CN114990917A - Cooking method for preparing moso bamboo lyocell fiber grade dissolving pulp - Google Patents
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- 238000010411 cooking Methods 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 41
- 229920000875 Dissolving pulp Polymers 0.000 title claims abstract description 27
- 244000302661 Phyllostachys pubescens Species 0.000 title claims abstract description 25
- 235000003570 Phyllostachys pubescens Nutrition 0.000 title claims abstract description 25
- 229920000433 Lyocell Polymers 0.000 title claims abstract description 22
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims abstract description 89
- 239000007788 liquid Substances 0.000 claims abstract description 37
- 239000000203 mixture Substances 0.000 claims abstract description 28
- 239000002904 solvent Substances 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 238000005406 washing Methods 0.000 claims abstract description 22
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims abstract description 21
- 235000017491 Bambusa tulda Nutrition 0.000 claims abstract description 21
- 241001330002 Bambuseae Species 0.000 claims abstract description 21
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims abstract description 21
- 239000011425 bamboo Substances 0.000 claims abstract description 20
- 239000002002 slurry Substances 0.000 claims abstract description 18
- 239000000835 fiber Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000005549 size reduction Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 15
- 239000002028 Biomass Substances 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 238000004537 pulping Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000000428 dust Substances 0.000 claims description 2
- 229920005610 lignin Polymers 0.000 abstract description 19
- 229920002488 Hemicellulose Polymers 0.000 abstract description 11
- 238000005265 energy consumption Methods 0.000 abstract description 8
- 239000000126 substance Substances 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 2
- 238000009835 boiling Methods 0.000 abstract 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 229920001131 Pulp (paper) Polymers 0.000 description 6
- 238000006116 polymerization reaction Methods 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 238000007605 air drying Methods 0.000 description 4
- 229920002678 cellulose Polymers 0.000 description 4
- 239000001913 cellulose Substances 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 4
- 238000003760 magnetic stirring Methods 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 239000010802 sludge Substances 0.000 description 4
- 239000002023 wood Substances 0.000 description 4
- 238000004061 bleaching Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 239000005708 Sodium hypochlorite Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000029087 digestion Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical compound [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 description 2
- 229960002218 sodium chlorite Drugs 0.000 description 2
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 description 1
- 241000209128 Bambusa Species 0.000 description 1
- 235000019743 Choline chloride Nutrition 0.000 description 1
- 241000219000 Populus Species 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000013475 authorization Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 description 1
- 229960003178 choline chloride Drugs 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
Classifications
-
- 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
- D21B1/02—Pretreatment of the raw materials by chemical or physical means
- D21B1/023—Cleaning wood chips or other raw materials
-
- 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
- D21C3/003—Pulping cellulose-containing materials with organic compounds
-
- 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
- D21C3/22—Other features of pulping processes
-
- 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
-
- 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
- D21C9/02—Washing ; Displacing cooking or pulp-treating liquors contained in the pulp by fluids, e.g. wash water or other pulp-treating agents
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
- D21H11/12—Pulp from non-woody plants or crops, e.g. cotton, flax, straw, bagasse
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/64—Paper recycling
Landscapes
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Mechanical Engineering (AREA)
- Paper (AREA)
Abstract
The invention discloses a cooking method for preparing moso bamboo lyocell fiber grade dissolving pulp, which comprises the following steps: performing size reduction treatment on the moso bamboo; mixing the raw materials with a p-toluenesulfonic acid solvent for a boiling reaction; after the cooking is finished, adding a washing liquid to dilute the mixture and then carrying out solid-liquid separation to obtain slurry, and carrying out ultrasonic treatment to ensure that the slurry has better performance. The key point of the invention is that in the cooking process stage, the excellent lignin and hemicellulose removing effect of the p-toluenesulfonic acid is utilized, the effective separation of the fibers under the conditions of mild reaction conditions, short time consumption, environmental protection and low energy consumption is realized, the high temperature, high pressure, high energy consumption and high chemical consumption required by the cooking of the bamboo raw material are obviously reduced, and the requirement on reaction equipment is reduced; in addition, in the method, the p-toluenesulfonic acid solvent and the washing liquid can be recycled, so that the burden of subsequent pollution treatment is reduced; therefore, the method has economic and environmental feasibility.
