CN107938341B - Preparation method of deodorizing cellulose fiber - Google Patents
Preparation method of deodorizing cellulose fiber Download PDFInfo
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- CN107938341B CN107938341B CN201711258683.0A CN201711258683A CN107938341B CN 107938341 B CN107938341 B CN 107938341B CN 201711258683 A CN201711258683 A CN 201711258683A CN 107938341 B CN107938341 B CN 107938341B
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- fiber
- acrylamide
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- copolymerization
- methylpropanesulfonic acid
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- 229920003043 Cellulose fiber Polymers 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 230000001877 deodorizing effect Effects 0.000 title claims abstract description 24
- 238000007334 copolymerization reaction Methods 0.000 claims abstract description 44
- 239000008234 soft water Substances 0.000 claims abstract description 39
- 238000003756 stirring Methods 0.000 claims abstract description 32
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 23
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 23
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000003513 alkali Substances 0.000 claims abstract description 21
- 239000011259 mixed solution Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000002781 deodorant agent Substances 0.000 claims abstract description 12
- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical compound CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-UHFFFAOYSA-N 0.000 claims description 76
- 238000006243 chemical reaction Methods 0.000 claims description 71
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 35
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 35
- 239000000203 mixture Substances 0.000 claims description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 19
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 12
- 230000007935 neutral effect Effects 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 4
- 238000006297 dehydration reaction Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 3
- 239000000835 fiber Substances 0.000 abstract description 75
- 238000004332 deodorization Methods 0.000 abstract description 18
- 230000000977 initiatory effect Effects 0.000 abstract description 8
- 230000009471 action Effects 0.000 abstract description 7
- 239000004519 grease Substances 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 5
- 206010042674 Swelling Diseases 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 3
- 230000008961 swelling Effects 0.000 abstract description 3
- 238000007380 fibre production Methods 0.000 abstract description 2
- 238000004886 process control Methods 0.000 abstract description 2
- IRLPACMLTUPBCL-KQYNXXCUSA-N 5'-adenylyl sulfate Chemical compound C1=NC=2C(N)=NC=NC=2N1[C@@H]1O[C@H](COP(O)(=O)OS(O)(=O)=O)[C@@H](O)[C@H]1O IRLPACMLTUPBCL-KQYNXXCUSA-N 0.000 abstract 1
- 239000000047 product Substances 0.000 description 48
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 16
- 239000000126 substance Substances 0.000 description 12
- 230000000694 effects Effects 0.000 description 11
- 238000005303 weighing Methods 0.000 description 7
- 229920001519 homopolymer Polymers 0.000 description 6
- 229910021529 ammonia Inorganic materials 0.000 description 5
- 210000004243 sweat Anatomy 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- HKVFISRIUUGTIB-UHFFFAOYSA-O azanium;cerium;nitrate Chemical compound [NH4+].[Ce].[O-][N+]([O-])=O HKVFISRIUUGTIB-UHFFFAOYSA-O 0.000 description 4
- 229910052791 calcium Inorganic materials 0.000 description 4
- 239000011575 calcium Substances 0.000 description 4
- 239000004744 fabric Substances 0.000 description 4
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 239000011941 photocatalyst Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- XMPZTFVPEKAKFH-UHFFFAOYSA-P ceric ammonium nitrate Chemical compound [NH4+].[NH4+].[Ce+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O XMPZTFVPEKAKFH-UHFFFAOYSA-P 0.000 description 3
- 238000004945 emulsification Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000009987 spinning Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- XYHKNCXZYYTLRG-UHFFFAOYSA-N 1h-imidazole-2-carbaldehyde Chemical compound O=CC1=NC=CN1 XYHKNCXZYYTLRG-UHFFFAOYSA-N 0.000 description 2
- GWYFCOCPABKNJV-UHFFFAOYSA-M 3-Methylbutanoic acid Natural products CC(C)CC([O-])=O GWYFCOCPABKNJV-UHFFFAOYSA-M 0.000 description 2
- 150000000703 Cerium Chemical class 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 2
- 241001122767 Theaceae Species 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- GWYFCOCPABKNJV-UHFFFAOYSA-N beta-methyl-butyric acid Natural products CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000003670 easy-to-clean Effects 0.000 description 2
- 239000003995 emulsifying agent Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 230000002522 swelling effect Effects 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- HDTRYLNUVZCQOY-UHFFFAOYSA-N α-D-glucopyranosyl-α-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OC1C(O)C(O)C(O)C(CO)O1 HDTRYLNUVZCQOY-UHFFFAOYSA-N 0.000 description 1
