CN115262241A - Surface treatment method of textile, special hyperchromic repairing agent and preparation method thereof - Google Patents
Surface treatment method of textile, special hyperchromic repairing agent and preparation method thereof Download PDFInfo
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- CN115262241A CN115262241A CN202210697490.XA CN202210697490A CN115262241A CN 115262241 A CN115262241 A CN 115262241A CN 202210697490 A CN202210697490 A CN 202210697490A CN 115262241 A CN115262241 A CN 115262241A
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- China
- Prior art keywords
- emulsion
- silicone oil
- fluorine
- amino silicone
- containing amino
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 230000000215 hyperchromic effect Effects 0.000 title claims abstract description 75
- 239000004753 textile Substances 0.000 title claims abstract description 74
- 238000004381 surface treatment Methods 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000000839 emulsion Substances 0.000 claims abstract description 204
- 229920013822 aminosilicone Polymers 0.000 claims abstract description 116
- 239000003921 oil Substances 0.000 claims abstract description 116
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 109
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 109
- 239000011737 fluorine Substances 0.000 claims abstract description 109
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 81
- 239000004744 fabric Substances 0.000 claims abstract description 80
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 73
- SOGFHWHHBILCSX-UHFFFAOYSA-J prop-2-enoate silicon(4+) Chemical compound [Si+4].[O-]C(=O)C=C.[O-]C(=O)C=C.[O-]C(=O)C=C.[O-]C(=O)C=C SOGFHWHHBILCSX-UHFFFAOYSA-J 0.000 claims abstract description 53
- 239000002994 raw material Substances 0.000 claims abstract description 21
- 238000011282 treatment Methods 0.000 claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000000576 coating method Methods 0.000 claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 11
- 238000007865 diluting Methods 0.000 claims abstract description 9
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 56
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 53
- 238000006243 chemical reaction Methods 0.000 claims description 48
- 239000003995 emulsifying agent Substances 0.000 claims description 47
- 238000010438 heat treatment Methods 0.000 claims description 47
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 41
- 238000002156 mixing Methods 0.000 claims description 39
- -1 polysiloxane Polymers 0.000 claims description 38
- 239000003999 initiator Substances 0.000 claims description 37
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 34
- 229920001296 polysiloxane Polymers 0.000 claims description 31
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 28
- 239000000178 monomer Substances 0.000 claims description 23
- 239000003054 catalyst Substances 0.000 claims description 21
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 21
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 21
- QTKPMCIBUROOGY-UHFFFAOYSA-N 2,2,2-trifluoroethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC(F)(F)F QTKPMCIBUROOGY-UHFFFAOYSA-N 0.000 claims description 20
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 20
- 229910052710 silicon Inorganic materials 0.000 claims description 20
- 239000010703 silicon Substances 0.000 claims description 20
- 238000004945 emulsification Methods 0.000 claims description 19
- 238000006116 polymerization reaction Methods 0.000 claims description 18
- 229960000583 acetic acid Drugs 0.000 claims description 17
- 239000012362 glacial acetic acid Substances 0.000 claims description 17
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 14
- 230000001804 emulsifying effect Effects 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 13
- 238000007720 emulsion polymerization reaction Methods 0.000 claims description 13
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 12
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 10
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 10
- DRRZZMBHJXLZRS-UHFFFAOYSA-N n-[3-[dimethoxy(methyl)silyl]propyl]cyclohexanamine Chemical compound CO[Si](C)(OC)CCCNC1CCCCC1 DRRZZMBHJXLZRS-UHFFFAOYSA-N 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 8
- 125000003118 aryl group Chemical group 0.000 claims description 8
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 7
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 7
- 150000002191 fatty alcohols Chemical class 0.000 claims description 7
- 230000009477 glass transition Effects 0.000 claims description 7
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 7
- 235000011152 sodium sulphate Nutrition 0.000 claims description 7
- 238000005507 spraying Methods 0.000 claims description 7
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 5
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 5
- 238000005086 pumping Methods 0.000 claims description 5
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 5
- KOJCPAMHGPVAEW-UHFFFAOYSA-N 2,4,6,8-tetraethyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound CC[SiH]1O[SiH](CC)O[SiH](CC)O[SiH](CC)O1 KOJCPAMHGPVAEW-UHFFFAOYSA-N 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 4
- KDJNNYXXPNIWGP-UHFFFAOYSA-N 2-methylprop-1-ene triethoxysilane Chemical compound C(C)O[SiH](OCC)OCC.C=C(C)C KDJNNYXXPNIWGP-UHFFFAOYSA-N 0.000 claims description 4
- CDOUZKKFHVEKRI-UHFFFAOYSA-N 3-bromo-n-[(prop-2-enoylamino)methyl]propanamide Chemical compound BrCCC(=O)NCNC(=O)C=C CDOUZKKFHVEKRI-UHFFFAOYSA-N 0.000 claims description 4
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 4
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 claims description 4
- 235000019329 dioctyl sodium sulphosuccinate Nutrition 0.000 claims description 4
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 claims description 4
- HTDJPCNNEPUOOQ-UHFFFAOYSA-N hexamethylcyclotrisiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O1 HTDJPCNNEPUOOQ-UHFFFAOYSA-N 0.000 claims description 4
- INJVFBCDVXYHGQ-UHFFFAOYSA-N n'-(3-triethoxysilylpropyl)ethane-1,2-diamine Chemical compound CCO[Si](OCC)(OCC)CCCNCCN INJVFBCDVXYHGQ-UHFFFAOYSA-N 0.000 claims description 4
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 claims description 4
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 claims description 4
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 4
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 4
- AMJQJHHAPXSEIZ-UHFFFAOYSA-N trimethyl-[[methylsilyloxy(diphenyl)silyl]oxy-diphenylsilyl]oxysilane Chemical compound C[SiH2]O[Si](O[Si](O[Si](C)(C)C)(C1=CC=CC=C1)C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1 AMJQJHHAPXSEIZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000003205 fragrance Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 33
- 238000005406 washing Methods 0.000 abstract description 20
- 229920000742 Cotton Polymers 0.000 description 25
- 230000006872 improvement Effects 0.000 description 24
- 238000005282 brightening Methods 0.000 description 23
- 238000012360 testing method Methods 0.000 description 19
- 229920000728 polyester Polymers 0.000 description 13
- 238000003756 stirring Methods 0.000 description 12
- 210000002268 wool Anatomy 0.000 description 8
- 239000003599 detergent Substances 0.000 description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- 238000013329 compounding Methods 0.000 description 6
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 6
- 239000000835 fiber Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 238000007605 air drying Methods 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000004040 coloring Methods 0.000 description 3
- 230000002354 daily effect Effects 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 238000009736 wetting Methods 0.000 description 3
- 244000025254 Cannabis sativa Species 0.000 description 2
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 description 2
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
- 235000009120 camo Nutrition 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 235000005607 chanvre indien Nutrition 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000007405 data analysis Methods 0.000 description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 description 2
- 239000000796 flavoring agent Substances 0.000 description 2
- 235000013355 food flavoring agent Nutrition 0.000 description 2
- 239000011487 hemp Substances 0.000 description 2
- 230000002045 lasting effect Effects 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 230000003020 moisturizing effect Effects 0.000 description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 2
- 230000000379 polymerizing effect Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000009864 tensile test Methods 0.000 description 2
- IRVZFACCNZRHSJ-UHFFFAOYSA-N 2,4,6,8-tetramethyl-2,4,6,8-tetraphenyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound O1[Si](C)(C=2C=CC=CC=2)O[Si](C)(C=2C=CC=CC=2)O[Si](C)(C=2C=CC=CC=2)O[Si]1(C)C1=CC=CC=C1 IRVZFACCNZRHSJ-UHFFFAOYSA-N 0.000 description 1
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical group OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 description 1
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 description 1
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 235000019568 aromas Nutrition 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 150000003141 primary amines Chemical class 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 230000036561 sun exposure Effects 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
- D06N3/128—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with silicon polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/46—Block-or graft-polymers containing polysiloxane sequences containing polyether sequences
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0086—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the application technique
- D06N3/0088—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the application technique by directly applying the resin
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0086—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the application technique
- D06N3/0088—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the application technique by directly applying the resin
- D06N3/009—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the application technique by directly applying the resin by spraying components on the web
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2209/00—Properties of the materials
- D06N2209/14—Properties of the materials having chemical properties
- D06N2209/141—Hydrophilic
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2209/00—Properties of the materials
- D06N2209/16—Properties of the materials having other properties
- D06N2209/1642—Hardnes
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Silicon Polymers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention relates to the technical field of textile surface treatment, and particularly discloses a textile surface treatment method, a special hyperchromic repairing agent and a preparation method thereof, wherein the textile surface treatment method comprises the following steps: preparing a hyperchromic repairing agent; diluting the hyperchromic repairing agent to obtain a surface treatment liquid; uniformly coating the surface of the textile fabric with the surface treatment liquid; drying the textile fabric subjected to coating treatment, wherein the temperature of the drying treatment is less than or equal to 60 ℃; the hyperchromic repairing agent comprises the following raw materials in parts by weight: 15-35 parts of fluorine-containing amino silicone oil emulsion, 10-50 parts of organic silicon acrylate emulsion and 20-70 parts of water. Correspondingly, the invention also provides a hyperchromic repairing agent and a preparation method thereof. The invention has the advantages of good color-enhancing and color-moistening effect, simple use method and good softness, hydrophilicity and washing resistance of the treated textile.
