3.5:2:1) in an amount which is 12 times the weight of the amorpha fruticosa wood flour, stirring, heating to 155 ℃, cooking for 2.5h, cooling, filtering, repeatedly washing collected filter residues with an organic solvent, and then washing with deionized water;
(3) alkali cooking treatment: adding an alkali liquor-organic solvent mixed solution (0.8mol of a sodium hydroxide solution/potassium hydroxide solution-isopropanol mixed solution with the volume ratio of 3:1) with the volume being 12 times of the weight of the filter residue into the filter residue washed by the organic solvent and the deionized water in the step (2), heating to 115 ℃, carrying out ultrasonic treatment for 3 hours under the condition that the power of ultrasonic wave is 365w, heating to 145 ℃, cooking for 2.5 hours, filtering, and collecting a solid filtrate;
(4) bleaching treatment: taking the solid filtrate obtained in the step (3), adding an organic acid-bleaching agent (acetic acid-sodium sulfite mixed solution) mixed solution with the volume 10 times of the weight of the solid filtrate, heating to 95 ℃, and bleaching for 1.8 hours to obtain amorpha fruticosa white pulp;
(5) microwave treatment: and (4) adding the amorpha fruticosa white pulp obtained in the step (4) into a calcium hydroxide solution according to the volume ratio of 1:6, treating under the conditions of power of 260w and temperature of 115 ℃, filtering and drying to obtain the amorpha fruticosa cellulose.
The yield of amorpha fruticosa cellulose under the process conditions is 84.18%.
Example 4
A method for extracting cellulose by utilizing amorpha fruticosa planted in saline-alkali soil comprises the following steps:
(1) pretreatment: peeling amorpha fruticosa, pulverizing, sieving, oven drying, and cooling to obtain amorpha fruticosa wood powder;
(2) acid cooking treatment: taking the amorpha fruticosa wood flour in the step (1), adding a mixed solution (a mixed solution of 80% ethanol-tartaric acid-tween-60 in a volume concentration of 5:3:2) of an organic solvent-organic acid-surfactant in an amount which is 15 times the weight of the amorpha fruticosa wood flour, stirring, heating to 180 ℃, cooking for 3h, cooling, filtering, repeatedly washing collected filter residues with the organic solvent, and washing with deionized water;
(3) alkali cooking treatment: adding an alkali liquor-organic solvent mixed solution (1mol of a sodium hydroxide solution-isopropanol mixed solution, wherein the volume ratio of the alkali liquor to the isopropanol is 3.5:1) with the volume 15 times of the weight of the filter residue into the filter residue washed by the organic solvent and the deionized water in the step (2), heating to 120 ℃, carrying out ultrasonic treatment for 4 hours under the condition that the ultrasonic power is 400w, heating to 150 ℃, cooking for 3 hours, filtering, and collecting a solid filtrate;
(4) bleaching treatment: taking the solid filtrate obtained in the step (3), adding an organic acid-bleaching agent (acetic acid-sodium sulfite mixed solution) mixed solution with the volume being 12 times of the weight of the solid filtrate, heating to 100 ℃, and bleaching for 2 hours to obtain amorpha fruticosa white pulp;
(5) microwave treatment: and (4) adding the amorpha fruticosa white pulp obtained in the step (4) into a calcium hydroxide solution according to the volume ratio of 1:8, treating under the conditions of the power of 300w and the temperature of 120 ℃, filtering and drying to obtain the amorpha fruticosa cellulose.
The yield of amorpha fruticosa cellulose under the process conditions is 83.25%.
In order to better prove that the yield of the cellulose product can be improved by extracting the cellulose by using the preparation method disclosed by the invention, 3 comparative examples are simultaneously made in the invention.
Comparative example 1
Different from the example 3, the mixed solution of ethanol and tartaric acid is added in the step (2), the other conditions are the same, and the yield of the amorpha fruticosa cellulose under the process condition is 77.68%.
Comparative example 2
Unlike example 3, ethanol and acid were added in step (3), no sonication was performed, and the same conditions were used, with an amorpha fruticosa cellulose yield of 77.85%.
