CN111979817A - Method for removing lignin from plant fiber - Google Patents
Method for removing lignin from plant fiber Download PDFInfo
- Publication number
- CN111979817A CN111979817A CN202010697503.4A CN202010697503A CN111979817A CN 111979817 A CN111979817 A CN 111979817A CN 202010697503 A CN202010697503 A CN 202010697503A CN 111979817 A CN111979817 A CN 111979817A
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- plant fiber
- pulp
- lignin
- heating
- solid
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- 229920005610 lignin Polymers 0.000 title claims abstract description 47
- 239000000835 fiber Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 230000007935 neutral effect Effects 0.000 claims abstract description 11
- 238000002791 soaking Methods 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 11
- 238000000926 separation method Methods 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 9
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 241000196324 Embryophyta Species 0.000 claims description 19
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 15
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 15
- 241001330002 Bambuseae Species 0.000 claims description 15
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 15
- 239000011425 bamboo Substances 0.000 claims description 15
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000000967 suction filtration Methods 0.000 claims description 8
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 7
- 238000010907 mechanical stirring Methods 0.000 claims description 7
- 229920001131 Pulp (paper) Polymers 0.000 claims description 5
- 238000003760 magnetic stirring Methods 0.000 claims description 5
- 239000010902 straw Substances 0.000 claims description 4
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 3
- 229920000742 Cotton Polymers 0.000 claims description 3
- 238000005485 electric heating Methods 0.000 claims description 3
- 239000010893 paper waste Substances 0.000 claims description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 3
- HDMGAZBPFLDBCX-UHFFFAOYSA-M potassium;sulfooxy sulfate Chemical compound [K+].OS(=O)(=O)OOS([O-])(=O)=O HDMGAZBPFLDBCX-UHFFFAOYSA-M 0.000 claims description 3
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 3
- 239000002023 wood Substances 0.000 claims description 3
- 244000025254 Cannabis sativa Species 0.000 claims description 2
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 claims description 2
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 claims description 2
- 235000014676 Phragmites communis Nutrition 0.000 claims description 2
- 235000009120 camo Nutrition 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 235000005607 chanvre indien Nutrition 0.000 claims description 2
- 239000004459 forage Substances 0.000 claims description 2
- 239000011487 hemp Substances 0.000 claims description 2
- OSVXSBDYLRYLIG-UHFFFAOYSA-N dioxidochlorine(.) Chemical compound O=Cl=O OSVXSBDYLRYLIG-UHFFFAOYSA-N 0.000 abstract description 8
- 239000004155 Chlorine dioxide Substances 0.000 abstract description 4
- 235000019398 chlorine dioxide Nutrition 0.000 abstract description 4
- DJIDJYCQPWEKOF-UHFFFAOYSA-N [Cl].NCCO Chemical compound [Cl].NCCO DJIDJYCQPWEKOF-UHFFFAOYSA-N 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical compound [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 abstract description 3
- 229960002218 sodium chlorite Drugs 0.000 abstract description 3
- GQBMZQUFIOSOMB-UHFFFAOYSA-N [Na].C(C)(=O)OO Chemical compound [Na].C(C)(=O)OO GQBMZQUFIOSOMB-UHFFFAOYSA-N 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 abstract description 2
- 239000012279 sodium borohydride Substances 0.000 abstract description 2
- 229920002678 cellulose Polymers 0.000 description 9
- 239000001913 cellulose Substances 0.000 description 9
- 229920002488 Hemicellulose Polymers 0.000 description 4
- 244000166124 Eucalyptus globulus Species 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 2
- 235000011613 Pinus brutia Nutrition 0.000 description 2
- 241000018646 Pinus brutia Species 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000008104 plant cellulose Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 244000101284 Pinus kesiya Species 0.000 description 1
- 235000005026 Pinus kesiya Nutrition 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Images
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
- D21C3/00—Pulping cellulose-containing materials
- D21C3/02—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes
- D21C3/022—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes in presence of S-containing 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
- 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
- D21H11/02—Chemical or chemomechanical or chemothermomechanical pulp
- D21H11/04—Kraft or sulfate pulp
-
- 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
-
- 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
- D21H11/14—Secondary fibres
Abstract
The invention discloses a method for removing lignin from plant fiber, which comprises the steps of crushing a plant fiber raw material to be removed of lignin, adding the crushed plant fiber raw material into persulfate solution, and soaking at room temperature to obtain a mixed material; heating the mixed material under stirring for several hours at constant temperature; and (3) carrying out solid-liquid separation, and repeatedly washing the obtained solid with water to be neutral to obtain the delignified fiber. The lignin removal rate of the invention can reach 96.6 percent at most; compared with the traditional sodium chlorite method, a chlorine-ethanolamine method, a chlorine dioxide method, a peracetic acid-sodium borohydride method and other processes, the method has the advantages of simple and convenient operation, short process flow, low energy consumption and low environmental hazard.