Description
Technical Field
The invention relates to the technical field of textile fabric treatment, in particular to a textile fabric surface treatment method, a special hyperchromic repairing agent and a preparation method thereof.
Background
A large number of textiles are used in everyday life, such as: clothes, home textiles, curtains and the like, which are bright in color just after purchase, but after a period of use, the textiles become light in color, yellow, old, dull due to exposure to factors such as sun exposure, oxidation and multiple scrubs, and it is difficult to renew and restore the original color of the textiles. In the prior art, an organic silicon deepening agent is used for treating a dyed fabric and then heating and baking the dyed fabric to form a film so as to reduce the reflection light quantity on the surface of the textile fabric, so that the textile fabric achieves a deep color effect. However, the organic silicon deepening agent not only has a complex synthesis process, but also can achieve the color-enhancing effect by heating in the surface treatment process. Meanwhile, the fabric treated by the organosilicon deepening agent has poor hydrophilicity.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a surface treatment method of textile fabric, which has good color enhancing and color moistening effects and simple use method, and the treated textile fabric has good softness, hydrophilicity and water washing resistance.
The technical problem to be solved by the invention is to provide a hyperchromic repairing agent and a preparation method thereof, which are environment-friendly, safe, good in hyperchromic and moisturizing effects, capable of enabling faded, light and yellow fabrics to increase the color, good in softness, hydrophilicity and water washing resistance, and suitable for textiles made of various materials.
In order to solve the technical problem, the invention provides a surface treatment method of a textile fabric, which comprises the following steps: preparing a hyperchromic repairing agent;
diluting the hyperchromic repairing agent to obtain a surface treatment solution;
uniformly coating the surface of the textile fabric with the surface treatment liquid;
drying the textile fabric subjected to coating treatment, wherein the temperature of the drying treatment is less than or equal to 60 ℃;
the hyperchromic repairing agent comprises the following raw materials in parts by weight:
15-35 parts of fluorine-containing amino silicone oil emulsion, 10-50 parts of organic silicon acrylate emulsion and 20-70 parts of water;
the fluorine-containing amino silicone oil emulsion is obtained by emulsifying fluorine-containing amino silicone oil;
the organic silicon acrylate emulsion is obtained by carrying out low-temperature polymerization reaction on acrylate, hydroxyl-terminated polysiloxane, a silane coupling agent, an emulsifier and an initiator, wherein the low-temperature polymerization reaction temperature is 70-90 ℃.
As an improvement of the scheme, the temperature of the drying treatment is 25-45 ℃.
As an improvement of the above scheme, the uniformly coating the surface of the textile fabric with the surface treatment liquid comprises: uniformly spraying the surface treatment liquid on the surface of the textile fabric;
alternatively, the textile is soaked in the surface treatment liquid.
As an improvement of the scheme, the fluorine-containing amino silicone oil comprises the following raw materials in parts by weight: 90-98 parts of organic silicon monomer, 1-6 parts of first silane coupling agent, 1-4 parts of trifluoroethyl methacrylate, 0.1-1 part of ammonium persulfate and 0.001-1 part of catalyst.
As an improvement of the scheme, the organic silicon monomer is one or more of octamethylcyclotetrasiloxane, alpha, omega-dihydroxy polydimethylsiloxane, hexamethylcyclotrisiloxane, tetramethyltetraphenyltetrasiloxane and tetraethylcyclotetrasiloxane;
the first silane coupling agent is one or more of gamma-aminopropyltriethoxysilane, 3-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, N-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane and gamma-diethylenetriamine propylmethyldimethoxysilane;
the catalyst is one or more of sodium hydroxide, potassium hydroxide, lithium hydroxide and tetramethyl ammonium hydroxide.
As an improvement of the scheme, the fluorine-containing amino silicone oil is prepared by the following method:
mixing an organic silicon monomer and a first silane coupling agent, heating, adding a catalyst, continuously heating, keeping the temperature for a preset time, and cooling;
adding trifluoroethyl methacrylate and ammonium persulfate, and reacting to obtain the fluorine-containing amino silicone oil.
As an improvement of the scheme, the fluorine-containing amino silicone oil emulsion is obtained by adding a first emulsifier, glacial acetic acid and water into the fluorine-containing amino silicone oil for reaction, and the adding mass ratio of the fluorine-containing amino silicone oil emulsion, the first emulsifier, the glacial acetic acid and the water is (20-35): (2-8): (0.05-2): (60-85).
As an improvement of the scheme, the first emulsifier is one or more of fatty alcohol-polyoxyethylene ether and dioctyl sodium sulfosuccinate.
As an improvement of the scheme, the organic silicon acrylate emulsion comprises the following raw materials in parts by weight:
20 to 30 portions of acrylic ester, 3 to 10 portions of hydroxyl terminated polysiloxane, 0.1 to 5 portions of second silane coupling agent, 1 to 5 portions of second emulsifier, 0.5 to 5 portions of initiator and 50 to 78 portions of water.
Preferably, the acrylate comprises one or more of methyl acrylate, butyl acrylate, methyl methacrylate and glycidyl methacrylate;
the second silane coupling agent comprises one or more of vinyl triethoxysilane, aminoethyl aminopropyl trimethoxysilane, isobutylene triethoxysilane, 3-aminopropyl triethoxysilane and gamma-diethylenetriamine propyl methyldimethoxysilane;
the second emulsifier comprises one or more of fatty alcohol-polyoxyethylene ether, nonylphenol polyoxyethylene ether and fatty alcohol ether sodium sulfate;
the initiator comprises one or more of sodium persulfate, potassium persulfate and ammonium persulfate.
As an improvement of the scheme, the organic silicon acrylate emulsion is prepared by the following method:
mixing acrylate, hydroxyl-terminated polysiloxane, a second silane coupling agent, a second emulsifier and water for pre-emulsification to obtain a pre-emulsion;
mixing part of the pre-emulsion with an initiator and water, heating and carrying out seed emulsion polymerization to obtain seed emulsion;
and dropwise adding the rest pre-emulsion and the initiator into the seed emulsion, adjusting the reaction temperature and preserving the heat after the dropwise adding is finished, and obtaining the organic silicon acrylate emulsion after the reaction is completed.
As an improvement of the scheme, the particle size of the organosilicon acrylic ester emulsion is 400 nm-800 nm;
the glass transition temperature of the acrylic ester is-70 ℃ to 0 ℃.
As an improvement of the scheme, the hyperchromic restoration agent also comprises a fragrant agent; based on the hyperchromic restoration agent, the adding amount of the aromatic is 0.2-0.8 part.
On the other hand, the invention also provides a special hyperchromic repairing agent for surface treatment of textiles, which comprises the following raw materials in parts by weight:
15-35 parts of fluorine-containing amino silicone oil emulsion, 10-50 parts of organic silicon acrylate emulsion and 20-70 parts of water;
the fluorine-containing amino silicone oil emulsion is obtained by emulsifying fluorine-containing amino silicone oil;
the organic silicon acrylate emulsion is obtained by carrying out low-temperature polymerization reaction on acrylate, hydroxyl-terminated polysiloxane, a silane coupling agent, an emulsifier and an initiator, wherein the low-temperature polymerization reaction temperature is 70-90 ℃.
As an improvement of the scheme, the fluorine-containing amino silicone oil comprises the following raw materials in parts by weight: 90 to 98 parts of organic silicon monomer, 1 to 6 parts of first silane coupling agent, 1 to 4 parts of trifluoroethyl methacrylate, 0.1 to 1 part of ammonium persulfate and 0.001 to 1 part of catalyst.
As an improvement of the scheme, the organic silicon monomer is one or more of octamethylcyclotetrasiloxane, alpha, omega-dihydroxy polydimethylsiloxane, hexamethylcyclotrisiloxane, tetramethyltetraphenylcyclotetrasiloxane and tetraethylcyclotetrasiloxane;
the first silane coupling agent is one or more of gamma-aminopropyltriethoxysilane, 3-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, N-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane and gamma-diethylenetriamine propylmethyldimethoxysilane;
the catalyst is one or more of sodium hydroxide, potassium hydroxide, lithium hydroxide and tetramethyl ammonium hydroxide.
As an improvement of the scheme, the fluorine-containing amino silicone oil is prepared by the following method:
mixing an organic silicon monomer and a first silane coupling agent, heating, adding a catalyst, continuously heating, keeping the temperature for a preset time, and cooling;
adding trifluoroethyl methacrylate and ammonium persulfate, and reacting to obtain the fluorine-containing amino silicone oil.