- PFTAWBLQPZVEMU-DZGCQCFKSA-N (+)-catechin Chemical compound C1([C@H]2OC3=CC(O)=CC(O)=C3C[C@@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-DZGCQCFKSA-N 0.000 description 1
- BSAIUMLZVGUGKX-BQYQJAHWSA-N (E)-non-2-enal Chemical compound CCCCCC\C=C\C=O BSAIUMLZVGUGKX-BQYQJAHWSA-N 0.000 description 1
- 229920000536 2-Acrylamido-2-methylpropane sulfonic acid Polymers 0.000 description 1
- XHZPRMZZQOIPDS-UHFFFAOYSA-N 2-Methyl-2-[(1-oxo-2-propenyl)amino]-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(C)(C)NC(=O)C=C XHZPRMZZQOIPDS-UHFFFAOYSA-N 0.000 description 1
- BSAIUMLZVGUGKX-UHFFFAOYSA-N 2-Nonenal Natural products CCCCCCC=CC=O BSAIUMLZVGUGKX-UHFFFAOYSA-N 0.000 description 1
- 241000193830 Bacillus <bacterium> Species 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 241000486761 Chilobrachys Species 0.000 description 1
- 206010063385 Intellectualisation Diseases 0.000 description 1
- 229910006069 SO3H Inorganic materials 0.000 description 1
- 239000004113 Sepiolite Substances 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- HDTRYLNUVZCQOY-WSWWMNSNSA-N Trehalose Natural products O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 HDTRYLNUVZCQOY-WSWWMNSNSA-N 0.000 description 1
- 208000037386 Typhoid Diseases 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- HDTRYLNUVZCQOY-LIZSDCNHSA-N alpha,alpha-trehalose Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 HDTRYLNUVZCQOY-LIZSDCNHSA-N 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- ADRVNXBAWSRFAJ-UHFFFAOYSA-N catechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3ccc(O)c(O)c3 ADRVNXBAWSRFAJ-UHFFFAOYSA-N 0.000 description 1
- 235000005487 catechin Nutrition 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229950001002 cianidanol Drugs 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 229910052624 sepiolite Inorganic materials 0.000 description 1
- 235000019355 sepiolite Nutrition 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 201000008297 typhoid fever Diseases 0.000 description 1
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
- D06M14/02—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of natural origin
- D06M14/04—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of natural origin of vegetal origin, e.g. cellulose or derivatives thereof
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/58—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides
- D06M11/59—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides with ammonia; with complexes of organic amines with inorganic substances
- D06M11/60—Ammonia as a gas or in solution
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/402—Amides imides, sulfamic acids
- D06M13/432—Urea, thiourea or derivatives thereof, e.g. biurets; Urea-inclusion compounds; Dicyanamides; Carbodiimides; Guanidines, e.g. dicyandiamides
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/285—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acid amides or imides
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
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Abstract
The invention discloses a preparation method of a deodorizing cellulose fiber, and belongs to the technical field of fiber production. Firstly, pretreating cellulose fibers with alkali liquor to remove impurities such as grease on the surfaces of the fibers, and meanwhile, completing the swelling treatment of the fibers; secondly, injecting soft water, adding AMPS and AA, stirring uniformly, then adding SDS, completing the preparation of the copolymerization mixed solution, the preparation is convenient, the copolymerization mixed solution is more uniform, and the process control is realized; and finally, carrying out copolymerization reaction on the treated cellulose fiber and the copolymerization mixed solution under the initiation action of ammonium ceric nitrate to finally obtain the deodorant cellulose fiber product. The deodorization product is prepared by adopting a copolymerization grafting method, and the method has little damage to fibers, does not cause the reduction of fiber strength, and does not damage the hand feeling of the fibers; and the deodorization fiber can be recycled for many times, the characteristics of the fiber such as color, texture and the like can not be changed, the market demand is greatly met, and the life quality of people is improved.
Description
Technical Field
The invention relates to a preparation method of fibers, in particular to a preparation method of deodorizing cellulose fibers, and belongs to the technical field of fiber production.
Background
Along with the improvement of the quality of life, people have increasing demands on sanitary, fresh and environment-friendly life styles besides the requirements on a full and healthy life. In daily life, people can sweat at any time, and particularly in a high-temperature airtight environment, the people often have peculiar smell, namely sweat odor, and after the sweat odor secretes sweat, some organic matters in the sweat release ammonia, acetic acid, isovaleric acid and the like.
