CN111455706B - Method for preparing dissolving pulp from waste cotton fabric, waste cotton yarn and other waste cotton materials - Google Patents
Method for preparing dissolving pulp from waste cotton fabric, waste cotton yarn and other waste cotton materials Download PDFInfo
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- CN111455706B CN111455706B CN202010329838.0A CN202010329838A CN111455706B CN 111455706 B CN111455706 B CN 111455706B CN 202010329838 A CN202010329838 A CN 202010329838A CN 111455706 B CN111455706 B CN 111455706B
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- 229920000742 Cotton Polymers 0.000 title claims abstract description 202
- 239000002699 waste material Substances 0.000 title claims abstract description 168
- 239000000463 material Substances 0.000 title claims abstract description 95
- 238000000034 method Methods 0.000 title claims abstract description 82
- 229920000875 Dissolving pulp Polymers 0.000 title claims abstract description 45
- 239000004744 fabric Substances 0.000 title claims abstract description 40
- 108090000790 Enzymes Proteins 0.000 claims abstract description 72
- 102000004190 Enzymes Human genes 0.000 claims abstract description 72
- 238000010411 cooking Methods 0.000 claims abstract description 67
- 230000008569 process Effects 0.000 claims abstract description 31
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 12
- 238000003801 milling Methods 0.000 claims abstract description 6
- 230000009257 reactivity Effects 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 69
- 229940088598 enzyme Drugs 0.000 claims description 69
- 239000004698 Polyethylene Substances 0.000 claims description 44
- 239000000203 mixture Substances 0.000 claims description 44
- -1 polyethylene Polymers 0.000 claims description 44
- 229920000573 polyethylene Polymers 0.000 claims description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 33
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 22
- 108010059892 Cellulase Proteins 0.000 claims description 20
- 229940106157 cellulase Drugs 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 20
- 239000003513 alkali Substances 0.000 claims description 12
- 229920000609 methyl cellulose Polymers 0.000 claims description 12
- 239000001923 methylcellulose Substances 0.000 claims description 12
- 235000010981 methylcellulose Nutrition 0.000 claims description 12
- 239000012752 auxiliary agent Substances 0.000 claims description 6
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 claims description 5
- 150000004056 anthraquinones Chemical group 0.000 claims description 5
- 238000005470 impregnation Methods 0.000 claims description 5
- 108010059820 Polygalacturonase Proteins 0.000 claims description 2
- 108010093305 exopolygalacturonase Proteins 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 23
- 239000000835 fiber Substances 0.000 abstract description 21
- 238000002791 soaking Methods 0.000 abstract description 14
- 238000010025 steaming Methods 0.000 abstract description 3
- 239000003814 drug Substances 0.000 abstract description 2
- 239000002002 slurry Substances 0.000 description 28
- 238000001914 filtration Methods 0.000 description 10
- 241000196324 Embryophyta Species 0.000 description 6
- 210000004027 cell Anatomy 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 229920002678 cellulose Polymers 0.000 description 5
- 239000001913 cellulose Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- YTWHNPHXSILERV-UHFFFAOYSA-N 1,2-dihydroanthracene-9,10-dione Chemical compound O=C1C2=CC=CC=C2C(=O)C2=C1C=CCC2 YTWHNPHXSILERV-UHFFFAOYSA-N 0.000 description 4
- GCDBEYOJCZLKMC-UHFFFAOYSA-N 2-hydroxyanthraquinone Chemical compound C1=CC=C2C(=O)C3=CC(O)=CC=C3C(=O)C2=C1 GCDBEYOJCZLKMC-UHFFFAOYSA-N 0.000 description 4
- NJWGQARXZDRHCD-UHFFFAOYSA-N 2-methylanthraquinone Chemical compound C1=CC=C2C(=O)C3=CC(C)=CC=C3C(=O)C2=C1 NJWGQARXZDRHCD-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 210000002421 cell wall Anatomy 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 238000004898 kneading Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000004537 pulping Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- OTBHDFWQZHPNPU-UHFFFAOYSA-N 1,2,3,4-tetrahydroanthracene-9,10-dione Chemical compound O=C1C2=CC=CC=C2C(=O)C2=C1CCCC2 OTBHDFWQZHPNPU-UHFFFAOYSA-N 0.000 description 2
- QCVMOSGPTRRUQZ-UHFFFAOYSA-N 2-nitroanthracene-9,10-dione Chemical compound C1=CC=C2C(=O)C3=CC([N+](=O)[O-])=CC=C3C(=O)C2=C1 QCVMOSGPTRRUQZ-UHFFFAOYSA-N 0.000 description 2
- PCFMUWBCZZUMRX-UHFFFAOYSA-N 9,10-Dihydroxyanthracene Chemical compound C1=CC=C2C(O)=C(C=CC=C3)C3=C(O)C2=C1 PCFMUWBCZZUMRX-UHFFFAOYSA-N 0.000 description 2
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 229920001277 pectin Polymers 0.000 description 2
- 239000001814 pectin Substances 0.000 description 2
- 235000010987 pectin Nutrition 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- GGCZERPQGJTIQP-UHFFFAOYSA-M sodium 2-anthraquinonesulfonate Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)[O-])=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-M 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241001330002 Bambuseae Species 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
Classifications
-
- 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