As an improvement of the scheme, the fluorine-containing amino silicone oil emulsion is obtained by adding a first emulsifier, glacial acetic acid and water into the fluorine-containing amino silicone oil for reaction, and the adding mass ratio of the fluorine-containing amino silicone oil emulsion to the first emulsifier to the glacial acetic acid to the water is (20-35): (2-8): (0.05-2): (60-85).
As an improvement of the scheme, the first emulsifier is one or more of fatty alcohol-polyoxyethylene ether and dioctyl sodium sulfosuccinate.
As an improvement of the scheme, the organosilicon acrylate emulsion comprises the following raw materials in parts by weight:
20 to 30 portions of acrylic ester, 3 to 10 portions of hydroxyl terminated polysiloxane, 0.1 to 5 portions of second silane coupling agent, 1 to 5 portions of second emulsifier, 0.5 to 5 portions of initiator and 50 to 78 portions of water.
Preferably, the acrylate comprises one or more of methyl acrylate, butyl acrylate, methyl methacrylate and glycidyl methacrylate;
the second silane coupling agent comprises one or more of vinyl triethoxysilane, aminoethyl aminopropyl trimethoxysilane, isobutylene triethoxysilane, 3-aminopropyl triethoxysilane and gamma-diethylenetriamine propyl methyldimethoxysilane;
the second emulsifier comprises one or more of fatty alcohol-polyoxyethylene ether, nonylphenol polyoxyethylene ether and fatty alcohol ether sodium sulfate;
the initiator comprises one or more of sodium persulfate, potassium persulfate and ammonium persulfate.
As an improvement of the scheme, the organic silicon acrylate emulsion is prepared by the following method:
mixing acrylate, hydroxyl-terminated polysiloxane, a second silane coupling agent, a second emulsifier and water for pre-emulsification to obtain a pre-emulsion;
mixing part of the pre-emulsion with an initiator and water, heating and carrying out seed emulsion polymerization to obtain seed emulsion;
and dropwise adding the rest pre-emulsion and the initiator into the seed emulsion, adjusting the reaction temperature and preserving the heat after the dropwise adding is finished, and obtaining the organic silicon acrylate emulsion after the reaction is completed.
As an improvement of the scheme, the particle size of the organic silicon acrylate emulsion is 400 nm-800 nm;
the glass transition temperature of the acrylate is-70 ℃ to 0 ℃.
As an improvement of the scheme, the hyperchromic restoration agent also comprises a flavoring agent; based on the hyperchromic restoration agent, the adding amount of the aromatic is 0.2-0.8 part.
Correspondingly, the invention also provides a preparation method of the hyperchromic restoration agent, which comprises the following steps:
(1) Preparing fluorine-containing amino silicone oil;
(2) Emulsifying the fluorine-containing amino silicone oil to obtain fluorine-containing amino silicone oil emulsion;
(3) Preparing organic silicon acrylate emulsion;
(4) According to the weight portion, 15 to 25 portions of the fluorine-containing amino silicone oil emulsion, 30 to 50 portions of the organic silicon acrylate emulsion and 20 to 70 portions of water are mixed to obtain a finished product.
As an improvement of the above scheme, the step (1) comprises:
mixing an organic silicon monomer and a first silane coupling agent, heating to 75-85 ℃, adding a catalyst, continuously heating to 130-135 ℃, keeping the temperature for 3-5 h, heating to 140-145 ℃, vacuumizing to low boiling, stopping vacuumizing when the viscosity reaches a preset value, and cooling to 80-85 ℃;
adding trifluoroethyl methacrylate and ammonium persulfate, and reacting for 2-3 hours to obtain the fluorine-containing amino silicone oil.
As an improvement of the scheme, the step (2) comprises the following steps:
firstly, mixing the fluorine-containing amino silicone oil, a first emulsifier and glacial acetic acid to obtain a first mixed solution;
and dropwise adding water into the first mixed solution, and uniformly mixing to obtain the fluorine-containing amino silicone oil emulsion.
As an improvement of the above scheme, the step (3) comprises:
mixing acrylate, hydroxyl-terminated polysiloxane, a second silane coupling agent, a second emulsifier and water for pre-emulsification to obtain a pre-emulsion;
mixing 20-40% of the pre-emulsion with an initiator and water, heating to 70-90 ℃, and carrying out seed emulsion polymerization reaction for 8-20 min to obtain seed emulsion;
and dropwise adding the rest 60-80% of pre-emulsion and initiator into the seed emulsion, adjusting the reaction temperature to 80-90 ℃ after dropwise adding is finished, keeping the temperature for 3-5 h, and adjusting the pH value of the reaction system after complete reaction to obtain the organic silicon acrylate emulsion.
The implementation of the invention has the following beneficial effects:
1. the surface treatment method of the textile fabrics provided by the invention is characterized in that the hyperchromic repairing agent is diluted and then uniformly sprayed or coated on the surface of the textile fabrics, and the hyperchromic repairing agent has low-temperature film-forming property, so that the textile fabrics are naturally dried or aired at the medium and low temperature lower than 60 ℃, and the hyperchromic and hyperchromic effects of the textile fabrics can be realized. The color of the fabric after natural air drying or airing is deepened and brightened, the fabric has soft hand feeling, the color fixing effect is lasting, and the washing resistance is excellent.
2. The hyperchromic repairing agent used by the invention is prepared by compounding fluorine-containing amino silicone oil emulsion and organic silicon acrylate emulsion. Wherein, the fluorine-containing amino silicone oil emulsion has low refractive index, good hand feeling softness and darkening and brightening effects. The organic silicon acrylate emulsion has good darkening and brightening effects, low-temperature film-forming property and good hydrophilicity. The two are compounded, so that excellent hyperchromic and hyperchromic effects can be obtained, the treated fabric has better color saturation, the color is more vivid, and the fabric also has good softness, hydrophilicity and water washing resistance.
Moreover, the color-increasing repairing agent not only has good color-increasing and color-moistening effects on daily clothes, but also can re-increase the color and brighten aiming at the long-term used fabrics which are seriously faded and become light and yellow, and has ideal color-moistening and repairing effects. The fabric is suitable for textile fabrics made of various materials, including but not limited to cotton, hemp, wool, silk and chemical fiber fabrics, is friendly to human body and environment, is environment-friendly and safe, and is suitable for various underclothes.
3. The hyperchromic repairing agent provided by the invention is simple in preparation method and low in cost, only the fluorine-containing amino silicone oil emulsion and the organic silicon acrylate emulsion are required to be mixed with water, and the process controllability is strong.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below.
The invention provides a surface treatment method of textile fabrics, which comprises the following steps:
(1) Preparing a hyperchromic repairing agent;
(2) Diluting the hyperchromic repairing agent to obtain a surface treatment solution;
(3) Uniformly coating the surface of the textile fabric with the surface treatment liquid;
(4) And drying the coated textile fabric, wherein the temperature of the drying treatment is less than or equal to 60 ℃.
The hyperchromic repairing agent comprises the following raw materials in parts by weight:
15-35 parts of fluorine-containing amino silicone oil emulsion, 10-50 parts of organic silicon acrylate emulsion and 20-70 parts of water;
the fluorine-containing amino silicone oil emulsion is obtained by emulsifying fluorine-containing amino silicone oil;
the organic silicon acrylate emulsion is obtained by carrying out low-temperature polymerization reaction on acrylate, hydroxyl-terminated polysiloxane, a silane coupling agent, an emulsifier and an initiator, wherein the low-temperature polymerization reaction temperature is 70-90 ℃.
Preferably, the hyperchromic restoration agent comprises the following raw materials in parts by weight: 17-23 parts of fluorine-containing amino silicone oil emulsion, 35-45 parts of organic silicon acrylate emulsion and 30-60 parts of water.
Preferably, the hyperchromic restoration agent comprises the following raw materials in parts by weight: 18-22 parts of fluorine-containing amino silicone oil emulsion, 38-42 parts of organic silicon acrylate emulsion and 35-50 parts of water.
The present invention is one kind of organosilicon acrylate polymerizing emulsion in milky blue color. By compounding the fluorine-containing amino silicone oil emulsion and the organic silicon acrylate emulsion in a specific ratio, faded, lightened and yellowish fabrics can be enhanced and brightened, moisturized and repaired and soft in hand feeling. The fluorine-containing amino silicone oil emulsion has soft and smooth hand feeling, can improve the hand feeling comfort of fabrics, and has good deepening effect, but has poor hydrophilic effect. The organosilicon acrylate polymerized emulsion has the advantages of hard hand feeling, obvious deepening effect, good low-temperature film forming property and better hydrophilic effect, and plays a role in determining the washability of fabrics. The hyperchromic repairing agent of the invention has the advantages of soft hand feeling, good hydrophilicity, good hyperchromic and moisturizing effects, water washing resistance and the like.
