CN109667154A - A kind of organic silicon rigidity-increasing depth finishing agent and its preparation process - Google Patents
A kind of organic silicon rigidity-increasing depth finishing agent and its preparation process Download PDFInfo
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- CN109667154A CN109667154A CN201811576292.8A CN201811576292A CN109667154A CN 109667154 A CN109667154 A CN 109667154A CN 201811576292 A CN201811576292 A CN 201811576292A CN 109667154 A CN109667154 A CN 109667154A
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- deep
- crude oil
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- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 34
- 239000010703 silicon Substances 0.000 title claims abstract description 34
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 25
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- -1 amino silicane Chemical compound 0.000 claims abstract description 70
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000010779 crude oil Substances 0.000 claims abstract description 35
- 239000003054 catalyst Substances 0.000 claims abstract description 34
- 239000007822 coupling agent Substances 0.000 claims abstract description 24
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 21
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 18
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000004945 emulsification Methods 0.000 claims abstract description 13
- 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 abstract description 13
- 229960000583 acetic acid Drugs 0.000 claims abstract description 8
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 8
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 8
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 26
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 24
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 24
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 22
- 229910019142 PO4 Inorganic materials 0.000 claims description 16
- 239000010452 phosphate Substances 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 13
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000010792 warming Methods 0.000 claims description 11
- ZOTKGMAKADCEDH-UHFFFAOYSA-N 5-triethoxysilylpentane-1,3-diamine Chemical compound CCO[Si](OCC)(OCC)CCC(N)CCN ZOTKGMAKADCEDH-UHFFFAOYSA-N 0.000 claims description 10
- RBNPOMFGQQGHHO-UHFFFAOYSA-N glyceric acid Chemical compound OCC(O)C(O)=O RBNPOMFGQQGHHO-UHFFFAOYSA-N 0.000 claims description 8
- XFRVVPUIAFSTFO-UHFFFAOYSA-N 1-Tridecanol Chemical compound CCCCCCCCCCCCCO XFRVVPUIAFSTFO-UHFFFAOYSA-N 0.000 claims description 7
- BIFQHCGLXZWNLN-UHFFFAOYSA-N 2,2,6-trifluoro-4-methyl-4-propyl-1,3,5,2,4,6-trioxatrisilinane Chemical compound CCC[Si]1(C)O[SiH](F)O[Si](F)(F)O1 BIFQHCGLXZWNLN-UHFFFAOYSA-N 0.000 claims description 7
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 claims description 7
- 229920002472 Starch Polymers 0.000 claims description 7
- 239000004359 castor oil Substances 0.000 claims description 7
- 235000019438 castor oil Nutrition 0.000 claims description 7
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 7
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 7
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 7
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 7
- 239000008107 starch Substances 0.000 claims description 7
- 235000019698 starch Nutrition 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- LTVDFSLWFKLJDQ-UHFFFAOYSA-N α-tocopherolquinone Chemical compound CC(C)CCCC(C)CCCC(C)CCCC(C)(O)CCC1=C(C)C(=O)C(C)=C(C)C1=O LTVDFSLWFKLJDQ-UHFFFAOYSA-N 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 230000033228 biological regulation Effects 0.000 claims description 3
- 238000007664 blowing Methods 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- 238000010008 shearing Methods 0.000 claims description 3
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 229910001950 potassium oxide Inorganic materials 0.000 claims 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 claims 1
- 239000000843 powder Substances 0.000 claims 1
- 239000013049 sediment Substances 0.000 claims 1
- 239000004744 fabric Substances 0.000 abstract description 73
- 238000004043 dyeing Methods 0.000 abstract description 13
- 239000004753 textile Substances 0.000 abstract description 8
- 239000012752 auxiliary agent Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 23
- 239000000047 product Substances 0.000 description 22
- 239000003921 oil Substances 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 17
- 229920013822 aminosilicone Polymers 0.000 description 12
- 239000000975 dye Substances 0.000 description 11
- 239000000839 emulsion Substances 0.000 description 10
- 238000000034 method Methods 0.000 description 8
- 238000011156 evaluation Methods 0.000 description 7
- 230000001804 emulsifying effect Effects 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 229920000742 Cotton Polymers 0.000 description 5
- 239000000835 fiber Substances 0.000 description 5
- 238000013112 stability test Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000006210 lotion Substances 0.000 description 4
- 229920001296 polysiloxane Polymers 0.000 description 4
- 238000007151 ring opening polymerisation reaction Methods 0.000 description 4
- 229920002545 silicone oil Polymers 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 239000006087 Silane Coupling Agent Substances 0.000 description 2