Description
Technical Field
The invention relates to a cooking method for preparing moso bamboo lyocell fiber grade dissolving pulp.
Background
With the rapid development of national socioeconomic, the demand of paper pulp is steadily increasing, and the paper pulp is usually obtained from wood through a pulping process. Although China is a country with low forest coverage, bamboo resources are quite rich, the varieties, areas and yields of bamboos are the top of the world, and moso bamboos are the most important bamboo species for long-term cultivation, the widest areas and the most important economic values in China.
The dissolving pulp is widely applied to the aspects of textile, food, rubber and the like at present, the preparation method of the traditional dissolving pulp is an acid sulfite method or a prehydrolysis sulfate method, the cooking temperature in the process of preparing the dissolving pulp by the prehydrolysis sulfate method is 160-180 ℃, the pressure is 800kPa, the pretreatment time is about 1-2h, and the total pulping time is about 5-6 h. The cooking temperature in the process of producing dissolving pulp by the acid sulfite method is 130-145 ℃, the cooking time is about 7 hours, and the total time is about 10-11 hours. For example, in the cooking process adopted in the Chinese patent authorization text CN111618961B, the temperature is firstly increased to 90-120 ℃ within 30-60min, the temperature is kept for 30-60min, the temperature is continuously increased to 165 ℃ of 155-. Chinese patent publication CN108660837A adopts choline chloride and lactic acid eutectic solvent to cook poplar chips under normal pressure condition, and pulp with alpha-cellulose content of 83.5% can be obtained, but the treatment temperature of the technology is as high as 150 ℃, and the treatment time is as long as 10 hours; the harsh conditions result in high energy consumption and great damage to the fibers, resulting in limited industrialization thereof. Therefore, the development of a low-energy-consumption green and environment-friendly dissolving pulp preparation method is a necessary way for the sustainable development of the pulping and papermaking industry.
The bamboo is not widely used due to the characteristics of thick cell wall, more impurity cells, high hardness, difficult penetration of liquid medicine and the like, and higher pressure reaction conditions are required. But in the p-toluenesulfonic acid cooking process, lignin and hemicellulose of bamboo wood can be efficiently removed, and the reaction condition is mild, the energy consumption is low, the time consumption is short, and the method is green and environment-friendly.
The p-toluenesulfonic acid attracts people's wide attention as a new green organic solvent, the lipophilic toluene part of the p-toluenesulfonic acid can separate lignin through pi-pi accumulation or hydrophobic effect to form micelle-shaped aggregates, so that the lignin is prevented from being re-aggregated, the hydrophilic sulfonic acid part points to water molecules to enable the lignin to be effectively dissolved, the solubility of the p-toluenesulfonic acid at normal temperature is low, and the concentrated waste acid solution can be cooled to the room temperature by using a commercially mature recrystallization technology to realize efficient p-toluenesulfonic acid recovery. For example, Chinese patent publication CN113430855A discloses that the concentration of p-toluenesulfonic acid is 75-80 wt%, the concentration of sodium hypochlorite is 0.7-1.6% (calculated by available chlorine), and the concentration of sodium chlorite is 0.5-1.25%; the solid-liquid ratio of the wood chips to the treatment liquid is 1: 20-1.5: 20 (g: mL), the pretreatment temperature is 90-105 ℃, the pretreatment time is 60-90 min, the digestion process is carried out, the lignin and hemicellulose removal rates are 89.02% and 87.16%, respectively, but the broadleaf wood chips are soaked in water for 4-6 hours at normal temperature and then are subjected to extrusion treatment and then are subjected to digestion reaction, the operation is time-consuming and tedious, the lignin removal rate is not high compared with that of the lignin digested by using p-toluenesulfonic acid alone, the hemicellulose removal rate is not high, the waste liquid treatment load is increased by adding sodium hypochlorite and sodium chlorite, chlorine-containing compounds are not easy to treat, and the environmental impact is large.