The surface treatment method of the textile fabrics comprises the steps of diluting the hyperchromic repairing agent, and then uniformly spraying or coating the hyperchromic repairing agent on the surfaces of the textile fabrics, wherein the hyperchromic repairing agent has low-temperature film-forming property, and the textile fabrics subjected to coating treatment are dried at the temperature of less than or equal to 60 ℃, so that the hyperchromic and hyperchromic properties of the textile fabrics can be realized. Preferably, the temperature of the drying treatment is 25 to 45 ℃. More preferably, the temperature of the drying treatment is 25 to 35 ℃.
The surface treatment solution can be uniformly applied to the surface of the textile fabric in various embodiments, including but not limited to: uniformly spraying the surface treatment liquid on the surface of the textile fabric; alternatively, the textile is soaked in the surface treatment liquid.
The detailed explanation of the hyperchromic restoration agent is that the fluorine-containing amino silicone oil emulsion is obtained by emulsifying fluorine-containing amino silicone oil.
In the prior art, amino silicone oil is generally directly used for the after-finishing of cotton fabrics, and the fabrics can be endowed with smooth hand feeling. However, in the present invention, by using the fluorochemical silicone oil emulsion, on the one hand, the polysiloxane backbone with amino groups can form a film on the fiber surface, thereby imparting excellent softness to the fiber. On the other hand, emulsion obtained by emulsifying the fluorine-containing amino silicone oil has low refractive index, so that good darkening and brightening effects are obtained.
Preferably, the fluorine-containing amino silicone oil comprises the following raw materials in parts by weight: 90 to 98 parts of organic silicon monomer, 1 to 6 parts of first silane coupling agent, 1 to 4 parts of trifluoroethyl methacrylate, 0.1 to 1 part of ammonium persulfate and 0.001 to 1 part of catalyst.
Preferably, the organosilicon monomer is one or more of octamethylcyclotetrasiloxane, alpha, omega-dihydroxypolydimethylsiloxane, hexamethylcyclotrisiloxane, tetramethyltetraphenyltetrasiloxane and tetraethylcyclotetrasiloxane;
the first silane coupling agent is one or more of gamma-aminopropyltriethoxysilane, 3-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, N-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane and gamma-diethylenetriamine propylmethyldimethoxysilane;
the catalyst is one or more of sodium hydroxide, potassium hydroxide, lithium hydroxide and tetramethyl ammonium hydroxide.
Conventional amino silicone oils are generally selected from silane coupling agents whose side chain is a secondary amine, and are polymerized in a proportion of low ammonia value. The cotton fabric treated by the traditional amino silicone oil emulsion is very easy to generate yellowing and color change in the shaping high-temperature baking process. The invention selects polyamine silane coupling agent with side chain as primary ammonia, and carries out polymerization reaction according to the proportion of medium-high ammonia value to polymerize into organosilicon high molecular compound; and adding trifluoroethyl methacrylate and ammonium persulfate to obtain the fluorine-containing amino silicone oil, wherein the hand feeling is softer, and primary amine is easily oxidized into a chromophoric group to develop color.
More preferably, the fluorine-containing amino silicone oil comprises the following raw materials in parts by weight: 90-95 parts of organic silicon monomer, 1-5 parts of first silane coupling agent, 2-3 parts of trifluoroethyl methacrylate, 0.1-1 part of ammonium persulfate and 0.001-1 part of catalyst.
Preferably, the first silane coupling agent is gamma-diethylenetriamine propyl-methyldimethoxysilane, so that the fabric has the characteristics of softness, smoothness, fluffiness, high elasticity and the like, and can play a good role in various fabrics such as cotton, hemp, wool, silk, chemical fiber fabrics and the like.
Further, the fluorine-containing amino silicone oil is prepared by the following method:
mixing an organic silicon monomer and a first silane coupling agent, heating, adding a catalyst, continuously heating, keeping the temperature for a preset time, and cooling;
adding trifluoroethyl methacrylate and ammonium persulfate, and reacting to obtain the fluorine-containing amino silicone oil.
Preferably, the fluorine-containing amino silicone oil is prepared by the following method:
mixing 90-98 parts of organic silicon monomer and 1-6 parts of first silane coupling agent according to parts by weight, heating, adding 0.001-1 part of catalyst, continuing to heat, keeping the temperature for preset time, cooling, adding 1-4 parts of trifluoroethyl methacrylate and 0.1-1 part of ammonium persulfate, and reacting for 2-3 hours to obtain the transparent viscous fluorine-containing amino silicone oil.
More preferably, the fluorine-containing amino silicone oil is prepared by the following method:
mixing 90-98 parts by weight of organic silicon monomer and 1-6 parts by weight of first silane coupling agent, heating to 75-85 ℃, adding 0.001-1 part by weight of catalyst, continuously heating to 130-135 ℃, keeping the temperature for 3-5 h, heating to 140-145 ℃, vacuumizing to low boiling, stopping vacuumizing when the viscosity reaches a preset value, and cooling to 80-85 ℃;
adding 1-4 parts of trifluoroethyl methacrylate and 0.1-1 part of ammonium persulfate, and reacting for 2-3 hours to obtain the transparent viscous fluorine-containing amino silicone oil.
The first emulsifier, glacial acetic acid and water are added into the fluorine-containing amino silicone oil, the fluorine-containing amino silicone oil is dispersed and emulsified at high speed by the emulsifier, and the amino silicone oil in the fluorine-containing amino silicone oil emulsion is uniformly dispersed in the water to form a stable micromolecule emulsion system, so that the fluorine-containing amino silicone oil emulsion with low refractive index is obtained.
The adding mass ratio of the fluorine-containing amino silicone oil emulsion, the first emulsifier, the glacial acetic acid and the water is preferably (20-35): (2-8): (0.05-2): (60-85). The first emulsifier is preferably one or more of fatty alcohol-polyoxyethylene ether and dioctyl sodium sulfosuccinate. The fatty alcohol-polyoxyethylene ether may further be preferably C10 branched fatty alcohol-polyoxyethylene ether, C12 straight-chain fatty alcohol-polyoxyethylene ether, or C13 branched fatty alcohol-polyoxyethylene ether, but is not limited thereto.
In the emulsification process, the invention controls the dropping speed of the reaction monomer and the catalyst by selecting the emulsifier and setting the emulsification proportion, so that the reaction is carried out smoothly, and the stability of the emulsion and the effects of darkening and brightening are ensured. Preferably, the fatty alcohol-polyoxyethylene ether with the HLB value of 12-15 and the fatty alcohol-polyoxyethylene ether with the HLB value of 6-9.5 are selected for compounding, and the two emulsifiers with high HLB value and low HLB value are matched for emulsification at a high emulsification ratio, so that the stability of the emulsion can be better ensured, and the darkening and brightening effects and the color fixing effects are further improved.
The organic silicon acrylate emulsion is obtained by carrying out low-temperature polymerization reaction on acrylate, hydroxyl-terminated polysiloxane, a silane coupling agent, an emulsifier and an initiator, wherein the low-temperature polymerization reaction temperature is 70-90 ℃.
Preferably, the silicone acrylate emulsion comprises the following raw materials in parts by weight:
20 to 30 portions of acrylic ester, 3 to 10 portions of hydroxyl terminated polysiloxane, 0.1 to 5 portions of second silane coupling agent, 1 to 5 portions of second emulsifier, 0.5 to 5 portions of initiator and 50 to 78 portions of water.
Wherein the acrylate comprises one or more of methyl acrylate, butyl acrylate, methyl methacrylate and glycidyl methacrylate;
the second silane coupling agent comprises one or more of vinyl triethoxysilane, aminoethyl aminopropyl trimethoxysilane, isobutylene triethoxysilane, 3-aminopropyl triethoxysilane and gamma-diethylenetriamine propyl methyldimethoxysilane;
the second emulsifier comprises one or more of fatty alcohol-polyoxyethylene ether, nonylphenol polyoxyethylene ether and fatty alcohol ether sodium sulfate;
the initiator comprises one or more of sodium persulfate, potassium persulfate and ammonium persulfate.
Specifically, the acrylate contains an unsaturated double bond and can be bonded with a silane coupling agent containing an unsaturated group. The acrylate is an ideal material with low refractive index, has strong darkening and brightening effects, is easy to form a film and has good fastness. The hydroxyl-terminated siloxane can be grafted with a silane coupling agent to form a long chain, so that the softness of the emulsion is improved. The silane coupling agent has hydroxyl and double bonds, can be combined with siloxane and acrylate, and grafts the polysiloxane to the acrylate side chain. And the emulsifier is used for uniformly dispersing the acrylate monomer in the form of monomer beads in water. And the initiator is a carrier for mutually polymerizing the acrylate, the hydroxyl-terminated siloxane and the silane coupling agent.