- 239000004902 Softening Agent Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 125000003368 amide group Chemical group 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 238000007667 floating Methods 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 238000004513 sizing Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000010186 staining Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- VFKZECOCJCGZQK-UHFFFAOYSA-M 3-hydroxypropyl(trimethyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CCCO VFKZECOCJCGZQK-UHFFFAOYSA-M 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 238000005282 brightening Methods 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- XIVLWOXCLOIZSW-UHFFFAOYSA-M chloromethyl-(2-hydroxypropyl)-dimethylazanium;chloride Chemical compound [Cl-].CC(O)C[N+](C)(C)CCl XIVLWOXCLOIZSW-UHFFFAOYSA-M 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- JJRDHFIVAPVZJN-UHFFFAOYSA-N cyclotrisiloxane Chemical compound O1[SiH2]O[SiH2]O[SiH2]1 JJRDHFIVAPVZJN-UHFFFAOYSA-N 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 125000005373 siloxane group Chemical group [SiH2](O*)* 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/6436—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing amino groups
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
- D06M15/11—Starch or derivatives thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/53—Polyethers
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/657—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing fluorine
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/01—Stain or soil resistance
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/11—Oleophobic properties
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a kind of organic silicon rigidity-increasing depth finishing agents, are related to textile dyeing and finishing auxiliary agent field, and the product includes following raw material: the deep crude oil of increasing: 30-50 parts, emulsifier: and 10-20 parts, water: 25-40 parts, glacial acetic acid: 5-10 parts；The deep crude oil of the increasing includes following raw material and its mass percent: octamethylcy-clotetrasiloxane: 55-85%, and amino silicane coupling agent: 5-20%, basic catalyst: 1-10% increases deep promotor: 1-10%, water: 1-10%.Preparation method are as follows: S1, each reagent configuration；S2, crude oil synthesis；S3, emulsification of crude oil.Composition of the invention can be used for fabric and increase deeply, and having reduces fabric surface refractive index, reaches and increases deep purpose to fabric, can dramatically increase fabric color depth, obtain colour purity just, and can increase fabric and slide the advantages of playing feel.
Description
Technical field
The present invention relates to textile dyeing and finishing auxiliary agent field, more specifically, it relates to a kind of organic silicon rigidity-increasing depth finishing agent and
Its preparation process.
Background technique
In recent years, with the continuous improvement of environmental requirement, dyeing industry national manufacturing industry second, useless since water consumption occupies
Water discharge amount is then that the recycling rate of waterused of the national 6th, water really only has the reasons such as 7%, and the various social pressures being subject to constantly increase
Greatly.Therefore the generation and discharge for how reducing dyeing waste water, respond the call of national policy, are a huge to present dyeing
Big problem.
Currently, the way of printing and dyeing enterprise is the injected volume by reducing dyestuff in dyeing course, to reduce dyeing waste water
It generates and discharges.But the reduction of dyestuff can but make the cloth after conventional dyeing process dark color is not deep, black is not black etc. occur
Phenomenon, it is difficult to meet requirement of the client to dark fabric.Therefore, to solve this problem, it will usually fabric is carried out to increase depths reason,
Existing fabric increases deep method are as follows: handles the finished product cloth that normal dyeing obtains with deep-dyeing agent, reduces dyed fabric
Surface obtains bathochromic effect to the refractive index of incident light.Wherein, fabric is handled with the deep-dyeing agent of low-refraction, is used in combination
Film forming is baked to reduce the reflection light quantity of fabric surface, so that fabric reaches heavy colour effect, it is in current textile fabric dyeing and finishing technology
A kind of common method.
But existing deep-dyeing agent is generally acrylic ester polymerization and forms, although this deep-dyeing agent, which can be such that fabric reaches, increases deep mesh
, but the feel of fabric cannot be improved, make the finished product cloth after having contaminated after having carried out increasing depths reason, it is also necessary to carry out again
Soft final finishing, makes that the production cost increases.
Summary of the invention
In view of the deficiencies of the prior art, the present invention intends to provide a kind of organic silicon rigidity-increasing depth finishing agent, pass through
It reduces fabric surface refractive index and reaches the deep purpose of increasing, fabric color depth can be dramatically increased, obtaining colour purity just, and can increase fabric
Sliding to play feel, energy-saving and environmental protection increase deeply, save dyestuff, reduce cost.