At present, there is also a lot of research on deodorizing fibers, and there are also many deodorizing fabrics on the market. The deodorizing principle of these products varies: firstly, adding a physical adsorption material during fiber spinning, and removing odor by adopting physical spinning; adding nano particles or photocatalyst into the fiber or performing surface post-treatment to decompose ammonia, formaldehyde and the like into carbon dioxide and water for deodorization; thirdly, by inhibiting and killing bacteria on the surface of the fabric, the generation of peculiar smell is prevented, and the fabric can react with ammonia gas, hydrogen sulfide and the like to achieve the aim of deodorization; and fourthly, deodorizing on the surface of the fabric through an after-finishing mode by utilizing the combined action of a physical mode and a chemical mode. Fifthly, sepiolite and trehalose are blended and spun in a lake-born subject group of Qingdao university, and the deodorization rate of the prepared deodorization fiber on ammonia gas, isovaleric acid, 2-nonenal and the like reaches more than 85%; research on the honeycomb microporous structure photocatalyst fibers shows that the photocatalyst fibers can effectively decompose harmful gases such as ammonia, formaldehyde, smoke odor and the like into carbon dioxide and water under sunlight and visible light, so that deodorization is realized; seven and the Chilobrachys Lijingzhao of the university of Tohua indicate that substances such as tea polyphenol, catechin and the like in tea fibers not only have good antibacterial property on typhoid bacillus, staphylococcus aureus and the like, but also can be combined with NH3、H2S and the like interact to deodorize; eighthly, Chen wenxing and the like dye silk fibers, fix the color in a copper (II) -ion-containing solution, and perform a complex reaction on copper (II) ions on the fibers with ammonia gas and hydrogen sulfide to deodorize.
However, these deodorization methods still have many problems such as: the deodorant fiber obtained by blending spinning can cause the problems of reduced fiber strength and poor hand feeling; the photocatalyst can damage the strength of the fiber while deodorizing, and metal ions in the fiber can affect the color of the fiber after being complexed with ammonia gas, hydrogen sulfide and the like.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of deodorizing cellulose fibers. The deodorizing cellulose fiber is prepared by adopting a copolymerization grafting method, and the method has small damage to the fiber, cannot cause the reduction of the fiber strength, and cannot damage the fiber hand feeling; and the deodorization fiber can be recycled for many times, the characteristics of the fiber such as color, texture and the like can not be changed, the market demand is greatly met, and the life quality of people is improved.
In order to achieve the technical purpose, the following technical scheme is proposed:
a preparation method of deodorizing cellulose fibers comprises the following steps:
A. pretreatment of cellulose fibres
Adding cellulose fibers serving as raw materials into a reaction kettle I, and adding the cellulose fibers in parts by mass (kg): taking alkali liquor with the volume (L) of 1:4-1:20, and adding the alkali liquor into the reaction kettle I; then, heating the reaction kettle I to 60-100 ℃, and stirring for 0.5-5 h; washing the mixed material by soft water until the mixed material is neutral, and dehydrating to obtain a product I for later use;
B. preparation of copolymerization mixture
And (2) injecting normal-temperature soft water into the reaction kettle II, wherein the mass (kg) of the 2-acrylamide-2-methylpropanesulfonic acid is as follows: and the volume (L) of the acrylic acid is 1:0.8-1:1.3, 2-acrylamide-2-methylpropanesulfonic acid and the acrylic acid are respectively taken and are respectively placed in a reaction kettle II, the mixture is uniformly stirred, and after the 2-acrylamide-2-methylpropanesulfonic acid is dissolved, the mass (kg) of the 2-acrylamide-2-methylpropanesulfonic acid is calculated as follows: weighing sodium dodecyl sulfate at a ratio of 1:0.02-1:0.20 in mass (kg), adding into a reaction kettle II, and stirring to completely dissolve to obtain a product II, namely a copolymerization mixed solution for later use;
C. copolymerization reaction
Mass (kg) of product I: weighing the product I, adding the product I into a reaction kettle II and uniformly mixing the product I and the product II, wherein the volume (L) of the product II is 1:4-1: 20; then, adding ammonium ceric nitrate into the reaction kettle II, stirring, heating to 40-80 ℃, and reacting for 1-8 h; after the reaction, the mixture is washed by soft water to be clear, dehydrated and dried to obtain the cellulose fiber copolymer, namely the deodorant cellulose fiber product.