The existing organosilicon acrylic ester emulsion is mostly applied to the fields of coatings, printing ink and industrial paint. According to the invention, the acrylate, the hydroxyl-terminated polysiloxane and the silane coupling agent are synthesized into the linear-chain high-molecular compound, so that when the hyperchromic repairing agent is used, a film can be formed on the emulsion under the condition of normal-temperature air drying without high-temperature baking, and the improvement of the washability is facilitated. Meanwhile, the amino group of the fluorine-containing amino silicone oil can form firmer grabbing force with cellulose fibers, so that the color fixing effect is improved, and the darkening and brightening effects are more durable. The existing clothes repairing agent can not form a film at low temperature and has good washability.
Preferably, the glass transition temperature of the acrylate is-70 ℃ to 0 ℃. More preferably, the glass transition temperature of the acrylate is-30 ℃ to-60 ℃. According to the organic silicon acrylate polymerization emulsion, the acrylate with a lower glass transition temperature is selected, the film forming temperature of the emulsion can be reduced after polymerization, the emulsion is more suitable for household products, the emulsion is formed into a film under the normal-temperature air drying condition, and the washability is improved.
Preferably, the silicone acrylate emulsion is prepared by the following method:
firstly, mixing acrylate, hydroxyl-terminated polysiloxane, a second silane coupling agent, a second emulsifier and water for pre-emulsification to obtain pre-emulsion;
mixing part of the pre-emulsion with an initiator and water, heating and carrying out seed emulsion polymerization to obtain seed emulsion;
and dropwise adding the rest pre-emulsion and the initiator into the seed emulsion, adjusting the reaction temperature and preserving the heat after the dropwise adding is finished, and obtaining the organic silicon acrylate emulsion after the reaction is completed.
More preferably, the silicone acrylate emulsion is prepared by the following method:
firstly, mixing 20-30 parts of acrylate, 3-10 parts of hydroxyl terminated polysiloxane, 0.4-3 parts of second silane coupling agent, 1-2 parts of second emulsifier and water for pre-emulsification to obtain pre-emulsion;
mixing 20-40% of the pre-emulsion with an initiator and 50-78 parts of water, heating to 70-90 ℃, and carrying out seed emulsion polymerization reaction for 8-20 min to obtain seed emulsion;
and (3) dropwise adding the residual 60-80% of pre-emulsion and initiator into the seed emulsion, adjusting the reaction temperature to 80-90 ℃ after dropwise adding, keeping the temperature for 3-5 h, and adjusting the pH of the reaction system to 6-7 after complete reaction to obtain the organic silicon acrylate emulsion.
Wherein the particle size of the organosilicon acrylic ester emulsion is preferably 400 nm-800 nm. Through a large number of experiments, the particle size of emulsion molecules has a certain relationship with brightening and brightening but has no linear relationship. When the particle size of the organic silicon acrylate emulsion is controlled between 400nm and 800nm, the organic silicon acrylate emulsion with excellent stability, darkening and brightening can be obtained.
As a best mode of carrying out the invention, the emulsion polymerization of silicone acrylates requires a comprehensive control of the following factors:
(1) Controlling the particle size of emulsion molecules to improve the darkening and brightening effects;
(2) The glass transition temperature and the synthesis ratio of different reaction materials are controlled to reduce the film forming temperature of the polymerized emulsion and improve the darkening and brightening effects;
(3) The technological parameters of the polymerization reaction are controlled to change, so that the stability of the emulsion is improved, the darkening and brightening effects are improved, and the film forming temperature is reduced.
Through the control of the three factors, the emulsion stability is greatly improved, the darkening and brightening effects are improved, the film can be formed at normal temperature, the fastness is good, the daily washing fastness test is met, and the darkening and brightening uniformity of various parts of clothes can be ensured.
Correspondingly, the invention also provides a special hyperchromic repairing agent for surface treatment of textiles, which comprises the following raw materials in parts by weight:
15-35 parts of fluorine-containing amino silicone oil emulsion, 10-50 parts of organic silicon acrylate emulsion and 20-70 parts of water;
the fluorine-containing amino silicone oil emulsion is obtained by emulsifying fluorine-containing amino silicone oil;
the organic silicon acrylate emulsion is obtained by carrying out low-temperature polymerization reaction on acrylate, hydroxyl-terminated polysiloxane, a silane coupling agent, an emulsifier and an initiator, wherein the low-temperature polymerization reaction temperature is 70-90 ℃.
It should be noted that the technical details of the hyperchromic repair agent are the same as those described above, and are not described herein again.
Further, the color-enhancing repairing agent can also comprise other auxiliary agents, such as a flavoring agent, but not limited to the above. Based on the hyperchromic repairing agent, the adding amount of the aromatic is 0.2-0.8 part, and the aromatic can emit different aromas, and has the effects of removing peculiar smell, refreshing and purifying clothes odor and perfuming.
When in use, the hyperchromic restoration agent is diluted and then uniformly sprayed on the fabric to be restored and then naturally dried, or the fabric to be processed is soaked in the dilution of the hyperchromic restoration agent, and naturally dried after moisture is removed. After the old clothes are simply and naturally air-dried by the product, the color deepening and brightening effects are remarkable, the color is bright and new instantly, the clothes are endowed with softer and more comfortable handfeel and better color fixing effect, the water washing resistance is excellent, more importantly, the product is friendly and safe to human body and environment, is suitable for various close-fitting clothes, and simultaneously meets the export standard of European and American safety and environmental protection.
Correspondingly, the invention also provides a preparation method of the hyperchromic repairing agent, which comprises the following steps:
(1) Preparing fluorine-containing amino silicone oil;
preferably, step (1) comprises:
mixing an organic silicon monomer and a first silane coupling agent, heating to 75-85 ℃, adding a catalyst, continuously heating to 130-135 ℃, keeping the temperature for 3-5 hours, heating to 140-145 ℃, performing vacuum pumping for low boiling, stopping the vacuum pumping when the viscosity reaches a preset value, and cooling to 80-85 ℃;
adding trifluoroethyl methacrylate and ammonium persulfate, and reacting for 2-3 hours to obtain the fluorine-containing amino silicone oil.
More preferably, step (1) comprises:
mixing 90-98 parts of organic silicon monomer and 1-6 parts of first silane coupling agent according to parts by weight, heating to 75-85 ℃, adding 0.001-1 part of catalyst, continuously heating to 130-135 ℃, keeping the temperature for 3-5 h, heating to 140 ℃, vacuumizing to low boiling, stopping vacuumizing when the viscosity reaches 12000-15000 mps, and cooling to 82-85 ℃;
adding 1-4 parts of trifluoroethyl methacrylate and 0.1-1 part of ammonium persulfate, and reacting for 2-3 hours to obtain the transparent viscous fluorine-containing amino silicone oil.
(2) Emulsifying the fluorine-containing amino silicone oil to obtain fluorine-containing amino silicone oil emulsion;
preferably, step (2) comprises:
firstly, mixing the fluorine-containing amino silicone oil, a first emulsifier and glacial acetic acid to obtain a first mixed solution;
and dropwise adding water into the first mixed solution, and uniformly mixing to obtain the fluorine-containing amino silicone oil emulsion.
More preferably, the step (2) comprises:
adding 2-5 parts of first emulsifier and 0.05-0.1 part of glacial acetic acid into 20-30 parts of fluorine-containing amino silicone oil, and mixing to obtain a first mixed solution;
and (3) dropwise adding 65-85 parts of water into the first mixed solution, and uniformly mixing to obtain the fluorine-containing amino silicone oil emulsion, wherein the dropwise adding speed of the water is 0.5-0.8 part/min.
(3) Preparing organic silicon acrylate emulsion;
preferably, step (3) comprises:
mixing acrylate, hydroxyl-terminated polysiloxane, a second silane coupling agent, a second emulsifier and water for pre-emulsification to obtain a pre-emulsion;
mixing 20-40% of the pre-emulsion with an initiator and water, heating to 70-90 ℃, and carrying out seed emulsion polymerization reaction for 8-20 min to obtain seed emulsion;
and (3) dropwise adding the residual 60-80% of pre-emulsion and initiator into the seed emulsion, adjusting the reaction temperature to 80-90 ℃ after dropwise adding, keeping the temperature for 3-5 h, and adjusting the pH of the reaction system after complete reaction to obtain the organic silicon acrylate emulsion.
More preferably, step (3) comprises:
firstly, mixing 20-30 parts of acrylate, 3-10 parts of hydroxyl terminated polysiloxane, 0.4-3 parts of second silane coupling agent, 1-2 parts of second emulsifier and water for pre-emulsification to obtain pre-emulsion;
mixing 20-40% of the pre-emulsion with an initiator and 50-78 parts of water, heating to 70-90 ℃, and carrying out seed emulsion polymerization reaction for 8-20 min to obtain seed emulsion;
and dropwise adding the rest 60-80% of pre-emulsion and initiator into the seed emulsion, adjusting the reaction temperature to 80-90 ℃ after dropwise adding, keeping the temperature for 3-5 h, and adjusting the pH of the reaction system to 6-7 after complete reaction to obtain the organic silicon acrylate emulsion, wherein the particle size of the organic silicon acrylate emulsion is 400-800 nm.