To achieve the above object, the present invention provides the following technical scheme that
A kind of organic silicon rigidity-increasing depth finishing agent, the product include following raw material: increasing deep crude oil: 30-50 parts, emulsifying
Agent: 10-20 parts, water: 25-40 parts, glacial acetic acid: 5-10 parts；
The deep crude oil of the increasing includes following raw material and its mass percent: octamethylcy-clotetrasiloxane: 55-85%, amino
Silane coupling agent: 5-20%, basic catalyst: 1-10% increases deep promotor: 1-10%, water: 1-10%.
By using above-mentioned technical proposal, octamethylcy-clotetrasiloxane is even with amino silane under the action of basic catalyst
Connection agent can form poly- amino silicone after ring-opening polymerisation.Detailed process are as follows: the amido organosilicon in amino silicane coupling agent
Monomer, which is first condensed, is made siloxane oligomer, and octamethylcy-clotetrasiloxane carries out ring-opening polymerisation, the two in the presence of base catalyst
Balanced reaction is carried out after forming short chain object of the end with active group, forms poly- amino silicone；It or is amido organosilicon list
Body is balanced in the presence of base catalyst with octamethylcy-clotetrasiloxane to react.
Since poly- amino silicone has both amino active group and organosilicon structures, thus and shown there are two types of structure
Performance.There is dipole effect in silicone molecules, it can effectively buffer and weaken the influence of external electrical field, thus to silicon is connected to
Hydroxyl on atom has protective effect, is allowed to the erosion not vulnerable to physical factor or chemical reagent.
The items product made of polysiloxane also has in addition to having corrosion-resistant, radiation resistance, high-low temperature resistant substantially
The characteristics such as agent of low hygroscopicity, high insulation resistance, low-k, low stress, vibration damping, environmental protection, hypotoxicity, fire retardant.Amino active group
Group polarity is extremely strong, reactivity worth is high, can be formed with the Interaction of substituents such as hydroxyl, the carboxyl of fiber surface in fiber surface
Very firm oriented attachment makes the frictional decrease between fiber, obtains good flexibility.
Simultaneously amino silicones can in a kind of organic film of fiber surface, this film to the absorption of light, reflection, refraction with
Untreated fabric is different, and the refractive index of silicone oil softening agent is lower, and about 1.4, the naked eyes of old friends have seemed increasing
Deep effect.
Emulsifier can improve the various surface tension constituted between phase in emulsion, be allowed to form uniform and stable dispersion
The substance of system or emulsion.Emulsifier is surface reactive material, has hydrophilic group and lipophilic group simultaneously in molecule, it is gathered in
On oil/water interface, interfacial tension can be reduced and reduction forms energy required for emulsion, to improve the energy of emulsion
Amount.
Further, the product also includes the raw material of following parts by weight: triethylamine: 1-5 parts, N, N- dimethyl ethanol
Amine: 5-10 parts.
By using above-mentioned technical proposal, triethylamine can react with amido silicon oil, increase hydrophilic radical-in lotion
COO-Content, improve the hydrophily of amido silicon oil, make the intersolubility of amido silicon oil and water enhance.It can make amido silicon oil simultaneously
In prepolymer dispersion after, hydrophobic strand crimps nucleation, and hydrophilic ion radical is located at particle surface, and towards in water,
As a large amount of-COO-Anion aggregated particle surface, and attract corresponding cation, after stablizing one can be formed in particle surface
Electric double layer generates electromotive force.This electromotive force can prevent close to each other between particle and agglomerate, and play similar emulsifier
Effect improves amido silicon oil emulsifying effectiveness, and the emulsion particle diameter made is small, stablizes, and the phenomenon that be not in floating oil.N, N- bis-
Methylethanolamine is as solvent, to improve the solubility of triethylamine, while as the presence for helping emulsion, to improve amino silicone
Oily emulsifying effectiveness.
Further, the deep crude oil of the increasing includes following raw material and its mass percent: octamethylcy-clotetrasiloxane: 60-
80%, amino silicane coupling agent: 8-15%, basic catalyst: 1-5% increases deep promotor: 3-6%, trifluoro propyl methyl ring three
Siloxanes: 1-10%, end-capping reagent: 0.5-1%, water: 4-10%.
By using above-mentioned technical proposal: trifluoro propyl methyl cyclotrisiloxane can make amino-modified silicone, to
Amino silicone has middle introducing fluorine ion, improves the water repellency of fabric, while having effects that oleophobic, hating dirt, is easier cloth
Washing.The refractive index that film can be reduced simultaneously, improves the increasing depth effect of cloth.
Further, the end-capping reagent includes following raw material and its mass percent: hexamethyldisiloxane: 30-50%,
3- chloro-2-hydroxypropyl-trimethyl ammonium chloride: 20-40%, isopropanol: 20-40%.