Therefore, there is a need to develop a method of pulping lyocell grade dissolving pulp that reduces the amount of cooking chemicals used while reducing the cost of subsequent pollution treatment.
Disclosure of Invention
In order to overcome the disadvantages and shortcomings of the prior art, the primary object of the present invention is to provide a cooking method for preparing a dissolving pulp of a bamboo lyocell fiber grade.
The purpose of the invention is realized by the following scheme:
a stewing method for preparing moso bamboo lyocell fiber grade dissolving pulp specifically comprises the following steps:
(1) performing biomass size reduction treatment on a moso bamboo raw material, then performing dust removal and drying treatment, mixing the moso bamboo and a p-toluenesulfonic acid solvent, and performing a cooking reaction; after the cooking is finished, a mixture of the p-toluenesulfonic acid and the slurry is obtained;
(2) adding washing liquid into the mixture obtained in the step (1) for dilution, then carrying out solid-liquid separation to respectively obtain a black liquid and slurry mixture, and continuously washing the slurry mixture by using the washing liquid until the pH value reaches neutral;
(3) and (3) carrying out ultrasonic treatment on the slurry mixture obtained in the step (2), so that the fibers are dispersed more, the slurry performance is better, and the unbleached pulp for preparing lyocell fiber-grade dissolving pulp is obtained.
The raw material of the moso bamboo subjected to the biomass size reduction treatment in the step (1) is 40-60 meshes;
the p-toluenesulfonic acid solvent in the step (1) is a mixture of p-toluenesulfonic acid and water, and the acid concentration of the p-toluenesulfonic acid is 70% or 80%;
the solid-liquid ratio of the raw bamboo material to the p-toluenesulfonic acid solvent in the step (1) is 1: 20;
the cooking temperature in the step (1) is 70-110 ℃, and the cooking time is 1 h;
the washing solution in the step (2) is at least one of acetone, ethanol and water;
the ultrasonic treatment time used in the step (3) is 10-20 s, and the ultrasonic frequency is 40 kHz.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the method adopts the biomass size reduction treatment, directly mixes the biomass size reduction treatment with the p-toluenesulfonic acid solvent, does not need other additives, has a single and simple cooking process, has a reaction temperature of less than or equal to 110 ℃ and a time of 60min, can send the unbleached pulp to a bleaching system for further treatment after only 2h from material preparation to cooking completion, has alpha-cellulose of 85.55% under the optimal process condition, and has a polymerization degree which is in advance in accordance with the Lyocell fiber grade dissolving pulp standard, and does not need to reduce the polymerization degree.
(2) The key point of the cooking method for preparing the moso bamboo lyocell fiber grade dissolving pulp is that in the cooking process stage, because the lyocell fiber grade dissolving pulp strictly requires low content of hemicellulose and lignin, a large amount of hemicellulose and lignin are removed in the cooking stage to reduce the consumption of chemicals in the subsequent bleaching stage, thereby relieving the complexity of the bleaching process and further achieving the standard of the lyocell fiber grade dissolving pulp. According to the method, the excellent lignin and hemicellulose removing effect of the p-toluenesulfonic acid is utilized, so that the effective separation of the fibers under the conditions of mild reaction conditions, short time consumption, environmental protection and low energy consumption is realized, the high-temperature, high-pressure, high-energy consumption and high chemical consumption required by the cooking of the bamboo raw material are obviously reduced, and the requirements on reaction equipment are reduced; in addition, the selected p-toluenesulfonic acid solvent has low cost, is nontoxic and harmless, can be recycled repeatedly, reduces the consumption of cooking chemicals, simultaneously reduces the subsequent pollution treatment cost, and is economic and environment-friendly.
(3) In the cooking process method provided by the invention, the requirement on equipment is relatively low, the cooking reaction can be finished under normal pressure without high pressure, the temperature required by cooking is obviously reduced, and the energy consumption is greatly reduced.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The reagents used in the examples are commercially available without specific reference.