Further, in the step A, the alkali liquor is any one of sodium hydroxide solution, ammonia water and urea.
Furthermore, in the step A, the mass concentration of the alkali liquor is 0.5-1.0%, the cellulose fibers can be dissolved in the alkali liquor, and the alkali liquor with the mass concentration of 0.5-1.0% is selected, so that the cellulose fibers can be fully cleaned and swelled, and excessive fiber loss caused by the fact that the cellulose fibers are dissolved in the alkali liquor can be avoided.
Further, in the step B, before adding the 2-acrylamide-2-methyl propanesulfonic acid in the step B, the mass concentration of the 2-acrylamide-2-methyl propanesulfonic acid is controlled to be 1-20%, and the mass concentration of AMPS is equal to the total mass of AMPS/(AMPS, AA and soft water). Because the acid can damage the cellulose fiber and reduce the strength of the fiber, and the low AMPS dosage can cause the deodorization effect of the fiber to be poor, the mass fraction is selected to be 1-20%, so that the deodorization effect of the fiber can be ensured, and the strength of the fiber cannot be greatly damaged.
Further, in the step C, the added mass of the ammonium cerium nitrate is 5-20% of that of the 2-acrylamide-2-methylpropanesulfonic acid, the reaction can be initiated only when the ammonium cerium nitrate reaches a specific concentration, the amount of the ammonium cerium nitrate required for initiating the cellulose fibers is certain, and the excessive ammonium cerium nitrate can greatly initiate AMPS and AA to generate a homopolymer; 5-20% of ammonium ceric nitrate is selected, so that the fiber can be effectively initiated to react with AMPS and AA, and excessive AMPS and AA homopolymers can not be generated.
The invention adopts the following principle:
the cerium salt is used for initiating the cellulose fiber to graft the vinyl monomer, so as to realize the modification of the cellulose fiber. All the C2-C3 parts in cellulose glucose ring have-OH, complex is generated under the action of cerium salt, and the complex is decomposed to form free radicalThe vinyl monomer with high activity is subjected to copolymerization reaction, namely, under the action of ammonium ceric nitrate, free radicals are firstly formed on the cellulose fiber molecular chain, and then copolymerization reaction is carried out on the cellulose fiber molecular chain, the cellulose fiber and Acrylic Acid (AA) and 2-acrylamide-2-methylpropanesulfonic Acid (AMPS) SO as to enable the fiber to have-COOH and-SO3H group, with NH3Reaction is carried out, thereby achieving the purpose of removing ammonia gas.
In the present invention, the action of the substances involved:
alkali liquor: firstly, impurities such as grease on the surface of the fiber can be removed, secondly, the alkali solution has a certain swelling effect on the fiber, and the treated fiber can better react with drugs;
soft water: firstly, the solution is used as a solvent to dissolve the substances added in the step A, B, and secondly, the fibers are cleaned;
2-acrylamido-2-methylpropanesulfonic acid: the product can be used together with acrylic acid to achieve the purpose of deodorization;
acrylic acid: the deodorant is acted with 2-acrylamide-2-methylpropanesulfonic acid together to achieve the aim of deodorization;
sodium dodecyl sulfate: firstly, 2-acrylamide-2-methylpropanesulfonic acid and acrylic acid are emulsified, and the generated homopolymer cannot be adhered to the surface of the fiber and is easier to clean; secondly, the fiber has a permeation function and permeates into the fiber, so that the reaction is more sufficient;
cerium ammonium nitrate: the initiating fiber reacts with the 2-acrylamide-2-methylpropanesulfonic acid and the acrylic acid to play an initiating role.