Description
Technical Field
The invention belongs to the technical field of pulping and papermaking, and particularly relates to a method for removing lignin in plant fibers by a chemical method.
Background
Cellulose is a polysaccharide which is widely distributed and has the highest content in the nature, the yield of the plant cellulose is about 1800 hundred million tons every year, and the plant cellulose is the most promising renewable and biodegradable natural polymer for replacing non-renewable resources such as coal, natural gas, petroleum and the like. Cotton is the purest cellulose source of nature, and the cellulose content is close to 100%, mainly used for the fabric and medical health that human life needs. The cellulose content of other plant fibers is relatively low, and the cellulose in the wood accounts for 40-50%, 10-30% of hemicellulose and 20-30% of lignin; cellulose in the straw pulp accounts for 30-40%, 15-25% of hemicellulose and 20-30% of lignin; cellulose in the bamboo pulp accounts for 40-50%, 15-25% of hemicellulose and 20-30% of lignin; cellulose in the waste paper pulp accounts for 50-61%, lignin 10-20% and hemicellulose 5-15%; that is, if cellulose in plant fiber is used as raw material, lignin in the fiber needs to be removed first, and the lignin removal mainly comprises: sodium chlorite method, chlorine-ethanolamine method, chlorine dioxide method, peracetic acid-sodium borohydride method and the like, but the methods have the defects of long process flow, complex operation, large environmental hazard and the like.
Disclosure of Invention
In order to solve the problems, the invention provides a method for removing lignin in plant fibers, which adopts persulfate to remove the lignin in the plant fibers, and persulfate solution dissolved in water generates a large amount of SO with strong oxidizing capability4 -Radicals and H2O2And opening aromatic rings of the lignin to degrade the lignin which is not dissolved in water into small molecular compounds which are dissolved in water, thereby removing the lignin in the plant fiber.
The invention is realized by the following technical scheme: a method for removing lignin from plant fiber comprises the following steps:
(1) crushing the plant fiber raw material to be delignified;
(2) adding the crushed raw materials obtained in the step (1) into 5-60 wt% of persulfate solution according to the solid-to-liquid ratio g/g of 1: 20-120, and soaking at room temperature for 2-12 hours to obtain a mixed material;
(3) under the condition of stirring, heating the mixed material obtained in the step (2) to 40-90 ℃, and keeping the temperature for 1-16 hours to remove lignin in the fiber;
(4) and (3) carrying out solid-liquid separation, and repeatedly washing the obtained solid with water to be neutral to obtain the delignified fiber.
The plant fiber raw material is one or more than two of bamboo chips, wood chips, forage, wood pulp, straw pulp, hemp pulp, reed pulp, cane pulp, bamboo pulp, rag pulp, cotton pulp and waste paper pulp.
The persulfate is ammonium persulfate, sodium persulfate, potassium persulfate or potassium hydrogen persulfate.
The stirring condition is one of mechanical stirring or magnetic stirring.
The heating is one of water bath heating, electric heating plate heating and electric furnace heating.
The solid-liquid separation is one or two of suction filtration and centrifugation.
Compared with the prior art, the invention has the following advantages:
(1) the persulfate adopted by the invention can generate a large amount of SO when dissolved in water4 -Radicals and H2O2The free radicals and hydrogen peroxide molecules have extremely strong oxidizing capability, and can open aromatic rings of lignin, so that lignin which is insoluble in water is degraded into water-soluble small molecular compounds to be removed from plant fibers.