Example 1
A cooking method for preparing moso bamboo lyocell fiber grade dissolving pulp comprises the following steps:
p-toluenesulfonic acid was mixed with water so that the mass fraction of the p-toluenesulfonic acid solvent was 70%, and a uniform and transparent liquid p-toluenesulfonic acid solvent was formed by magnetic stirring at 60 ℃. Cutting the biomass size of the raw bamboo material into 40-60 meshes, cleaning the sludge on the surface with clear water, air-drying for 3 days in a dry environment, measuring the moisture of the raw bamboo material, and placing the raw bamboo material in a sealing bag for later use.
Respectively weighing 10.00g of moso bamboo 40-60 mesh (absolute dry) and 200ml of paratoluenesulfonic acid solvent, mixing and adding into a normal-pressure reaction kettle for carrying out cooking reaction, wherein the cooking time is 60min, and the cooking temperature is 90 ℃. After cooking, 200ml of washing liquid (water) is added to dilute the solid-liquid mixture, then solid-liquid separation is carried out to respectively obtain a mixture of black liquor and slurry, and the washing liquid is continuously used for washing the slurry mixture until the pH value reaches neutral.
And then, carrying out ultrasonic treatment on the pulp mixture to ensure that the fibers are more dispersed and the pulp performance is better, thus obtaining unbleached pulp for preparing lyocell fiber-grade dissolving pulp. By calculation, the yield of the paper pulp is 42.02%, the lignin content is 8.54%, the lignin removal rate is 88.47%, the hemicellulose removal rate is 87.37%, the cellulose retention rate is 85.55%, the alpha-cellulose content of the unbleached pulp is 85.36% -88.79%, and the polymerization degree is 535-550.
Example 2
A cooking method for preparing moso bamboo lyocell fiber grade dissolving pulp comprises the following steps:
p-toluenesulfonic acid was mixed with water so that the mass fraction of the p-toluenesulfonic acid solvent was 70%, and a uniform and transparent liquid p-toluenesulfonic acid solvent was formed by magnetic stirring at 60 ℃. Cutting the biomass size of the raw bamboo material into 40-60 meshes, cleaning the sludge on the surface with clear water, air-drying for 3 days in a dry environment, measuring the moisture of the raw bamboo material, and placing the raw bamboo material in a sealing bag for later use.
Respectively weighing 10.00g of moso bamboo 40-60 meshes (absolute dry) and 200ml of p-toluenesulfonic acid solvent, mixing, adding into a normal pressure reaction kettle, and performing cooking reaction for 60min at 100 ℃. After cooking, 200ml of washing liquid (ethanol) is added to dilute the solid-liquid mixture, then solid-liquid separation is carried out to respectively obtain a mixture of black liquor and slurry, and the washing liquid is continuously used for washing the slurry mixture until the pH value reaches neutral.
And then carrying out ultrasonic treatment on the pulp mixture to ensure that the fibers are more dispersed and the pulp performance is better, thus obtaining the unbleached pulp for preparing lyocell fiber-grade dissolving pulp. Through calculation, the yield of the paper pulp is 36.33%, the lignin content is 6.83%, the lignin removal rate is 91.67%, the hemicellulose removal rate is 89.93%, the cellulose retention rate is 82.07%, the alpha-cellulose content of the unbleached pulp is 82.65% -86.94%, and the polymerization degree is 508-520.
Example 3
A cooking method for preparing moso bamboo lyocell fiber grade dissolving pulp comprises the following steps:
p-toluenesulfonic acid was mixed with water so that the mass fraction of the p-toluenesulfonic acid solvent was 80%, and a uniform and transparent liquid p-toluenesulfonic acid solvent was formed by magnetic stirring at 60 ℃. Cutting the biomass size of the raw bamboo material into 40-60 meshes, cleaning the sludge on the surface with clear water, air-drying for 3 days in a dry environment, measuring the moisture of the raw bamboo material, and placing the raw bamboo material in a sealing bag for later use.
Respectively weighing 10.00g of moso bamboo 40-60 meshes (absolute dry) and 200ml of p-toluenesulfonic acid solvent, mixing, adding into a normal pressure reaction kettle, and performing cooking reaction for 60min at the temperature of 90 ℃. After cooking, 200ml of washing liquid (acetone) is added to dilute the solid-liquid mixture, then solid-liquid separation is carried out to respectively obtain a mixture of black liquor and slurry, and the washing liquid is continuously used for washing the slurry until the pH value reaches neutral.