(4) According to the weight portion, 15 to 25 portions of the fluorine-containing amino silicone oil emulsion, 30 to 50 portions of the organic silicon acrylate emulsion and 20 to 70 portions of water are mixed to obtain a finished product.
The hyperchromic repairing agent provided by the invention is simple in preparation method and low in cost, only the fluorine-containing amino silicone oil emulsion and the organic silicon acrylate emulsion are required to be mixed with water, and the process controllability is strong.
The invention is further illustrated by the following specific examples:
example 1
The embodiment provides a surface treatment method of textile fabric, which comprises the following steps:
1. preparing hyperchromic repairing agent
1. Preparing the fluorine-containing amino silicone oil:
adding 97kg of octamethylcyclotetrasiloxane and 2.8kg of gamma-glycidoxypropyltrimethoxysilane into a reaction kettle, heating to 90 ℃, adding 0.2kg of tetramethylammonium hydroxide, heating to 135 ℃, keeping the temperature for 4 hours, heating to 140 ℃, vacuumizing, and pumping out the oligomer. And cooling to 82 ℃, adding 1.8kg of trifluoroethyl methacrylate and 0.2kg of ammonium persulfate, and reacting for 2-3 hours to obtain the transparent viscous fluorine-containing amino silicone oil.
2. Emulsifying the fluorine-containing amino silicone oil to obtain a fluorine-containing amino silicone oil emulsion:
adding 25kg of fluorine-containing amino silicone oil, 5kg of fatty alcohol-polyoxyethylene ether and 0.5kg of glacial acetic acid into a reaction kettle, uniformly stirring, adding 69.5kg of water into a dropwise adding tank, slowly dropwise adding, slowly diluting the emulsion from a thick substance in the dropwise adding process, standing for defoaming when the emulsion is milky white after the water is completely added, and filtering and discharging to obtain the fluorine-containing amino silicone oil emulsion.
3. Preparing an organic silicon acrylate emulsion:
adding 22kg of acrylic acid-2-hydroxyethyl, 6kg of hydroxyl-terminated siloxane, 2kg of vinyl triethoxysilane and 1g of fatty alcohol ether sodium sulfate into a dripping tank, starting stirring for pre-emulsification, and when the emulsion is milky and is not layered, indicating that the pre-emulsification is finished to obtain pre-emulsion;
putting 30% of the pre-emulsion into a reaction kettle, adding 0.6kg of ammonium persulfate and 68.4 parts of deionized water, heating to 80 ℃ for seed emulsion polymerization, and obtaining seed emulsion after 10 min;
and (3) dropwise adding the remaining 70% of pre-emulsion and 1.4kg of ammonium persulfate into the seed emulsion, after finishing dropwise adding for 2 hours, adjusting the reaction temperature to 85 ℃, continuing to react for 4 hours, and after complete reaction, adjusting the pH value to 6-7 to obtain the blue-emitting white organic silicon acrylate emulsion.
4. Compounding:
adding 40kg of water into a reaction kettle, adding 0.3kg of aromatic, uniformly stirring, adding 15kg of fluorine-containing amino silicone oil emulsion and 44.7kg of organic silicon acrylate emulsion, and uniformly stirring to obtain a finished product.
2. Diluting the hyperchromic repairing agent, wherein the ratio of hyperchromic repairing agent/water is 1: mixing the components in a ratio of 20 times to obtain surface treatment liquid;
3. uniformly spraying the surface treatment liquid on the surface of the textile fabric;
4. and (3) naturally drying the sprayed or soaked textile at room temperature.
Example 2
The embodiment provides a surface treatment method of textile fabric, which comprises the following steps:
1. preparing hyperchromic repairing agent
1. Preparing the fluorine-containing amino silicone oil:
adding 98kg of tetramethyltetraphenyltetrasiloxane and 1.8kg of N-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane into a reaction kettle, heating to 90 ℃, adding 0.2kg of potassium hydroxide, heating to 135 ℃, keeping the temperature for 5 hours, heating to 140 ℃, vacuumizing, and extracting an oligomer. And (3) cooling to 83 ℃, adding 1.5kg of trifluoroethyl methacrylate and 0.3kg of ammonium persulfate, and reacting for 2.5 hours to obtain the transparent viscous fluorine-containing amino silicone oil.
2. Emulsifying the fluorine-containing amino silicone oil to obtain a fluorine-containing amino silicone oil emulsion:
adding 30kg of fluorine-containing amino silicone oil, 6kg of fatty alcohol-polyoxyethylene ether and 0.6kg of glacial acetic acid into a reaction kettle, uniformly stirring, adding 63.4kg of water into a dropwise adding tank, slowly dropwise adding, slowly thinning the emulsion from a thick substance in the dropwise adding process, standing for defoaming when the emulsion is milky white after the water is completely added, and filtering and discharging to obtain the fluorine-containing amino silicone oil emulsion.
3. Preparing an organic silicon acrylate emulsion:
adding 24kg of butyl acrylate, 3kg of hydroxyl-terminated siloxane, 2kg of vinyl triethoxysilane and 1kg of fatty alcohol ether sodium sulfate into a dripping tank, starting stirring for pre-emulsification, and when the emulsion is milky white and does not layer, indicating that the pre-emulsification is finished to obtain pre-emulsion;
putting 30% of the pre-emulsion into a reaction kettle, adding 0.3kg of ammonium persulfate and 68.4kg of deionized water, heating to 80 ℃ for seed emulsion polymerization, and obtaining seed emulsion after 10 min;
and (3) dropwise adding the residual 70% of pre-emulsion and 0.7kg of initiator into the seed emulsion, adjusting the reaction temperature to 85 ℃ after the dropwise adding is finished for 3 hours, continuing to react for 4 hours, and adjusting the pH value to 6-7 by using alkali liquor after the reaction is completed to obtain the blue-emitting white organic silicon acrylate emulsion.
4. Compounding:
adding 40kg of water into a reaction kettle, adding 0.3kg of aromatic, uniformly stirring, adding 18kg of fluorine-containing amino silicone oil emulsion and 41.7kg of organic silicon acrylate emulsion, and uniformly stirring to obtain a finished product.
2. Diluting the hyperchromic repairing agent, wherein the ratio of hyperchromic repairing agent/water is 1: mixing the raw materials in a proportion of 18 times to obtain surface treatment liquid;
3. uniformly spraying the surface treatment liquid on the surface of the textile fabric;
4. and naturally drying the sprayed or soaked textile fabric at room temperature.
Example 3
The embodiment provides a surface treatment method of textile fabric, which comprises the following steps:
1. preparing hyperchromic repairing agent
1. Preparing the fluorine-containing amino silicone oil:
adding 90kg of octamethylcyclotetrasiloxane and 1.8kg of N-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane into a reaction kettle, heating to 90 ℃, adding 0.2kg of tetramethylpotassium hydroxide, heating to 138 ℃, keeping the temperature for 4 hours, heating to 140 ℃, vacuumizing, and extracting an oligomer. And (3) cooling to 85 ℃, adding 2.5kg of trifluoroethyl methacrylate and 0.2kg of ammonium persulfate, and reacting for 3 hours to obtain the transparent viscous fluorine-containing amino silicone oil.
2. Emulsifying the fluorine-containing amino silicone oil to obtain a fluorine-containing amino silicone oil emulsion:
adding 30kg of fluorine-containing amino silicone oil, 6kg of fatty alcohol-polyoxyethylene ether and 0.6kg of glacial acetic acid into a reaction kettle, uniformly stirring, slowly dropwise adding 63.4kg of water, slowly thinning the emulsion from a thick substance in the dropwise adding process, standing for defoaming when the emulsion is milky after the water is dropwise added, and filtering and discharging to obtain the fluorine-containing amino silicone oil emulsion.
3. Preparing an organic silicon acrylate emulsion:
adding 24kg of ethyl acrylate, 3kg of hydroxyl-terminated siloxane, 2kg of vinyl triethoxysilane and 1kg of fatty alcohol ether sodium sulfate into a dropwise adding tank, starting stirring for pre-emulsification, and when the emulsion is milky white and does not layer, indicating that the pre-emulsification is finished to obtain a pre-emulsion;
putting 40% of the pre-emulsion into a reaction kettle, adding 0.6kg of ammonium persulfate and 68.4kg of deionized water, heating to 80 ℃ to carry out seed emulsion polymerization, and obtaining seed emulsion after 10 min;
and (3) dropwise adding the residual 60% of pre-emulsion and 0.9kg of initiator into the seed emulsion, after 2 hours of dropwise adding, adjusting the reaction temperature to 85 ℃, continuing to react for 4 hours, and after the reaction is completed, adjusting the pH value to 6-7 by using alkali liquor to obtain the blue-emitting white organic silicon acrylate emulsion.
4. Compounding:
adding 40kg of water into a reaction kettle, adding 0.3kg of aromatic finishing agent, uniformly stirring, adding 19kg of fluorine-containing amino silicone oil emulsion and 40.7kg of organic silicon acrylate emulsion, and uniformly stirring to obtain a finished product.