- D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
- D21C5/005—Treatment of cellulose-containing material with microorganisms or enzymes
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21B—FIBROUS RAW MATERIALS OR THEIR MECHANICAL TREATMENT
- D21B1/00—Fibrous raw materials or their mechanical treatment
- D21B1/04—Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres
- D21B1/06—Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres by dry methods
- D21B1/063—Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres by dry methods using grinding devices
-
- 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
- D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Microbiology (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Paper (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention relates to a method for preparing dissolving pulp from waste cotton fabrics, waste cotton yarns and other waste cotton materials, which comprises the following process flows: enzyme treatment → preimpregnation → cooking, wherein the cotton fiber content of the waste cotton material (waste cotton yarn, waste denim or waste cotton cloth) is more than 75wt%, when the waste cotton material is a fabric, a high-concentration disc mill is used for disc milling before the enzyme treatment, the alpha fiber content of pulp obtained by washing and spin-drying pulp after cooking is 90-95 wt%, the reactivity is 50-120 s, and the polymerization degree is 400-550. According to the method for preparing the dissolving pulp from the waste cotton fabrics, the waste cotton yarns and other waste cotton materials, the enzyme treatment is carried out before the pre-soaking and the steaming, so that the reaction performance and the alpha fiber content of the dissolving pulp can be improved, the operation is simple, the medicine dosage of the pre-soaking and steaming process is saved, and the method is suitable for popularization and application.
Description
Technical Field
The invention belongs to the technical field of waste recovery engineering, and relates to a method for preparing dissolving pulp from waste cotton fabrics, waste cotton yarns and other waste cotton materials.
Background
Due to the popularization of the fast fashion concept and the increase of the consumption level, a large amount of waste cotton materials are generated all over the world every year. Most of the waste cotton materials are buried or burned, the utilization value is low, and a large amount of pollution is generated. In addition, the research on the utilization modes of the waste cotton materials at home and abroad is very wide, such as the regeneration of cotton yarns from the waste cotton materials, the manufacture of non-woven products, carbon materials, cellulose derivative materials and the like, and although the utilization modes have higher utilization value, most of the utilization modes are difficult to treat the waste cotton materials in a large scale or in an industrialized mode and have the characteristic of low utilization rate.
The dissolving pulp prepared from the waste cotton material is a novel efficient high-value utilization mode, and the reaction performance and the content of alpha fibers are important parameters for measuring the pulp performance in the pulping process of the waste cotton material. Reactivity refers to the ability of the cellulose molecules in the dissolving pulp to react with other substances (carbon disulphide in the viscose production process). The alpha-cellulose content is the alpha-cellulose content in the pulp, the alpha-cellulose content determines the quality of the pulp, the stability of the cellulose on the action of alkali in the production process can be basically reflected, and the alpha-cellulose content of high-quality dissolving pulp is generally more than 93 wt%.
At present, there are two main methods for improving the reaction performance: pulping and enzyme treatment, wherein the enzyme treatment process is simple in treatment and has a good reaction performance improvement effect. The patent application (CN201610997546.8) discloses a biological enzyme pretreatment method for bamboo chemical mechanical pulp, which researches the influence of the biological enzyme pretreatment on the pulp forming performance; patent application (CN201710859395.4) discloses a method for treating pulp with complex enzyme liquid. In the process flow of the enzyme treatment, the waste cotton material is generally subjected to pre-soaking and cooking treatment after pre-treatment, and then subjected to the enzyme treatment, or the enzyme treatment process and the pulping process are combined, so that the aim of improving the reaction performance is fulfilled, the enzyme treatment can not be directly carried out on the fabric generally, because the fibers of the waste cotton material are interwoven and combined tightly, if the waste cotton material is directly used for the enzyme treatment, the reaction performance of the cotton fiber in the cotton fabric can be improved unevenly due to uneven enzyme contact, the improvement effect is not good, and although the enzyme treatment can improve the reaction performance to a certain extent, the content of the methyl cellulose cannot be improved simultaneously.