By adopting the technical scheme, the beneficial technical effects brought are as follows:
1) in the invention, firstly, alkali liquor pretreatment is carried out on cellulose fibers to remove impurities such as grease on the surfaces of the fibers and complete the swelling treatment of the fibers; secondly, injecting soft water, adding AMPS and AA, stirring uniformly, and then adding SDS to finish the preparation of the copolymerization mixed solution, wherein the preparation process is convenient, the generated copolymerization mixed solution is uniform, and the process control is effectively realized; and finally, carrying out copolymerization reaction on the treated cellulose fiber and the copolymerization mixed solution under the initiation action of ammonium ceric nitrate to finally obtain the deodorant cellulose fiber product. The deodorization fiber product is prepared by adopting a copolymerization grafting method, so that the market demand is greatly met, and the life quality of people is improved; meanwhile, the method is simple to operate, and can realize the controllability and the intellectualization of the process;
2) in the invention, the deodorizing cellulose fiber prepared by adopting the copolymerization grafting method has little damage to the fiber, does not cause the reduction of the fiber strength, and does not damage the fiber hand feeling;
3) in the invention, the prepared deodorization fiber can be recycled for many times without changing the characteristics of the fiber such as color, texture and the like;
4) in step A of the present invention, the treatment with the alkaline solution has two functions: firstly, impurities such as grease on the surface of the fiber can be removed, secondly, the alkali solution has a certain swelling effect on the fiber, and the treated fiber can better react with the subsequent copolymerization mixed solution. And the reason why the fiber is washed to be neutral: the subsequent cerium ammonium nitrate has better reaction performance in neutral to acidic environment, and the subsequent copolymerization mixed liquid is prevented from reacting with the residual alkali liquor, so that the effect of the final product is reduced. The soft water is adopted for washing, so that no other water exists, the soft water is used because calcium and magnesium substances are removed from the soft water, if the residual calcium and magnesium substances in the cellulose fibers react with the subsequently added copolymerization mixed liquid, the effect of the finally obtained product is reduced, and the damage of the soft water to the reaction kettle is extremely low. The temperature is raised to 60-100 ℃, and the temperature is set, so that the alkali liquor can more easily clean impurities such as grease on the surface of the cellulose fiber. Stirring for 0.5-5h, and fully washing and swelling the fibers by the alkali liquor during stirring. The ratio of the cellulose fiber to the alkali liquor is 1:4-1:20, and the fiber can be fully cleaned and swelled without causing excessive waste of water and alkali. The proportion of the fiber is larger than the proportion, so that waste is caused, and the fiber is not fully cleaned and swelled when the proportion of the fiber is smaller than the proportion;
5) in the step B of the invention, soft water is injected into the reaction kettle II, but other water can not be used, because the soft water mainly dissolves the added AMPS and AA in the reaction kettle II, calcium and magnesium substances contained in the soft water are low and cannot react with the added AMPS and AA, the product quality is better ensured, and the reaction kettle can be better protected from being damaged by using the soft water. During the preparation of the copolymerization mixed solution, AMPS and AA are added firstly, and SDS is added, because: AMPS and AA are both acids, and are mutually dissolved in soft water more easily without other influences, SDS is used as an emulsifier, and after the AMPS and the AA are dissolved uniformly, emulsification is carried out, so that the obtained emulsion is more uniform. The ratio of AMPS to AA is 1:0.8-1:1.3, under the condition of the ratio, AMPS and AA are crossly distributed uniformly in the fiber obtained after the reaction with the cellulose fiber, and the fiber under the structure has good deodorization performance. If the ratio is larger or smaller than the above ratio, the structure of the fibers becomes irregular, and the deodorizing effect is not good. And (3) uniformly stirring the AMPS and the AA at a constant speed, so that after SDS is added for emulsification, the number of the AMPS and the AA wrapped in each emulsified particle is uniform. The proportion of 1:0.02-1:0.20 is adopted between AMPS and SDS, under the proportion, the added SDS can not only fully emulsify AMPS and AA, but also can better clean finally obtained fibers, if the proportion is less than the proportion, the emulsification is not sufficient, a large amount of homopolymer can be generated in subsequent reaction, the amounts of AMPS and AA grafted to the fibers are reduced, and the homopolymer is adhered to the fibers and is not easy to clean; the SDS can permeate into the fibers and is more than the mixture ratio, so the fibers are not easy to clean in the subsequent cleaning;
6) in the step C of the invention, the product I and the product II are mixed according to the proportion of 1:4-1:20, and under the proportion, the cellulose fiber and the copolymerization mixed solution can be ensured to fully react to obtain the deodorant fiber with better effect, and the copolymerization mixed solution can not be wasted. Because the reaction degree between the cellulose fiber and the copolymerization mixed solution is limited and is larger than the proportion, the fiber with better effect can not be obtained, and the waste of the medicine can be caused; if the ratio is less than the above ratio, the reaction degree between the cellulose fiber and the copolymerization mixed solution is not sufficient, and the obtained fiber has poor deodorization effect. Adding ammonium ceric nitrate into the reaction kettle II, wherein the ammonium ceric nitrate plays an initiating role in the reaction, and the target reaction can be generated between the product I and the product II under the action of the ammonium ceric nitrate; adding ammonium ceric nitrate into the reaction kettle II, stirring, heating to 40-80 ℃, and reacting for 1-8 h; the initiation of ammonium ceric nitrate needs to be carried out at a certain temperature, and the optimal reaction temperature range is 40-80 ℃. Because the content of calcium and magnesium substances in the soft water is extremely low, the deodorization effect of the fiber cannot be reduced by adopting soft water for washing. After copolymerization, washing with soft water to be clear, mainly washing substances generated in the polymerization reaction process and initiated by AMPS and AA homopolymer, emulsifier SDS and ammonium ceric nitrate, wherein the substances are generated in the steps of adding ammonium ceric nitrate to initiate the reaction process of cellulose fibers and AMPS and AA, and washing substances can be generated by controlling the amount of the substances and the process conditions, because ammonium ceric nitrate also initiates the reaction of AMPS and AA when the cellulose fibers and AMPS and AA are initiated to react, the washing with soft water is required to be clear.