2. Diluting the hyperchromic restoration agent, wherein the ratio of hyperchromic restoration agent/water is 1: mixing the components in a ratio of 20 times to obtain surface treatment liquid;
3. uniformly spraying the surface treatment liquid on the surface of the textile fabric;
4. and naturally airing the sprayed or soaked textile at room temperature.
The surface treated textiles of examples 1-3 were tested and the results were as follows:
1. color enhancement effect
The hyperchromic effect method comprises the following steps: the surface treatment methods of examples 1 to 3 were respectively used for the treatment of black cotton clothes, dark blue polyester cotton clothes, light blue wool clothes and red polyester cotton clothes, and the coloring effect was evaluated by the coloring rate and the coloring uniformity, and the test results are shown in tables 1 and 2. The brightening uniformity is judged and evaluated according to human eyes, and the testing method of the brightening rate comprises the following steps: folding the experimental fabrics before and after the deepening treatment into a plurality of layers, testing the fabrics on a datacolor color measuring instrument according to the same lines, and testing the K/S value of eight points on each piece of fabric.
Depth increase = K/S value after fabric treatment/K/S value before fabric treatment 100%.
Table 1 shows the results of measuring the depth increase of the clothes treated in examples 1 to 3
| Black cotton clothes | Dark blue polyester-cotton clothes | Light blue woolen clothes | Red polyester cotton clothes | |
| Example 1 treated garment | 110％ | 120％ | 120％ | 130％ |
| Example 2 treated garments | 130％ | 150％ | 150％ | 130％ |
| Example 3 treated clothes | 150％ | 160％ | 150％ | 140％ |
Table 2 shows the results of the test of the uniformity of brightening of the clothes treated in examples 1 to 3
| Black cotton clothes | Dark blue polyester cotton clothes | Light blue wool clothes | Red polyester cotton clothes | |
| Example 1 treated garment | Is substantially uniform | Uniformity | Uniformity | Uniformity |
| Example 2 treated clothes | Uniformity | Uniformity | Uniformity | Uniformity |
| Example 3 treated garments | Uniformity | Uniformity | Uniformity | Uniformity |
From the above, the surface treatment method of the invention can achieve ideal darkening and brightening effects on textiles with various colors and materials, such as black cotton clothes, dark blue polyester cotton clothes, light blue wool clothes, red polyester cotton clothes and the like, and has good brightening uniformity.
2. Wash resistance test
Water washing resistance test method: the clothes treated in the examples 1 to 3 are put into a washing machine, 5L of warm water with the temperature of 40 to 40 ℃ is added, and after the clothes are washed for 40min at the rotating speed of 800 r/min, the hand feeling and the shrinking effect of the washed clothes are evaluated, wherein the evaluation criteria are as follows:
1-3 points show that the shrinkage of the clothes is 5-10% (excluding 5%), and the clothes are hard;
4-6 points show that the shrinkage of the clothes is 1-5% (excluding the shrinkage of 1%, including 5%), and the clothes are slightly hard;
7-9 minutes shows that the shrinkage of the clothes is 0-1% (excluding 0, including 1%), and the clothes have soft hand feeling;
10 points indicate that the garment has no shrinkage and a soft feel.
The test results are shown in table 3.
Table 3 shows the results of the water-washing resistance test of the clothes treated in examples 1 to 3
| Black cotton clothes | Dark blue polyester cotton clothes | Red polyester cotton clothes | |
| Example 1 treated garment | 9 minutes | 8 is divided into | 8 is divided into |
| Example 2 treated garments | 10 minutes | 10 minutes | 10 minutes |
| Example 3 treated clothes | 10 minutes | 10 minutes | 10 minutes |
From the above, the clothes after the surface treatment of the invention have good water washing resistance, the shrinkage rate of the clothes can be controlled within 1%, and the clothes have soft hand feeling.
It should be noted that the woolen clothes were not tested for water-washing resistance because they could not be washed with water.
3. Treated garment Strength testing
The tear strength test method is carried out in accordance with GB/T3917.1-1997. The tear strength test results are shown in table 4:
table 4 shows the results of the tear strength test of the clothes treated in examples 1 to 3
| Black cotton clothes | Dark blue polyester cotton clothes | Light blue wool clothes | Red polyester cotton clothes | |
| Garment before treatment | 632N | 532N | 438N | 564N |
| Example 1 treated garment | 680N | 603N | 476N | 642N |
| Example 2 treated clothes | 654N | 622N | 501N | 623N |
| Example 3 treated garments | 701N | 658N | 523N | 642N |
From the above, the clothes subjected to the surface treatment of the invention have high tear strength and good strength performance.
4. Post-treatment garment hydrophilicity testing
The hydrophilicity test method is as follows: dripping water on the surface of the fabric from a certain height, testing the time required for the mirror reflection of the water drop to disappear, namely the wetting time, and judging the hydrophilicity of the fabric according to the time length. The hydrophilicity test results are shown in table 5:
table 5 shows the results of the hydrophilicity test of the clothes treated in examples 1 to 3
From the above, the clothes subjected to the surface treatment of the invention have short wetting time and good hydrophilic performance, wherein the wetting time is short for black cotton clothes, dark blue polyester cotton clothes, light blue wool clothes and red polyester cotton clothes.
The wool clothes were not tested for hydrophilicity, since they could not be washed with water.
5. After washing the clothes several times, the tensile properties of the clothes were tested
Example 3 was selected for tensile testing with multiple washes, the tensile testing was performed according to the national standard GB/T3923.2-2013, specifically the grab, 1 inch grab, CRE tensile tester, at a speed of 50mm/min, with the results shown in table 6 below:
table 6 shows the tensile Property results of the garments after multiple treatments
As can be seen from the above, the weft breaking strength and the warp breaking strength of the commercial detergent of example 3 were both reduced to some extent after washing. Analysis on the weft breaking strength and the warp breaking strength data shows that the strength drop value after washing in example 3 is obviously lower than that after washing in a commercial detergent, which may be that the emulsion after the clothes treated in example 3 is air-dried is more complete and firm in film formation on the fibers of the clothes, and has a certain protection effect on the strength of the fibers.
The commercially available detergent is a bluish-white brightening solution.
6. After washing the clothes for a plurality of times, testing the color difference of the clothes
Example 3 was selected for a color difference test for multiple washes, the color difference was measured according to the national standard GB/T3979-2008 "method for measuring object color", and the results are shown in table 7:
table 7 shows the results of color difference measurement of clothes after multiple treatments
As can be seen from the above, in the above data, the CIE L value represents the brightness; the CIE a value represents red/green, the value is that the red light is positive, and the green light is negative; CIE b value represents yellow/blue, and the value is positive and is yellow light bias, and the value is negative and is blue light bias; the CIE C value is the color light saturation; the CIE H value is the hue angle value bar coordinate. From the above data analysis, using illuminant D65 Deg as an example, the color lightness CIE L degradation values of the commercial detergents in the first to sixth washes were: 1. -0.54; 2. -0.78; 3. -0.84; 4. -0.85; 5. -0.85; 6. -0.86; in example 3, the reduction values of color lightness vividness in the first to sixth washes were: 1. -0.24; 2. -0.32; 3. -0.36; 4. -0.38; 5. -0.38; 6. -0.40. From the data analysis of the light sources A10 Deg, F02 10Deg, the CIE L drop of the commercial detergent is significantly greater than that of example 3 in 6 successive washes. This demonstrates that example 3 has significantly better color retention than the commercial care solutions.
Therefore, as the number of washing times increases, the color is lost, however, the hyperchromic restoration agent of the invention in the example 3 has obvious contrast with the commercial detergent, and the color retention of the invention is obviously better than that of the commercial care solution.
The commercially available detergent is a bluish-moon brightening solution.
In conclusion, the hyperchromic repairing agent is simple to use, does not need to be heated and baked after being used, and can form a film under the condition of natural air drying to realize the deepening and hyperchromic of the color of the textile fabrics made of various materials. In addition, the color-increasing repairing agent has good fastness on textiles, meets the daily washing fastness test, and has a lasting color fixing effect. Moreover, the textile treated by the hyperchromic repairing agent has soft hand feeling and good hydrophilicity.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (21)
1. A method for surface treatment of a textile fabric, comprising:
preparing a hyperchromic repairing agent;
diluting the hyperchromic repairing agent to obtain a surface treatment solution;
uniformly coating the surface of the textile fabric with the surface treatment liquid;
drying the textile fabric subjected to coating treatment, wherein the temperature of the drying treatment is less than or equal to 60 ℃;
the hyperchromic repairing agent comprises the following raw materials in parts by weight:
15-35 parts of fluorine-containing amino silicone oil emulsion, 10-50 parts of organic silicon acrylate emulsion and 20-70 parts of water;
the fluorine-containing amino silicone oil emulsion is obtained by emulsifying fluorine-containing amino silicone oil;
the organic silicon acrylate emulsion is obtained by carrying out low-temperature polymerization reaction on acrylate, hydroxyl-terminated polysiloxane, a silane coupling agent, an emulsifier and an initiator, wherein the low-temperature polymerization reaction temperature is 70-90 ℃.