Therefore, it is very important to research a method for preparing dissolving pulp by using waste cotton materials, which can improve the reaction performance and the content of alpha fibers.
Disclosure of Invention
The invention provides a method for preparing dissolving pulp from waste cotton fabrics, waste cotton yarns and other waste cotton materials, and aims to solve the problem that the reaction performance and the content of alpha fibers cannot be simultaneously improved when the dissolving pulp is prepared from the waste cotton materials in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing dissolving pulp from waste cotton fabrics, waste cotton yarns and other waste cotton materials comprises the following process flows: enzyme treatment → preimpregnation → cooking; when the waste cotton material is a fabric, a high-concentration disc mill is also used for disc milling before enzyme treatment.
The principle of the invention is as follows:
the invention adopts the process flow of enzyme treatment → preimpregnation → cooking, and when the waste cotton material is a fabric, a high-concentration disc grinder disc grinding process is added before the enzyme treatment process; the high-concentration disc mill can change the interwoven cotton fabric into independent fibers by disc milling, so that the phenomenon that the cotton fibers in the cotton fabric contact enzyme is not uniform due to tight combination because the fibers of waste cotton materials are interwoven with each other during subsequent enzyme treatment is avoided, the reaction performance is improved non-uniformly, and the improvement effect is poor; the enzyme treatment is a process of fully damaging the primary wall and the secondary wall of the plant cell of the cotton fiber by using the action of enzyme; the pre-impregnation can ensure that the alkali liquor is fully and uniformly contacted with the waste cotton material, thereby being beneficial to improving the subsequent cooking uniformity and improving the uniformity of polymerization degree and performance of the pulp; the digestion is a process of removing non-methyl fiber substances in the slurry by fully contacting alkali liquor and waste cotton material waste under high temperature and high pressure.
The plant cell primary wall contains fiber, pectin, hemicellulose and other impurities, the content of alpha fiber is low due to the impurities, the pre-soaking and cooking processes are the processes of removing the impurities and improving the content of the alpha fiber, the prior art usually carries out enzyme treatment after the cooking is finished, when the method is used for pre-soaking and cooking, the plant cell primary wall is not damaged by enzyme, the contact reaction of pulp and alkali liquor can be prevented, the impurities are not favorably removed, and therefore the content of the alpha fiber cannot be effectively improved. The invention changes the interlaced cotton fabrics into independent fibers by carrying out high-concentration disc mill disc grinding on the waste cotton materials in the fabric form, so that the enzyme treatment can be carried out before the preimpregnation, the enzyme treatment can destroy the primary wall of plant cells, the pulp can be fully contacted with alkali liquor in the preimpregnation and cooking processes, the impurities are effectively removed, the content of alpha fibers is improved, and in addition, the enzyme treatment process can also remove the impurities except the non-fibers, and the content of the alpha fibers is further improved.
As a preferred technical scheme:
the method for preparing the dissolving pulp from the waste cotton materials such as the waste cotton fabrics and the waste cotton yarns has the advantage that the cotton fiber content of the waste cotton materials is more than 75 wt%.
The method for preparing the dissolving pulp from the waste cotton fabrics, the waste cotton yarns and other waste cotton materials is characterized in that the waste cotton materials are the waste cotton yarns, the waste jean or the waste cotton fabrics.
According to the method for preparing the dissolving pulp from the waste cotton materials such as the waste cotton fabrics and the waste cotton yarns, before the enzyme treatment, the waste cotton materials are mechanically chopped, so that the length of cotton fibers in the waste cotton materials is 4-5 cm. The purpose of mechanical chopping is to ensure that enzyme liquid is fully contacted with cotton fibers, if mechanical chopping is not carried out, the cotton yarn is about ten centimeters to twenty centimeters in length and is wound into a cluster, and the cluster of cotton yarn cannot be contacted with the enzyme liquid in the early stage of an enzyme treatment process and can be gradually and uniformly contacted with the enzyme liquid along with the time.