Detailed Description
In the following, specific embodiments of the technical solutions of the present invention are clearly and completely described, and it is obvious that the described embodiments are only a part of the embodiments of the technical solutions of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
A preparation method of deodorizing cellulose fiber comprises the following specific process steps:
A. pretreatment of cellulose fibres
Adding cellulose fibers serving as raw materials into a reaction kettle I, and adding the cellulose fibers in parts by mass (kg): taking the sodium hydroxide solution with the volume (L) of 1:10, and adding the sodium hydroxide solution into the reaction kettle I; then, heating the reaction kettle I to 90 ℃, and stirring for 1 h; washing the mixed material by soft water to be neutral, and dehydrating to obtain a product I for later use;
B. preparation of copolymerization mixture
And (2) injecting normal-temperature soft water into the reaction kettle II, wherein the mass (kg) of the 2-acrylamide-2-methylpropanesulfonic acid is as follows: and (2) respectively taking 2-acrylamide-2-methylpropanesulfonic acid and acrylic acid according to the volume (L) of 1:1, placing the two materials in a reaction kettle II, uniformly stirring the two materials until the two materials are uniform, and dissolving the 2-acrylamide-2-methylpropanesulfonic acid, wherein the mass (kg) of the 2-acrylamide-2-methylpropanesulfonic acid is as follows: weighing sodium dodecyl sulfate according to the mass ratio of 1:0.08, adding the sodium dodecyl sulfate into a reaction kettle II, and stirring until the sodium dodecyl sulfate is completely dissolved to obtain a product II, namely a copolymerization mixed solution for later use;
C. copolymerization reaction
Mass (kg) of product I: weighing the product I, adding the product I into a reaction kettle II and uniformly mixing the product I and the product II, wherein the volume (L) of the product II is 1: 10; then, adding ammonium ceric nitrate into the reaction kettle II, stirring, heating to 58 ℃, and reacting for 4 hours; after the reaction, the mixture is washed by soft water to be clear, dehydrated and dried to obtain the cellulose fiber copolymer, namely the deodorant cellulose fiber product.
In step A, the concentration of the sodium hydroxide solution is 0.8%.
In the step B, before adding the 2-acrylamide-2-methylpropanesulfonic acid, the mass concentration of the 2-acrylamide-2-methylpropanesulfonic acid is controlled to be 10%.
In the step C, the added mass of the cerium ammonium nitrate is 13% of the mass of the 2-acrylamide-2-methylpropanesulfonic acid.
Example 2
A preparation method of deodorizing cellulose fibers comprises the following steps:
A. pretreatment of cellulose fibres
Adding cellulose fibers serving as a raw material into a reaction kettle I, adding 4L of sodium hydroxide solution with the mass concentration of 0.5% into each kilogram of the raw material, heating the reaction kettle I to 60 ℃, and stirring for 5 hours; then soft water is used for washing the mixed materials to be neutral, and dehydration is carried out to obtain a product I for later use;
B. preparation of copolymerization mixture
Injecting normal-temperature soft water into a reaction kettle II, adding 2-acrylamide-2-methylpropanesulfonic acid, adding 0.8L of acrylic acid into each kilogram of 2-acrylamide-2-methylpropanesulfonic acid, uniformly stirring until the mixture is uniform, adding 0.02kg of sodium dodecyl sulfate into each kilogram of 2-acrylamide-2-methylpropanesulfonic acid after the 2-acrylamide-2-methylpropanesulfonic acid is dissolved, and stirring until the mixture is completely dissolved to obtain a product II, namely a copolymerization mixed solution for later use;
before adding 2-acrylamide-2-methylpropanesulfonic acid, controlling the mass concentration of 2-acrylamide-2-methylpropanesulfonic acid to be 1%;
C. copolymerization reaction
Adding 0.05kg of the product I into each liter of the product II in a reaction kettle II, uniformly mixing, then adding ammonium ceric nitrate into the reaction kettle II, stirring, heating to 40 ℃, and reacting for 8 hours; after the reaction, washing the mixture by soft water until the mixture is clear, dehydrating and drying the mixture to obtain a cellulose fiber copolymer, namely a deodorant cellulose fiber product;
the added mass of the ammonium ceric nitrate is 5 percent of the mass of the 2-acrylamide-2-methylpropanesulfonic acid.