2. The method for surface treatment of textile fabric according to claim 1, wherein the temperature of the drying treatment is 25 to 45 ℃.
3. The method for surface treatment of textile fabric according to claim 1, wherein the uniformly coating the surface of the textile fabric with the surface treatment liquid comprises:
uniformly spraying the surface treatment liquid on the surface of the textile fabric;
alternatively, the textile is soaked in the surface treatment liquid.
4. The method for surface treatment of textile fabrics according to claim 1, wherein the fluoro amino silicone oil comprises the following raw materials in parts by weight: 90 to 98 parts of organic silicon monomer, 1 to 6 parts of first silane coupling agent, 1 to 4 parts of trifluoroethyl methacrylate, 0.1 to 1 part of ammonium persulfate and 0.001 to 1 part of catalyst.
5. The method for surface treatment of textile fabric according to claim 4, wherein the organosilicon monomer is one or more selected from octamethylcyclotetrasiloxane, α, ω -dihydroxypolydimethylsiloxane, hexamethylcyclotrisiloxane, tetramethyltetraphenyltetrasiloxane, and tetraethylcyclotetrasiloxane;
the first silane coupling agent is one or more of gamma-aminopropyltriethoxysilane, 3-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, N-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane and gamma-diethylenetriamine propylmethyldimethoxysilane;
the catalyst is one or more of sodium hydroxide, potassium hydroxide, lithium hydroxide and tetramethyl ammonium hydroxide.
6. The method for surface treatment of textile fabric according to claim 4, wherein the fluorochemical amino silicone oil is prepared by the following method:
mixing an organic silicon monomer and a first silane coupling agent, heating, adding a catalyst, continuously heating, keeping the temperature for a preset time, and cooling;
adding trifluoroethyl methacrylate and ammonium persulfate, and reacting to obtain the fluorine-containing amino silicone oil.
7. The method for surface treatment of textile fabrics according to claim 1, 4 or 5, wherein the fluorine-containing amino silicone oil emulsion is obtained by adding a first emulsifier, glacial acetic acid and water into the fluorine-containing amino silicone oil for reaction, and the mass ratio of the addition of the fluorine-containing amino silicone oil emulsion, the first emulsifier, the glacial acetic acid and the water is (20-35): (2-8): (0.05-2): (60-85).
8. The method for surface treatment of textile fabric according to claim 7, wherein the first emulsifier is one or more of fatty alcohol-polyoxyethylene ether and dioctyl sodium sulfosuccinate.
9. The surface treatment method of the textile fabric according to claim 1, wherein the silicone acrylate emulsion comprises the following raw materials in parts by weight:
20 to 30 portions of acrylic ester, 3 to 10 portions of hydroxyl terminated polysiloxane, 0.1 to 5 portions of second silane coupling agent, 1 to 5 portions of second emulsifier, 0.5 to 5 portions of initiator and 50 to 78 portions of water.
10. The method for surface treatment of textile fabric according to claim 9, wherein the acrylate comprises one or more of methyl acrylate, butyl acrylate, methyl methacrylate, glycidyl methacrylate;
the second silane coupling agent comprises one or more of vinyl triethoxysilane, aminoethyl aminopropyl trimethoxysilane, isobutylene triethoxysilane, 3-aminopropyl triethoxysilane and gamma-diethylenetriamine propyl methyldimethoxysilane;
the second emulsifier comprises one or more of fatty alcohol-polyoxyethylene ether, nonylphenol polyoxyethylene ether and fatty alcohol ether sodium sulfate;
the initiator comprises one or more of sodium persulfate, potassium persulfate and ammonium persulfate.
11. The method for surface treatment of textile fabrics according to claim 9, wherein the silicone acrylate emulsion is prepared by the following method:
mixing acrylate, hydroxyl-terminated polysiloxane, a second silane coupling agent, a second emulsifier and water for pre-emulsification to obtain a pre-emulsion;
mixing part of the pre-emulsion with an initiator and water, heating and carrying out seed emulsion polymerization to obtain seed emulsion;
and dropwise adding the rest pre-emulsion and the initiator into the seed emulsion, adjusting the reaction temperature and preserving the heat after the dropwise adding is finished, and obtaining the organic silicon acrylate emulsion after the reaction is completed.
12. The method for surface treatment of textile fabric according to claim 9, wherein the particle size of the silicone acrylate emulsion is 400nm to 800nm;
the glass transition temperature of the acrylic ester is-70 ℃ to 0 ℃.
13. The special hyperchromic repairing agent for the surface treatment of the textile is characterized by comprising the following raw materials in parts by weight:
15-35 parts of fluorine-containing amino silicone oil emulsion, 10-50 parts of organic silicon acrylate emulsion and 20-70 parts of water;
the fluorine-containing amino silicone oil emulsion is obtained by emulsifying fluorine-containing amino silicone oil;
the organic silicon acrylate emulsion is obtained by carrying out low-temperature polymerization reaction on acrylate, hydroxyl-terminated polysiloxane, a silane coupling agent, an emulsifier and an initiator, wherein the low-temperature polymerization reaction temperature is 70-90 ℃.
14. The hyperchromic restoration agent according to claim 13, wherein the fluoro amino silicone oil comprises the following raw materials in parts by weight: 90 to 98 parts of organic silicon monomer, 1 to 6 parts of first silane coupling agent, 1 to 4 parts of trifluoroethyl methacrylate, 0.1 to 1 part of ammonium persulfate and 0.001 to 1 part of catalyst.
15. The hyperchromic restoration agent according to claim 13, wherein the fluorine-containing amino silicone oil emulsion is obtained by adding a first emulsifier, glacial acetic acid and water into the fluorine-containing amino silicone oil for reaction, and the adding mass ratio of the fluorine-containing amino silicone oil emulsion, the first emulsifier, the glacial acetic acid and the water is (20-35): (2-8): (0.05-2): (60 to 85).
16. The hyperchromic restoration agent according to claim 13, wherein the silicone acrylate emulsion comprises the following raw materials in parts by weight:
20 to 30 portions of acrylic ester, 3 to 10 portions of hydroxyl terminated polysiloxane, 0.1 to 5 portions of second silane coupling agent, 1 to 5 portions of second emulsifier, 0.5 to 5 portions of initiator and 50 to 78 portions of water.
17. The hyperchromic restoration agent according to claim 13, further comprising a fragrance;
based on the hyperchromic restoration agent, the adding amount of the aromatic is 0.2-0.8 part.
18. A method for preparing the hyperchromic restoration agent according to any one of claims 13-17, comprising:
(1) Preparing fluorine-containing amino silicone oil;
(2) Emulsifying the fluorine-containing amino silicone oil to obtain fluorine-containing amino silicone oil emulsion;
(3) Preparing organic silicon acrylate emulsion;
(4) According to the weight portion, 15 to 25 portions of the fluorine-containing amino silicone oil emulsion, 30 to 50 portions of the organic silicon acrylate emulsion and 20 to 70 portions of water are mixed to obtain a finished product.
19. The process for producing a hyperchromic restoration agent according to claim 18, wherein step (1) comprises:
mixing an organic silicon monomer and a first silane coupling agent, heating to 75-85 ℃, adding a catalyst, continuously heating to 130-135 ℃, keeping the temperature for 3-5 hours, heating to 140-145 ℃, performing vacuum pumping for low boiling, stopping the vacuum pumping when the viscosity reaches a preset value, and cooling to 80-85 ℃;
adding trifluoroethyl methacrylate and ammonium persulfate, and reacting for 2-3 hours to obtain the fluorine-containing amino silicone oil.
20. The process for preparing a hyperchromic restoration agent according to claim 18, wherein step (2) comprises:
firstly, mixing the fluorine-containing amino silicone oil, a first emulsifier and glacial acetic acid to obtain a first mixed solution;
and dropwise adding water into the first mixed solution, and uniformly mixing to obtain the fluorine-containing amino silicone oil emulsion.
21. The process for preparing a hyperchromic restoration agent according to claim 18, wherein step (3) comprises:
mixing acrylate, hydroxyl-terminated polysiloxane, a second silane coupling agent, a second emulsifier and water for pre-emulsification to obtain a pre-emulsion;
mixing 20-40% of the pre-emulsion with an initiator and water, heating to 70-90 ℃, and carrying out seed emulsion polymerization reaction for 8-20 min to obtain seed emulsion;
and (3) dropwise adding the residual 60-80% of pre-emulsion and initiator into the seed emulsion, adjusting the reaction temperature to 80-90 ℃ after dropwise adding, keeping the temperature for 3-5 h, and adjusting the pH of the reaction system after complete reaction to obtain the organic silicon acrylate emulsion.
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