And then, carrying out ultrasonic treatment on the pulp mixture to ensure that the fibers are more dispersed and the pulp performance is better, thus obtaining unbleached pulp for preparing lyocell fiber-grade dissolving pulp. According to calculation, the yield of the paper pulp is 37.03%, the lignin content is 5.22%, the lignin removal rate is 93.14%, the hemicellulose removal rate is 90.21%, the cellulose retention rate is 80.16%, the alpha-cellulose content of the unbleached pulp is 80.87% -83.43%, and the polymerization degree is 491-515.
Example 4
A cooking method for preparing moso bamboo lyocell fiber grade dissolving pulp comprises the following steps:
p-toluenesulfonic acid was mixed with water so that the mass fraction of the p-toluenesulfonic acid solvent was 80%, and a uniform and transparent liquid p-toluenesulfonic acid solvent was formed by magnetic stirring at 60 ℃. Cutting the biomass size of the raw bamboo material into 40-60 meshes, cleaning the sludge on the surface with clear water, air-drying for 3 days in a dry environment, measuring the moisture of the raw bamboo material, and placing the raw bamboo material in a sealing bag for later use.
Respectively weighing 10.00g of moso bamboo 40-60 meshes (absolute dry) and 200ml of p-toluenesulfonic acid solvent, mixing, adding into a normal pressure reaction kettle, and performing cooking reaction for 60min at 100 ℃. After cooking, 200ml of washing liquid (acetone/water, v/v ═ 1:1) is added to dilute the solid-liquid mixture, then solid-liquid separation is carried out, black liquor and slurry mixtures are respectively obtained, and the washing of the slurry mixture with the washing liquid is continued until the pH value reaches neutrality.
And then carrying out ultrasonic treatment on the pulp mixture to ensure that the fibers are more dispersed and the pulp performance is better, thus obtaining the unbleached pulp for preparing lyocell fiber-grade dissolving pulp. According to calculation, the yield of the paper pulp is 33.86%, the lignin content is 4.69%, the lignin removal rate is 94.36%, the hemicellulose removal rate is 92.43%, the cellulose retention rate is 78.16%, the alpha-cellulose content of the unbleached pulp is 79.75% -81.26%, and the polymerization degree is 462-480.
Comparative example 1
P-toluenesulfonic acid concentration was 50% (or 60%), cooking temperature was 90 ℃ (or 100 ℃):
respectively weighing 10.00g of moso bamboo 40-60 meshes (absolute dry) and 200ml of p-toluenesulfonic acid solvent, mixing, adding into a normal pressure reaction kettle, and performing cooking reaction for 60 min. After the cooking is finished, the pulp cannot be formed, and the purpose of pulping cannot be achieved.
Comparative example 2
The concentration of p-toluenesulfonic acid is 90%, and the cooking temperature is 90 ℃ or 100 DEG C
Respectively weighing 10.00g of moso bamboo 40-60 meshes (absolute dry) and 200ml of p-toluenesulfonic acid solvent, mixing, adding into a normal pressure reaction kettle, and performing cooking reaction for 60 min. After the cooking is finished, the fiber loss is serious, and the purpose of pulping cannot be achieved.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (7)
1. A cooking method for preparing moso bamboo lyocell fiber grade dissolving pulp is characterized by comprising the following steps:
(1) performing biomass size reduction treatment on a moso bamboo raw material, then performing dust removal and drying treatment, mixing the moso bamboo and a p-toluenesulfonic acid solvent, and performing a cooking reaction; after the cooking is finished, a mixture of the p-toluenesulfonic acid and the slurry is obtained;
(2) adding washing liquid into the mixture obtained in the step (1) for dilution, then carrying out solid-liquid separation to respectively obtain a black liquid and slurry mixture, and continuously washing the slurry mixture by using the washing liquid until the pH value reaches neutral;
(3) and (3) performing ultrasonic treatment on the pulp mixture obtained in the step (2) to ensure that the fibers are more dispersed and the pulp performance is better, so as to obtain unbleached pulp for preparing lyocell fiber-grade dissolving pulp.