(2) Compared with the traditional sodium chlorite method, the chlorine-ethanolamine method, the chlorine dioxide method and other methods, the method has the advantages of simple and convenient operation, short process flow, low energy consumption, low environmental hazard and the like. The traditional method has long process flow and complex operation, needs multiple feeding, and also needs multi-stage bleaching if the chlorine dioxide method is adopted. The method provided by the invention can realize the lignin removal rate of more than 90% by one-step feeding without any external operation steps. Secondly, the discharged waste liquid is chlorine-free waste water containingNH4 +And SO4 2-And NH is4 +And SO4 2-Easier to remove than chlorine-containing waste water, e.g. by adjusting NH4 +And SO4 2-Form (NH)4)2SO4And then separation can be achieved by crystallization.
Drawings
FIG. 1 is a photograph of the bamboo chips of example 1 before and after lignin removal;
FIG. 2 is a photograph of unbleached eucalyptus pulp of example 3 before and after lignin removal;
FIG. 3 is a photograph of unbleached Simon pine pulp of example 5 before and after lignin removal.
Detailed Description
The present invention will be described in further detail with reference to the following examples, but the scope of the present invention is not limited to the above-mentioned descriptions.
Example 1
(1) Crushing bamboo chips into bamboo scraps;
(2) adding 10g of the bamboo sawdust in the step (1) into 500g of 35wt% ammonium persulfate solution according to the solid-to-liquid ratio g/g of 1:50, and soaking for 2 hours at room temperature to obtain a mixed material;
(3) under the condition of mechanical stirring, heating the mixed material obtained in the step (2) in a water bath to 70 ℃, and keeping the temperature for 16 hours to remove lignin in the fiber;
(4) and (3) carrying out suction filtration, and repeatedly washing the obtained solid with water to be neutral to obtain the delignified fiber, wherein the lignin removal rate is 93.6%.
Example 2
(1) Crushing bamboo chips into bamboo scraps;
(2) adding 10g of the bamboo sawdust in the step (1) into 500g of 25wt% potassium persulfate solution according to the solid-to-liquid ratio g/g of 1:50, and soaking for 4 hours at room temperature to obtain a mixed material;
(3) under the condition of mechanical stirring, heating the mixed material obtained in the step (2) in a water bath to 70 ℃, and keeping the temperature for 12 hours to remove lignin in the fiber;
(4) and (4) performing suction filtration, and repeatedly washing the obtained solid with water to be neutral to obtain the delignified fiber, wherein the lignin removal rate is 86.9%.
Example 3
(1) Crushing unbleached eucalyptus pulp boards into chips;
(2) adding 10g of the scraps obtained in the step (1) into 250g of 40wt% ammonium persulfate solution according to the solid-to-liquid ratio g/g of 1:25, and soaking for 6 hours at room temperature to obtain a mixed material;
(3) under the condition of mechanical stirring, heating the mixed material obtained in the step (2) in a water bath to 70 ℃, and keeping the temperature for 8 hours to remove lignin in the fiber;
(4) after centrifugal separation, the obtained solid is repeatedly washed to be neutral by water, and the delignified fiber is obtained, and the lignin removal rate is 89.6 percent.
Example 4
(1) Crushing bamboo chips into bamboo scraps;
(2) according to the solid-to-liquid ratio g/g of 1:20, adding 20g of the bamboo sawdust in the step (1) into 400g of 20wt% potassium hydrogen persulfate solution, and soaking at room temperature for 8 hours to obtain a mixed material;
(3) under the condition of magnetic stirring, heating the mixed material electric heating plate in the step (2) to 70 ℃, and keeping the temperature for 6 hours to remove lignin in the fiber;
(4) and (3) carrying out suction filtration, and repeatedly washing the obtained solid with water to be neutral to obtain the delignified fiber, wherein the lignin removal rate is 93.6%.
Example 5
(1) Crushing unbleached Sipun pine pulp into chips;
(2) adding 15g of the scraps obtained in the step (1) into 400g of ammonium persulfate solution with the concentration of 45wt% according to the solid-to-liquid ratio g/g of 1:26.67, and soaking for 6 hours at room temperature to obtain a mixed material;
(3) under the condition of mechanical stirring, heating the mixed material obtained in the step (2) to 80 ℃ in an electric furnace, and keeping the temperature for 4 hours to remove lignin in the fiber;
(4) after suction filtration and centrifugal separation, the obtained solid is repeatedly washed to be neutral by water, and the delignified fiber is obtained, wherein the lignin removal rate is 96.6 percent.