The method for preparing the dissolving pulp from the waste cotton materials such as the waste cotton fabrics and the waste cotton yarns comprises the following steps of: firstly, mixing waste cotton materials, an enzyme solution, a sulfuric acid solution and water in a polyethylene bag to obtain a mixture with a pH value of 4.5-6.5, wherein the activity of the enzyme is influenced by the pH value, and the enzyme can better play a role only when the activity of the enzyme is stronger under a proper pH value; and then placing the polyethylene bag at the temperature of 40-65 ℃ for 30-90 min, kneading the polyethylene bag every 5-15 min, placing the polyethylene bag at the temperature of 90-100 ℃ for 30-50 min, and finally filtering, washing and drying the mixture to obtain the cotton yarn after enzyme treatment.
According to the method for preparing the dissolving pulp from the waste cotton materials such as the waste cotton fabrics and the waste cotton yarns, the using amount of the enzyme in the mixture is 5-30U/g, and the content of the waste cotton materials in the mixture is 5 wt%.
In the method for preparing dissolving pulp from waste cotton fabrics, waste cotton yarns and other waste cotton materials, the enzyme treatment is to destroy the cell walls of plant cells, and the main components of the cell walls are cellulose and pectin, so the enzyme treatment adopts cellulase and/or pectinase.
According to the method for preparing the dissolving pulp from the waste cotton materials such as the waste cotton fabrics and the waste cotton yarns, the cotton yarns subjected to enzyme treatment are mixed with water, alkali and an auxiliary agent, and then are pre-impregnated and cooked, wherein the pre-impregnation temperature is 70-110 ℃, the time is 10-30 min, the cooking temperature is 150-180 ℃, and the time is 1-3 h.
According to the method for preparing the dissolving pulp from the waste cotton fabrics, the waste cotton yarns and other waste cotton materials, the mass ratio of the cotton yarns subjected to enzyme treatment to water, alkali and an auxiliary agent is 80-100: 16-25: 20-25: 0.01-0.05, the alkali is sodium hydroxide, and the auxiliary agent is anthraquinone and derivatives thereof. Alkali (sodium hydroxide) can dissolve non-alpha fiber substances, fully destroy cell walls of plant cells, and improve the content and the reactivity of alpha fiber. The existence of anthraquinone can protect cellulose, reduce annular peeling of cotton fiber in the cooking process, and reduce the reduction of pulp viscosity and yield.
According to the method for preparing the dissolving pulp from the waste cotton materials such as the waste cotton fabrics and the waste cotton yarns, after cooking, the pulp is washed and dried to obtain the pulp, the methyl cellulose content is 90-95 wt%, the reaction performance is 50-120 s, and the polymerization degree is 400-550. Wherein, the testing method of the content of the alpha-fiber adopts FZ/T50010.4; the method for testing the reaction performance adopts FZ/T50010.13.
Has the advantages that:
(1) according to the method for preparing the dissolving pulp from the waste cotton fabrics, the waste cotton yarns and other waste cotton materials, the enzyme treatment is carried out before the pre-impregnation and the cooking, so that the reaction performance and the alpha fiber content of the dissolving pulp can be effectively improved;
(2) the method for preparing the dissolving pulp from the waste cotton fabrics, the waste cotton yarns and other waste cotton materials is simple to operate, saves the medicine dosage of the pre-soaking and steaming process, and is suitable for popularization and use.
Detailed Description
The invention will be further illustrated with reference to specific embodiments. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
A method for preparing dissolving pulp from waste cotton fabrics, waste cotton yarns and other waste cotton materials comprises the following process flows: enzyme treatment → preimpregnation → cooking; the method specifically comprises the following steps:
(1) mechanically chopping waste cotton materials (waste cotton yarns with the cotton fiber content of 100 wt%) to enable the length of cotton fibers to be 4-5 cm;
(2) carrying out enzyme treatment, comprising the following steps:
(2.1) mixing the waste cotton material, cellulase solution, sulfuric acid solution (2mol/L) and water in a polyethylene bag to obtain a mixture with the pH value of 5.2; wherein the dosage of the cellulase in the mixture is 8U/g, and the content of the waste cotton material in the mixture is 5 wt%;
(2.2) placing the polyethylene bag at the temperature of 50 ℃ for 60min, and rubbing the polyethylene bag once every 8 min;
(2.3) placing the polyethylene bag at the temperature of 95 ℃ for 45 min;
(2.4) filtering, washing and drying the mixture to obtain slurry;
(3) mixing the slurry obtained in the step (2.4) with water, sodium hydroxide and anthraquinone, and then pre-impregnating and cooking, wherein the pre-impregnating temperature is 80 ℃, the time is 25min, and the cooking temperature is 150 ℃, and the time is 3 h; wherein the mass ratio of the slurry, the water, the sodium hydroxide and the anthraquinone is 90:18:20: 0.03;
(4) after cooking, pulp is cleaned and dried to obtain the pulp with the methyl cellulose content of 94 wt%, the reaction performance of 66s and the polymerization degree of 450.