By using above-mentioned technical proposal, the work of siloxane group and the end in amido silicon oil in hexamethyldisiloxane
Property group react, in a certain range, to prevent the product of macromolecule from generating the control of the molecular weight of product, thus
Cause the effective component in amido silicon oil to reduce, reduces the increasing depth effect of amido silicon oil.
The amino silicone of generation can be had modification by 3- chloro-2-hydroxypropyl-trimethyl ammonium chloride, generate quaternized amino silicone
Oil, having the amino silicone generated has the effect of antibacterial, sterilization.Isopropanol is to dissolve hexamethyldisiloxane and the chloro- 2- of 3-
Hydroxypropyl-trimethyl ammonium chloride, improves the solubility of 3- chloro-2-hydroxypropyl-trimethyl ammonium chloride, while can also be improved amino silicone
The emulsification of oil, can be used as the presence of assistant for emulsifying agent.
Further, the silane coupling agent includes following raw material and its mass percent: 3- (2- aminoethyl)-aminopropyl
Triethoxysilane: 30-50%, polyetheramine: 10-20%, phosphate ester starch: 10-20%, water: 20-40%.
By using above-mentioned technical proposal, 3- (2- aminoethyl)-aminopropyl triethoxysilane and four silicon oxygen of prestox ring
Alkane can form amido silicon oil after ring-opening polymerisation under the effect of the catalyst.Polyetheramine can improve the wearability of cloth, and
3- (2- aminoethyl)-aminopropyl triethoxysilane can occur hydrogen bond with polyetheramine and connect, and improve between polyetheramine and cloth
Affinity, be easy to polyetheramine and be adhered to design on fabric surface, further increase the wearability of cloth.3- (2- aminoethyl)-ammonia simultaneously
It will form the very high-OH of activity after propyl-triethoxysilicane hydrolyzable, hydrogen bond can be formed with-OH present on cloth and connect,
And then improve the degree of adhesion of amido silicon oil and cloth.
The paste liquid transparency with higher and viscosity of phosphate ester starch and stronger gumminess, and its stabilization for pasting liquid
Property it is high, retrogradation is weak, can improve the flexibility for the film that product is formed on cloth, improves the feel of fabric.Phosphate simultaneously
There is excellent emulsifying capacity to animal and plant fat, aliphatic ester, silicone oil, mineral oil, amido silicon oil can be carried out tentatively
Emulsification, improves the emulsification degree of silicone oil；And it is with antistatic, and it is good with skin compatibility, there is good table at low concentrations
Face activity, shows excellent wetting scourability and synergistic function.
Further, the basic catalyst include one of potassium hydroxide, sodium hydroxide, tetramethyl oxyammonia or
It is several.
Further, the emulsifier includes following raw material and its mass percent: different tridecanol polyoxyethylene ether: 20-
45%, Castor Oil Phosphate Ester Salt: 20-40%, polyoxyethylene glycerol ether: 20-30%, isopropanol: 10-20%.
By using above-mentioned technical proposal, different tridecanol polyoxyethylene ether, Castor Oil Phosphate Ester Salt and polyoxyethylene glycerol
Ether can emulsify amido silicon oil, improve the various surface tension constituted between phase in emulsion, be allowed to be formed uniform and stable
The substance of dispersion or emulsion.
Due to that can generate many harmful foams in industrial processes, and it is thin that polyoxyethylene glycerol ether both ends, which have,
Water chain, and the intermediate block copolymer for being separated with hydrophilic chain, the molecule of this structure are easy to lie down shape and are gathered in gas-liquid interface, inhibit
Bubble generates, to achieve the purpose that eliminate bubble, improves industrial production efficiency.
Isopropanol improves different tridecanol polyoxyethylene ether, Castor Oil Phosphate Ester Salt, polyoxyethylene glycerol ether as solvent
Solubility, while the emulsifying effectiveness of emulsifier can be improved as assistant for emulsifying agent.