2. The cooking method according to claim 1, wherein: the raw material of the moso bamboo subjected to the biomass size reduction treatment in the step (1) is 40-60 meshes.
3. The cooking method according to claim 1, wherein: the p-toluenesulfonic acid solvent in the step (1) is a mixture of p-toluenesulfonic acid and water, and the acid concentration of the p-toluenesulfonic acid is 70% or 80%.
4. The cooking method according to claim 1, wherein: the solid-liquid ratio of the raw bamboo material to the p-toluenesulfonic acid solvent in the step (1) is 1: 20.
5. a pulping process according to claim 1, characterized in that: the cooking temperature in the step (1) is 70-110 ℃, and the cooking time is 1 h.
6. The cooking method according to claim 1, wherein: the washing solution in the step (2) is usually at least one of acetone, ethanol and water.
7. The cooking method according to claim 1, wherein: the ultrasonic treatment time used in the step (3) is 10-20 s, and the ultrasonic frequency is 40 kHz.
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| Publication number | Priority date | Publication date | Assignee | Title |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04126725A (en) * | 1990-09-18 | 1992-04-27 | Oji Paper Co Ltd | Production of lignocellulose-phenolic compound combination co-using blasting method |
| CN105189857A (en) * | 2013-01-25 | 2015-12-23 | 文迪克斯环境股份有限公司 | Process for isolating cellulose from cellulosic biomass, isolated cellulose of type i and composite materials comprising same |
| CN110485188A (en) * | 2019-07-16 | 2019-11-22 | 华南理工大学 | A kind of wood fibre synchronization prepares the method and its application of high pure cellulose and lignin nanoparticle |
| CN110894696A (en) * | 2019-10-30 | 2020-03-20 | 南京林业大学 | Method for bleaching bamboo pulp |
| CN113293636A (en) * | 2021-04-25 | 2021-08-24 | 齐鲁工业大学 | Preparation method of broadleaf wood dissolving pulp |
| CN113430855A (en) * | 2021-05-20 | 2021-09-24 | 齐鲁工业大学 | Preparation method and application of broadleaf wood dissolving pulp |
| CN114086414A (en) * | 2021-10-26 | 2022-02-25 | 华南理工大学 | Lignocellulose pulping method based on acidic eutectic solvent |
-
2022
- 2022-05-19 CN CN202210543981.9A patent/CN114990917A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04126725A (en) * | 1990-09-18 | 1992-04-27 | Oji Paper Co Ltd | Production of lignocellulose-phenolic compound combination co-using blasting method |
| CN105189857A (en) * | 2013-01-25 | 2015-12-23 | 文迪克斯环境股份有限公司 | Process for isolating cellulose from cellulosic biomass, isolated cellulose of type i and composite materials comprising same |
| CN110485188A (en) * | 2019-07-16 | 2019-11-22 | 华南理工大学 | A kind of wood fibre synchronization prepares the method and its application of high pure cellulose and lignin nanoparticle |
| CN110894696A (en) * | 2019-10-30 | 2020-03-20 | 南京林业大学 | Method for bleaching bamboo pulp |
| CN113293636A (en) * | 2021-04-25 | 2021-08-24 | 齐鲁工业大学 | Preparation method of broadleaf wood dissolving pulp |
| CN113430855A (en) * | 2021-05-20 | 2021-09-24 | 齐鲁工业大学 | Preparation method and application of broadleaf wood dissolving pulp |
| CN114086414A (en) * | 2021-10-26 | 2022-02-25 | 华南理工大学 | Lignocellulose pulping method based on acidic eutectic solvent |
Non-Patent Citations (2)
| Title |
|---|
| 尹崇鑫等: "稻草低温p-TsOH制浆性能研究", 《中国造纸学报》 * |
| 沈珮琰: "有机酸体系下溶解浆的制备及机制研究", 《齐鲁工业大学硕士学位论文》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2024051158A1 (en) * | 2022-09-06 | 2024-03-14 | 绍兴文理学院 | Preparation method for distillers grain-based lyocell fiber pulp |
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