Example 2
A method for preparing dissolving pulp from waste cotton fabrics, waste cotton yarns and other waste cotton materials comprises the following process flows: high-concentration disc mill disc milling → enzyme treatment → preimpregnation → cooking; the method specifically comprises the following steps:
(1) mechanically cutting waste cotton material (waste jean with cotton fiber content of 100 wt%) into 2 × 2cm2Soaking the small denim blocks in 6.25 wt% sodium hydroxide solution for 3 hours, cleaning the small denim blocks, carrying out disc grinding on a high-concentration disc grinder twice, wherein the disc distance is 0.25mm and 0.2mm respectively, and measuring the solid content after spin-drying moisture of the disc-ground cotton fibers;
(2) carrying out enzyme treatment, comprising the following steps:
(2.1) mixing the waste cotton material, cellulase solution, sulfuric acid solution (2mol/L) and water in a polyethylene bag to obtain a mixture with the pH value of 4.5; wherein the dosage of the cellulase in the mixture is 6U/g, and the content of the waste cotton material in the mixture is 5 wt%;
(2.2) placing the polyethylene bag at the temperature of 40 ℃ for 90min, and rubbing the polyethylene bag once every 5 min;
(2.3) placing the polyethylene bag at the temperature of 90 ℃ for 50 min;
(2.4) filtering, washing and drying the mixture to obtain slurry;
(3) mixing the slurry obtained in the step (2.4) with water, sodium hydroxide and 2-methylanthraquinone, and then pre-soaking and cooking, wherein the pre-soaking temperature is 85 ℃ and the cooking temperature is 155 ℃ and the cooking time is 2.5 hours; wherein the mass ratio of the slurry, the water, the sodium hydroxide and the 2-methylanthraquinone is 80:16:22: 0.01;
(4) after cooking, pulp is cleaned and dried to obtain the pulp with the methyl cellulose content of 92 wt%, the reaction performance of 57s and the polymerization degree of 420.
Example 3
A method for preparing dissolving pulp from waste cotton fabrics, waste cotton yarns and other waste cotton materials comprises the following process flows: high-concentration disc mill disc milling → enzyme treatment → preimpregnation → cooking; the method specifically comprises the following steps:
(1) mechanically cutting waste cotton material (waste jean with cotton fiber content of 100 wt%) into 2 × 2cm2Soaking the small denim blocks in 6.25 wt% sodium hydroxide solution for 3 hours, cleaning the small denim blocks, carrying out disc grinding on a high-concentration disc grinder twice, wherein the disc distance is 0.25mm and 0.2mm respectively, and measuring the solid content after spin-drying moisture of the disc-ground cotton fibers;
(2) carrying out enzyme treatment, comprising the following steps:
(2.1) mixing the waste cotton material, cellulase solution, sulfuric acid solution (2mol/L) and water in a polyethylene bag to obtain a mixture with the pH value of 5.5; wherein the dosage of the cellulase in the mixture is 10U/g, and the content of the waste cotton material in the mixture is 5 wt%;
(2.2) placing the polyethylene bag at the temperature of 45 ℃ for 80min, and rubbing the polyethylene bag once every 6 min;
(2.3) placing the polyethylene bag at the temperature of 95 ℃ for 40 min;
(2.4) filtering, washing and drying the mixture to obtain slurry;
(3) mixing the slurry obtained in the step (2.4) with water, sodium hydroxide and anthrahydroquinone, and then pre-impregnating and cooking, wherein the pre-impregnating temperature is 70 ℃ and the cooking time is 30min and the cooking temperature is 150 ℃ and the cooking time is 3 h; wherein the mass ratio of the slurry, the water, the sodium hydroxide and the anthrahydroquinone is 100:20:25: 0.05;
(4) after cooking, pulp is cleaned and dried to obtain the pulp with the methyl cellulose content of 90wt%, the reaction performance of 50s and the polymerization degree of 400.