Example 3
A preparation method of deodorizing cellulose fibers comprises the following steps:
A. pretreatment of cellulose fibres
Adding cellulose fibers serving as a raw material into a reaction kettle I, adding 20L of ammonia water with the mass concentration of 1.0% into each kilogram of the raw material, heating the reaction kettle I to 100 ℃, and stirring for 0.5 h; then soft water is used for washing the mixed materials to be neutral, and dehydration is carried out to obtain a product I for later use;
B. preparation of copolymerization mixture
Injecting normal-temperature soft water into a reaction kettle II, adding 2-acrylamide-2-methylpropanesulfonic acid, adding 1.3L of acrylic acid into each kilogram of 2-acrylamide-2-methylpropanesulfonic acid, uniformly stirring until the mixture is uniform, adding 0.20kg of sodium dodecyl sulfate into each kilogram of 2-acrylamide-2-methylpropanesulfonic acid after the 2-acrylamide-2-methylpropanesulfonic acid is dissolved, and stirring until the mixture is completely dissolved to obtain a product II, namely a copolymerization mixed solution for later use;
before adding 2-acrylamide-2-methylpropanesulfonic acid, controlling the mass concentration of 2-acrylamide-2-methylpropanesulfonic acid to be 20%;
C. copolymerization reaction
Adding 0.25kg of product I into each liter of product II in a reaction kettle II, uniformly mixing, then adding ammonium ceric nitrate into the reaction kettle II, stirring, heating to 80 ℃, and reacting for 1 h; after the reaction, washing the mixture by soft water until the mixture is clear, dehydrating and drying the mixture to obtain a cellulose fiber copolymer, namely a deodorant cellulose fiber product;
the added mass of the ammonium ceric nitrate is 20% of the mass of the 2-acrylamide-2-methylpropanesulfonic acid.
Example 4
A preparation method of deodorizing cellulose fibers comprises the following steps:
A. pretreatment of cellulose fibres
Adding cellulose fibers serving as a raw material into a reaction kettle I, adding 12L of urea alkali liquor with the mass concentration of 0.8% into each kilogram of the raw material, heating the reaction kettle I to 80 ℃, and stirring for 3 hours; then soft water is used for washing the mixed materials to be neutral, and dehydration is carried out to obtain a product I for later use;
B. preparation of copolymerization mixture
Injecting normal-temperature soft water into a reaction kettle II, adding 2-acrylamide-2-methylpropanesulfonic acid, adding 1.1L of acrylic acid into each kilogram of 2-acrylamide-2-methylpropanesulfonic acid, uniformly stirring until the mixture is uniform, adding 0.12kg of sodium dodecyl sulfate into each kilogram of 2-acrylamide-2-methylpropanesulfonic acid after the 2-acrylamide-2-methylpropanesulfonic acid is dissolved, and stirring until the mixture is completely dissolved to obtain a product II, namely a copolymerization mixed solution for later use;
before adding 2-acrylamide-2-methylpropanesulfonic acid, controlling the mass concentration of 2-acrylamide-2-methylpropanesulfonic acid to be 12%;
C. copolymerization reaction
Adding 0.14kg of product I into each liter of product II in a reaction kettle II, uniformly mixing, then adding ammonium ceric nitrate into the reaction kettle II, stirring, heating to 60 ℃, and reacting for 5 hours; after the reaction, washing the mixture by soft water until the mixture is clear, dehydrating and drying the mixture to obtain a cellulose fiber copolymer, namely a deodorant cellulose fiber product;
the adding mass of the ammonium ceric nitrate is 13 percent of the mass of the 2-acrylamide-2-methylpropanesulfonic acid
Example 5
A preparation method of deodorizing cellulose fibers comprises the following steps:
A. pretreatment of cellulose fibres
Taking 1.8kg of cellulose fiber as a raw material, adding the raw material into a reaction kettle I, taking 18L of sodium hydroxide solution with the mass concentration of 1%, and adding the sodium hydroxide solution into the reaction kettle I; then, heating the reaction kettle I to 80 ℃, and stirring for 3 hours; washing the mixed material by soft water until the mixed material is neutral, and dehydrating to obtain a product I for later use;
B. preparation of copolymerization mixture