Comparative example 3
Unlike example 3, only bleaching agent was added in step (4) and microwave treatment was not performed in step (5), and the yield of amorpha fruticosa cellulose under the same process conditions was 78.42%.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (7)
1. A method for extracting cellulose by utilizing amorpha fruticosa planted in saline-alkali soil is characterized by comprising the following steps:
(1) pretreatment: peeling amorpha fruticosa, pulverizing, sieving, oven drying, and cooling to obtain amorpha fruticosa wood powder;
(2) acid cooking treatment: taking the amorpha fruticosa wood flour in the step (1), adding a mixed solution of an organic solvent, an organic acid and a surfactant, stirring, heating, cooking, cooling, filtering, repeatedly washing collected filter residues with the organic solvent, and then washing with deionized water; wherein the organic solvent in the mixed solution of the organic solvent, the organic acid and the surfactant is ethanol, n-butanol or isopropanol; the organic acid is citric acid, tartaric acid or oxalic acid; the surfactant is tween-60; the cooking temperature is 120-;
(3) alkali cooking treatment: adding an alkali liquor-organic solvent mixed solution into the filter residue washed by the organic solvent and the deionized water in the step (2), performing ultrasonic treatment, heating, cooking, filtering, and collecting solid filtrate; wherein the mixed solution of the alkali liquor and the organic solvent is a mixed solution of 0.5-1mol of sodium hydroxide solution/potassium hydroxide solution-isopropanol;
(4) bleaching treatment: adding the solid filtrate obtained in the step (3) into an organic acid-bleaching agent mixed solution for bleaching to obtain amorpha fruticosa white pulp;
(5) microwave treatment: and (4) adding the amorpha fruticosa white pulp obtained in the step (4) into a calcium hydroxide solution, performing microwave treatment, filtering, and drying to obtain the amorpha fruticosa cellulose.
2. The method for extracting cellulose from amorpha fruticosa planted in saline-alkali soil according to claim 1, which comprises the following steps: the mixed solution of the organic solvent, the organic acid and the surfactant is mixed solution of ethanol/isopropanol-tartaric acid-tween-60.
3. The method for extracting cellulose from amorpha fruticosa planted in saline-alkali soil according to claim 2, which comprises the following steps: the volume concentration of the ethanol is 65-80%.
4. The method for extracting cellulose from amorpha fruticosa planted in saline-alkali soil according to claim 1, which comprises the following steps: the temperature in the ultrasonic treatment in the step (3) is 80-120 ℃, the time is 1-4h, and the power of the ultrasonic wave is 200-400 w.
5. The method for extracting cellulose from amorpha fruticosa planted in saline-alkali soil according to claim 1, which comprises the following steps: and (4) the organic acid-bleaching agent mixed solution is a mixed solution of acetic acid-tetraacetylethylenediamine/sodium hypochlorite/sodium sulfite.
6. The method for extracting cellulose from amorpha fruticosa planted in saline-alkali soil according to claim 1, which comprises the following steps: in the step (4), the bleaching temperature is 60-100 ℃, and the bleaching time is 1-2 h.
7. The method for extracting cellulose from amorpha fruticosa planted in saline-alkali soil according to claim 1, which comprises the following steps: the power of the microwave treatment in the step (5) is 200-300w, and the temperature is 80-120 ℃.
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US5219601A (en) * | 1991-03-15 | 1993-06-15 | Elf Atochem S.A. | Two-step bleaching of plant materials |
CN102277760A (en) * | 2011-08-30 | 2011-12-14 | 内蒙古科技大学 | Pre-processing method in process of producing paper pulp |
CN103669064A (en) * | 2013-12-13 | 2014-03-26 | 四川永丰纸业股份有限公司 | Preparation process of acetified bamboo pulp |
CN104357931A (en) * | 2014-11-28 | 2015-02-18 | 赵兵 | Fluorescent salix mongolica regenerated cellulose fibers and preparation method thereof |
CN106368034A (en) * | 2016-11-14 | 2017-02-01 | 哈尔滨工业大学 | Method for extracting cellulose from traditional Chinese medicine dregs and application of cellulose |
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Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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US5219601A (en) * | 1991-03-15 | 1993-06-15 | Elf Atochem S.A. | Two-step bleaching of plant materials |
CN102277760A (en) * | 2011-08-30 | 2011-12-14 | 内蒙古科技大学 | Pre-processing method in process of producing paper pulp |
CN103669064A (en) * | 2013-12-13 | 2014-03-26 | 四川永丰纸业股份有限公司 | Preparation process of acetified bamboo pulp |
CN104357931A (en) * | 2014-11-28 | 2015-02-18 | 赵兵 | Fluorescent salix mongolica regenerated cellulose fibers and preparation method thereof |
CN106368034A (en) * | 2016-11-14 | 2017-02-01 | 哈尔滨工业大学 | Method for extracting cellulose from traditional Chinese medicine dregs and application of cellulose |
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