Example 4
A method for preparing dissolving pulp from waste cotton fabrics, waste cotton yarns and other waste cotton materials comprises the following process flows: enzyme treatment → preimpregnation → cooking; the method specifically comprises the following steps:
(1) mechanically chopping waste cotton materials (waste cotton yarns with the cotton fiber content of 100 wt%) to enable the length of cotton fibers to be 4-5 cm;
(2) carrying out enzyme treatment, comprising the following steps:
(2.1) mixing the waste cotton material, cellulase solution, sulfuric acid solution (2mol/L) and water in a polyethylene bag to obtain a mixture with the pH value of 6.2; wherein the dosage of the cellulase in the mixture is 5U/g, and the content of the waste cotton material in the mixture is 5 wt%;
(2.2) placing the polyethylene bag at the temperature of 55 ℃ for 40min, and rubbing the polyethylene bag once every 10 min;
(2.3) placing the polyethylene bag at the temperature of 98 ℃ for 45 min;
(2.4) filtering, washing and drying the mixture to obtain slurry;
(3) mixing the slurry obtained in the step (2.4) with water, sodium hydroxide and dihydroanthraquinone, and then pre-impregnating and cooking, wherein the pre-impregnating temperature is 90 ℃ and the cooking time is 20min, and the cooking temperature is 160 ℃ and the cooking time is 2 h; wherein the mass ratio of the slurry, the water, the sodium hydroxide and the dihydroanthraquinone is 85:25:20: 0.03;
(4) after cooking, pulp is cleaned and dried to obtain the pulp with the methyl cellulose content of 94 wt%, the reaction performance of 106s and the polymerization degree of 520.
Example 5
A method for preparing dissolving pulp from waste cotton fabrics, waste cotton yarns and other waste cotton materials comprises the following process flows: enzyme treatment → preimpregnation → cooking; the method specifically comprises the following steps:
(1) mechanically chopping waste cotton materials (waste cotton yarns with the cotton fiber content of 100 wt%) to enable the length of cotton fibers to be 4-5 cm;
(2) carrying out enzyme treatment, comprising the following steps:
(2.1) mixing the waste cotton material, cellulase solution, sulfuric acid solution (2mol/L) and water in a polyethylene bag to obtain a mixture with the pH value of 5.5; wherein the dosage of the cellulase in the mixture is 15U/g, and the content of the waste cotton material in the mixture is 5 wt%;
(2.2) placing the polyethylene bag at the temperature of 60 ℃ for 50min, and rubbing the polyethylene bag once every 12 min;
(2.3) placing the polyethylene bag at the temperature of 92 ℃ for 35 min;
(2.4) filtering, washing and drying the mixture to obtain slurry;
(3) mixing the slurry obtained in the step (2.4) with water, sodium hydroxide and dihydroanthraquinone, and then pre-impregnating and cooking, wherein the pre-impregnating temperature is 100 ℃, the time is 15min, and the cooking temperature is 170 ℃, and the time is 1.5 h; wherein the mass ratio of the slurry, the water, the sodium hydroxide and the dihydroanthraquinone is 95:23:25: 0.04;
(4) after cooking, pulp is cleaned and dried to obtain the pulp with the methyl cellulose content of 94 wt%, the reaction performance of 98s and the polymerization degree of 510.
Example 6
A method for preparing dissolving pulp from waste cotton fabrics, waste cotton yarns and other waste cotton materials comprises the following process flows: enzyme treatment → preimpregnation → cooking; the method specifically comprises the following steps:
(1) mechanically chopping waste cotton materials (waste cotton yarns with the cotton fiber content of 100 wt%) to enable the length of cotton fibers to be 4-5 cm;
(2) carrying out enzyme treatment, comprising the following steps:
(2.1) mixing the waste cotton material, cellulase solution, sulfuric acid solution (2mol/L) and water in a polyethylene bag to obtain a mixture with the pH value of 6.4; wherein the dosage of the cellulase in the mixture is 20U/g, and the content of the waste cotton material in the mixture is 5 wt%;
(2.2) placing the polyethylene bag at 50 ℃ for 40min, and kneading the polyethylene bag every 15 min;
(2.3) placing the polyethylene bag at the temperature of 100 ℃ for 30 min;
(2.4) filtering, washing and drying the mixture to obtain slurry;
(3) mixing the slurry obtained in the step (2.4) with water, sodium hydroxide and tetrahydroanthraquinone, and then pre-soaking and cooking, wherein the pre-soaking temperature is 110 ℃ and the cooking time is 10min, and the cooking temperature is 180 ℃ and the cooking time is 1 h; wherein the mass ratio of the slurry, the water, the sodium hydroxide and the tetrahydroanthraquinone is 90:25:25: 0.02;
(4) after cooking, pulp is cleaned and dried to obtain the pulp with the methyl cellulose content of 94 wt%, the reaction performance of 120s and the polymerization degree of 550.