Injecting normal-temperature soft water into a reaction kettle II, respectively weighing 1.8kg of 2-acrylamide-2-methylpropanesulfonic acid and 1.8L of acrylic acid, placing the weighed materials in the reaction kettle II, controlling the mass concentration of the 2-acrylamide-2-methylpropanesulfonic acid to be 10% (AMPS mass/(AMPS, AA and soft water) total mass), uniformly stirring the materials to be uniform, weighing 0.144kg of sodium dodecyl sulfate after the 2-acrylamide-2-methylpropanesulfonic acid is dissolved, adding the weighed materials into the reaction kettle II, and stirring the materials to be completely dissolved to obtain a product II, namely a copolymerization mixed solution for later use;
C. copolymerization reaction
Respectively weighing 1.8kg of product I and 18L of product II, adding into a reaction kettle II, and uniformly mixing; then, 0.30kg of ammonium ceric nitrate is added into the reaction kettle II, stirred, heated to 60 ℃ and reacted for 5 hours; after the reaction, the mixture is washed by soft water to be clear, dehydrated and dried to obtain the cellulose fiber copolymer, namely the deodorant cellulose fiber product.
Example 6
On the basis of the above examples 1 to 5, the deodorizing fiber effect was tested, and a sensory test method was used.
Respectively placing 5g of untreated fiber and deodorized cellulose fiber in two closed flasks, and respectively adding 10-15ml of 0.75% ammonia water solution into the two flasks; after standing for 15-20min, the gas in the two flasks was smelled by 3 normal smelling testers, and the results showed that: the bottle of untreated fiber had a strong ammonia odor, and the flask in which the cellulose fiber was deodorized had little ammonia odor. The above results were still obtained after washing both fibers and 5 cycles.
Claims (4)
1. A preparation method of deodorizing cellulose fiber is characterized by comprising the following steps: the method comprises the following steps:
A. pretreatment of cellulose fibres
Adding cellulose fibers serving as a raw material into a reaction kettle I, adding 4-20L of alkali liquor into each kilogram of raw material, heating the reaction kettle I to 60-100 ℃, and stirring for 0.5-5 h; then soft water is used for washing the mixed materials to be neutral, and dehydration is carried out to obtain a product I for later use;
B. preparation of copolymerization mixture
Injecting normal-temperature soft water into a reaction kettle II, adding 2-acrylamide-2-methylpropanesulfonic acid, adding 0.8-1.3L of acrylic acid into each kilogram of 2-acrylamide-2-methylpropanesulfonic acid, uniformly stirring until the mixture is uniform, adding 0.02-0.20kg of sodium dodecyl sulfate into each kilogram of 2-acrylamide-2-methylpropanesulfonic acid after the 2-acrylamide-2-methylpropanesulfonic acid is dissolved, and stirring until the mixture is completely dissolved to obtain a product II, namely a copolymerization mixed solution for later use;
C. copolymerization reaction
Adding 0.05-0.25kg of product I into each liter of product II in a reaction kettle II, uniformly mixing, then adding ammonium ceric nitrate into the reaction kettle II, stirring, heating to 40-80 ℃, and reacting for 1-8 hours; after the reaction, washing the mixture by soft water until the mixture is clear, dehydrating and drying the mixture to obtain a cellulose fiber copolymer, namely a deodorant cellulose fiber product;
the adding mass of the ammonium ceric nitrate is 5-20% of the mass of the 2-acrylamide-2-methylpropanesulfonic acid.
2. The method for producing a deodorizing cellulose fiber according to claim 1, characterized in that: in the step A, the alkali liquor is any one of sodium hydroxide solution, ammonia water and urea.
3. The method for producing deodorizing cellulose fibers according to claim 1 or 2, characterized in that: in the step A, the mass fraction of the alkali liquor is 0.5-1.0%.
4. The method for producing a deodorizing cellulose fiber according to claim 1, characterized in that: in the step B, before adding the 2-acrylamide-2-methylpropanesulfonic acid, controlling the mass concentration of the 2-acrylamide-2-methylpropanesulfonic acid to be 1-20%.
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