Example 6
(1) Crushing straw into chips;
(2) adding the scraps obtained in the step (1) into 35wt% sodium persulfate solution according to the solid-to-liquid ratio g/g of 1:50, and soaking for 2 hours at room temperature to obtain a mixed material;
(3) under the condition of mechanical stirring, heating the mixed material obtained in the step (2) in a water bath to 40 ℃, and keeping the temperature for 16 hours to remove lignin in the fiber;
(4) and (4) performing suction filtration, and repeatedly washing the obtained solid with water to be neutral to obtain the delignified fiber, wherein the lignin removal rate is 88.8%.
Example 7
(1) Crushing unbleached pinus kesiya pulp into chips;
(2) adding 10g of the scraps obtained in the step (1) into 1000g of ammonium persulfate solution with the concentration of 60wt% according to the solid-to-liquid ratio g/g of 1:100, and soaking for 2 hours at room temperature to obtain a mixed material;
(3) under the condition of magnetic stirring, heating the mixed material obtained in the step (2) in a water bath to 90 ℃, and keeping the temperature for 4 hours to remove lignin in the fiber;
(4) after centrifugal separation, the obtained solid is repeatedly washed to be neutral by water, and the delignified fiber is obtained, and the lignin removal rate is 90.3 percent.
Example 8
(1) Crushing waste corrugated paper into chips;
(2) adding 10g of the scraps obtained in the step (1) into 1200g of ammonium persulfate solution with the concentration of 5wt% according to the solid-to-liquid ratio g/g of 1:120, and soaking for 12 hours at room temperature to obtain a mixed material;
(3) under the condition of magnetic stirring, heating the mixed material obtained in the step (2) in a water bath to 50 ℃, and keeping the temperature for 1h to remove lignin in the fiber;
(4) after suction filtration and centrifugal separation, the obtained solid is repeatedly washed to be neutral by water, and the delignified fiber is obtained, wherein the lignin removal rate is 41.1 percent.
Claims (6)
1. A method for removing lignin from plant fiber is characterized by comprising the following steps:
(1) crushing the plant fiber raw material to be delignified;
(2) adding the crushed raw materials obtained in the step (1) into 5-60 wt% of persulfate solution according to the solid-to-liquid ratio g/g of 1: 20-120, and soaking at room temperature for 2-12 hours to obtain a mixed material;
(3) under the condition of stirring, heating the mixed material in the step (2) to 40-90 ℃, and keeping the temperature for 1-16 h;
(4) and (3) carrying out solid-liquid separation, and repeatedly washing the obtained solid with water to be neutral to obtain the delignified fiber.
2. The method of claim 1, wherein the lignin removal from the plant fiber comprises: the plant fiber raw material is one or more than two of bamboo chips, wood chips, forage, wood pulp, straw pulp, hemp pulp, reed pulp, cane pulp, bamboo pulp, rag pulp, cotton pulp and waste paper pulp.
3. The method of claim 1, wherein the lignin removal from the plant fiber comprises: the persulfate is ammonium persulfate, sodium persulfate, potassium persulfate or potassium hydrogen persulfate.
4. The method of claim 1, wherein the lignin removal from the plant fiber comprises: the stirring condition is one of mechanical stirring or magnetic stirring.
5. The method of claim 1, wherein the lignin removal from the plant fiber comprises: the heating is one of water bath heating, electric heating plate heating and electric furnace heating.
6. The method of claim 1, wherein the lignin removal from the plant fiber comprises: the solid-liquid separation is one or two of suction filtration and centrifugation.
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CN202010697503.4A CN111979817A (en) | 2020-07-20 | 2020-07-20 | Method for removing lignin from plant fiber |
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CN202010697503.4A CN111979817A (en) | 2020-07-20 | 2020-07-20 | Method for removing lignin from plant fiber |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113263572A (en) * | 2021-05-24 | 2021-08-17 | 北京林业大学 | Method for degrading VOCs in wood by using ultrasonic activation persulfate |
CN114016149A (en) * | 2021-08-31 | 2022-02-08 | 南京森奇新材料科技有限公司 | Cellulose fiber, cellulose fiber dispersion liquid and preparation method thereof |
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2020
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113263572A (en) * | 2021-05-24 | 2021-08-17 | 北京林业大学 | Method for degrading VOCs in wood by using ultrasonic activation persulfate |
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CN114016149B (en) * | 2021-08-31 | 2023-11-28 | 南京森奇新材料科技有限公司 | Cellulose fiber, cellulose fiber dispersion liquid and preparation method thereof |
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