Example 7
A method for preparing dissolving pulp from waste cotton fabrics, waste cotton yarns and other waste cotton materials comprises the following process flows: enzyme treatment → preimpregnation → cooking; the method specifically comprises the following steps:
(1) mechanically chopping waste cotton materials (waste cotton yarns with the cotton fiber content of 100 wt%) to enable the length of cotton fibers to be 4-5 cm;
(2) carrying out enzyme treatment, comprising the following steps:
(2.1) mixing the waste cotton material, cellulase solution, sulfuric acid solution (2mol/L) and water in a polyethylene bag to obtain a mixture with the pH value of 5.4; wherein the dosage of the cellulase in the mixture is 25U/g, and the content of the waste cotton material in the mixture is 5 wt%;
(2.2) placing the polyethylene bag at 55 ℃ for 70min, and kneading the polyethylene bag every 10 min;
(2.3) placing the polyethylene bag at the temperature of 95 ℃ for 35 min;
(2.4) filtering, washing and drying the mixture to obtain slurry;
(3) mixing the slurry obtained in the step (2.4) with water, sodium hydroxide and 2-hydroxyanthraquinone, and then pre-soaking and cooking, wherein the pre-soaking temperature is 95 ℃ and the cooking time is 20min, and the cooking temperature is 165 ℃ and the cooking time is 2 h; wherein the mass ratio of the slurry, the water, the sodium hydroxide and the 2-hydroxyanthraquinone is 80:20:20: 0.01;
(4) after cooking, pulp is cleaned and dried to obtain the pulp with the methyl cellulose content of 95wt%, the reaction performance of 87s and the polymerization degree of 500.
Example 8
A method for preparing dissolving pulp from waste cotton fabrics, waste cotton yarns and other waste cotton materials comprises the following process flows: enzyme treatment → preimpregnation → cooking; the method specifically comprises the following steps:
(1) mechanically chopping waste cotton materials (waste cotton yarns with the cotton fiber content of 100 wt%) to enable the length of cotton fibers to be 4-5 cm;
(2) carrying out enzyme treatment, comprising the following steps:
(2.1) mixing the waste cotton material, cellulase solution, sulfuric acid solution (2mol/L) and water in a polyethylene bag to obtain a mixture with the pH value of 6.5; wherein the dosage of the cellulase in the mixture is 30U/g, and the content of the waste cotton material in the mixture is 5 wt%;
(2.2) placing the polyethylene bag at the temperature of 65 ℃ for 30min, and rubbing the polyethylene bag once every 8 min;
(2.3) placing the polyethylene bag at the temperature of 98 ℃ for 30 min;
(2.4) filtering, washing and drying the mixture to obtain slurry;
(3) mixing the slurry obtained in the step (2.4) with water, sodium hydroxide and 2-anthraquinone sodium sulfonate, and then pre-impregnating and cooking, wherein the pre-impregnating temperature is 90 ℃ and the cooking time is 25min, and the cooking temperature is 155 ℃ and the cooking time is 1.5 h; wherein the mass ratio of the slurry, the water, the sodium hydroxide and the 2-anthraquinone sodium sulfonate is 95:22:24: 0.04;
(4) after cooking, pulp is cleaned and dried to obtain the pulp with the methyl cellulose content of 94 wt%, the reaction performance of 96s and the polymerization degree of 510.
Example 9
A method for preparing dissolving pulp from waste cotton fabrics, waste cotton yarns and other waste cotton materials comprises the following process flows: enzyme treatment → preimpregnation → cooking; the method specifically comprises the following steps:
(1) mechanically chopping waste cotton materials (waste cotton yarns with the cotton fiber content of 100 wt%) to enable the length of cotton fibers to be 4-5 cm;
(2) carrying out enzyme treatment, comprising the following steps:
(2.1) mixing the waste cotton material, cellulase solution, sulfuric acid solution (2mol/L) and water in a polyethylene bag to obtain a mixture with the pH value of 6.5; wherein the dosage of the cellulase in the mixture is 30U/g, and the content of the waste cotton material in the mixture is 5 wt%;
(2.2) placing the polyethylene bag at the temperature of 65 ℃ for 30min, and rubbing the polyethylene bag once every 8 min;
(2.3) placing the polyethylene bag at the temperature of 98 ℃ for 30 min;
(2.4) filtering, washing and drying the mixture to obtain slurry;
(3) mixing the slurry obtained in the step (2.4) with water, sodium hydroxide and 2-nitroanthraquinone, and then pre-impregnating and cooking, wherein the pre-impregnating temperature is 90 ℃ and the cooking time is 25min, and the cooking temperature is 155 ℃ and the cooking time is 1.5 h; wherein the mass ratio of the slurry, the water, the sodium hydroxide and the 2-nitroanthraquinone is 95:22:24: 0.04;
(4) after cooking, pulp is cleaned and dried to obtain the pulp with the methyl cellulose content of 94 wt%, the reaction performance of 93s and the polymerization degree of 490.
Claims (9)
1. A method for preparing dissolving pulp by waste cotton materials is characterized by comprising the following process flows: enzyme treatment → preimpregnation → cooking; when the waste cotton material is a fabric, a high-concentration disc mill is also used for disc milling before enzyme treatment; the enzyme treatment process comprises the following steps: firstly, waste cotton materials, an enzyme solution, a sulfuric acid solution and water are mixed in a polyethylene bag to obtain a mixture with the pH value of 4.5-6.5, then the polyethylene bag is placed at the temperature of 40-65 ℃ for 30-90 min, the polyethylene bag is kneaded every 5-15 min, then the polyethylene bag is placed at the temperature of 90-100 ℃ for 30-50 min, and finally the mixture is filtered, washed and dried to obtain cotton yarns after enzyme treatment.
2. The method of claim 1, wherein the cotton fiber content of the waste cotton material is more than 75 wt%.
3. The method for preparing dissolving pulp from waste cotton materials according to claim 2, wherein the waste cotton materials are waste cotton yarns, waste jeans or waste cotton cloth.
4. The method for preparing dissolving pulp from waste cotton materials according to claim 1, wherein the waste cotton materials are mechanically chopped to make the length of cotton fiber be 4-5 cm before enzyme treatment.
5. The method for preparing dissolving pulp from waste cotton materials according to claim 1, wherein the amount of the enzyme in the mixture is 5-30U/g, and the content of the waste cotton materials in the mixture is 5 wt%.
6. The method for preparing dissolving pulp from waste cotton materials according to claim 1, characterized in that the enzyme treatment uses cellulase and/or pectinase.
7. The method for preparing dissolving pulp from waste cotton materials according to claim 1, wherein the dissolving pulp is prepared by mixing cotton yarns subjected to enzyme treatment with water, alkali and an auxiliary agent, and then performing pre-impregnation and cooking, wherein the pre-impregnation temperature is 70-110 ℃, the time is 10-30 min, and the cooking temperature is 150-180 ℃, and the time is 1-3 h.
8. The method for preparing dissolving pulp from waste cotton materials according to claim 7, wherein the mass ratio of the cotton yarn after enzyme treatment, water, alkali and an auxiliary agent is 80-100: 16-25: 20-25: 0.01-0.05, the alkali is sodium hydroxide, and the auxiliary agent is anthraquinone and derivatives thereof.
9. The method for preparing dissolving pulp from waste cotton materials as claimed in claim 8, wherein the dissolving pulp obtained by washing and spin-drying the dissolving pulp after cooking has a methyl cellulose content of 90-95 wt%, a reactivity of 50-120 s and a polymerization degree of 400-550.
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| CN112608513B (en) * | 2020-11-20 | 2022-09-02 | 湖北金环绿色纤维有限公司 | Method for preparing cellulose dissolving pulp from waste polyester-cotton blended fabric and product |
| CN112620298B (en) * | 2020-11-20 | 2022-04-15 | 湖北金环绿色纤维有限公司 | Preparation method of waterproof cellulose membrane |
| CN115125751A (en) * | 2022-06-01 | 2022-09-30 | 齐鲁工业大学 | A clean and efficient method for preparing cotton pulp from waste cotton textiles |
| CN115637603B (en) * | 2022-11-14 | 2023-06-02 | 山东银鹰股份有限公司 | Method for preparing pulp from waste pure cotton fabric, product obtained by method and application of pulp |
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