A kind of preparation method of organic silicon rigidity-increasing depth finishing agent, comprising the following steps:
S1: configuration amino silicane coupling agent: by 3- (2- aminoethyl)-aminopropyl triethoxysilane, polyetheramine, phosphate
Starch and water mix in a reservoir, heating heating, and stir 0.5-1h and obtain amino silicane coupling agent；
Configure emulsifier: by different tridecanol polyoxyethylene ether, Castor Oil Phosphate Ester Salt, polyoxyethylene glycerol ether, Yi Jiyi
Propyl alcohol mixes in a reservoir, heating heating, and stirs 0.5-1h and obtain emulsifier；
Configuration end-capping reagent: hexamethyldisiloxane, 3- chloro-2-hydroxypropyl-trimethyl ammonium chloride and isopropanol are being held
It is mixed in device, stirring 0.5-1h obtains end-capping reagent；
S2: octamethylcy-clotetrasiloxane and amino silicane coupling agent are added and blender and temperature are housed by the synthesis of crude oil
In the three-necked flask of meter, stirs and be warming up to 70-90 DEG C, addition basic catalyst stirs 20-30min, is warming up to 120-130
DEG C, insulation reaction 4-6h is being added trifluoro propyl methyl cyclotrisiloxane and basic catalyst, is stirring 20-30min, be warming up to
130-150 DEG C, insulation reaction 2-3h, reaction is cooled to 80-100 DEG C after viscosity reaches requirement, is added and increases deep promotor and envelope
Agent is held, the reaction was continued 1-3h vacuumizes 1-2h after the completion of heat preservation, is cooled to 50-70 DEG C of blowing to get sliding bullet and increases deep crude oil；
S3: emulsification of crude oil, emulsifier and crude oil according to certain mass than carrying out high speed shearing emulsification, while stirring plus water,
The 10%-20% of total Water is added, triethylamine and N, N- dimethylethanolamine is added, stirs to system phase inversion, is slowly added into surplus
Remaining water stirs while adding, and glacial acetic acid regulation system pH to 6.5-6.9 is added, and it is deep to obtain the milky white organic silicon rigidity-increasing with blue light
Finishing agent.
Further, the basic catalyst being added for the first time in the S2 includes potassium hydroxide, second of the alkalinity being added
Catalyst includes tetramethylammonium hydroxide, and the potassium hydroxide accounts for the 50-80% of basic catalyst total weight, tetramethyl hydroxide
Ammonium accounts for the 20-50% of basic catalyst total weight.
By using above-mentioned technical proposal, the catalytic activity of tetramethylammonium hydroxide is stronger than potassium hydroxide, but needs to heat up
To 135-140 DEG C of broken matchmaker 1h.Under normal circumstances, tetramethylammonium hydroxide cannot decompose completely, have a small amount of residual in system, lead
Crude oil is caused to contain remaining ammonia odor taste, flavescence, stability poor.Therefore potassium hydroxide conduct is selected when first time catalyst being added
Catalyst improves the quality of product.
In conclusion the invention has the following advantages:
1, the present invention is passed through under the action of basic catalyst with amino silicane coupling agent using octamethylcy-clotetrasiloxane
Poly- amino silicone can be formed after ring-opening polymerisation, since amino silicones can form a kind of organic film in fiber surface, this
Kind film is higher to the absorptivity of light, lower to reflection and refractive index, and about 1.4, the naked eyes of old friends have seemed the deep effect of increasing,
Obtaining makes fabric increase deep effect；
2, the present invention in preferably in crude oil add the trifluoro propyl methyl cyclotrisiloxane containing fluorine element, due to fluorine from
The water repellency of fabric can be improved in son, while having effects that oleophobic, hating dirt, and cloth is made to be easier to wash.It can drop simultaneously
The refractive index of low film improves the increasing depth effect of cloth.
Specific embodiment
Embodiment 1:
A kind of preparation method of organic silicon rigidity-increasing depth finishing agent, comprising the following steps:
S1: configuration amino silicane coupling agent, amino silicane coupling agent include following raw material and its mass percent: by 3-
(2- aminoethyl)-aminopropyl triethoxysilane: 40%, polyetheramine: 15%, phosphate ester starch: 15% and water: 30%, holding
It is mixed in device, heating heating, and stirs 0.7h under magnetic stirring apparatus and obtain amino silicane coupling agent；
Emulsifier is configured, emulsifier includes following raw material and its mass percent: by 30% different tridecanol polyoxyethylene
Ether, 30% Castor Oil Phosphate Ester Salt, 25% polyoxyethylene glycerol ether and 15% isopropanol, mix in a reservoir, rise
Temperature heating, and stir 0.7h under magnetic stirring apparatus and obtain emulsifier；
End-capping reagent is configured, end-capping reagent includes following raw material and its mass percent: hexamethyldisiloxane: 40%, 3- is chloro-
2- hydroxypropyl-trimethyl ammonium chloride: 30% and isopropanol: 30%, it mixes in a reservoir, and stirred under magnetic stirring apparatus
0.7h obtains end-capping reagent；
S2: octamethylcy-clotetrasiloxane and amino silicane coupling agent are added and blender and temperature are housed by the synthesis of crude oil
In the three-necked flask of meter, stirs and be warming up to 80 DEG C, addition basic catalyst stirs 25min, is warming up to 125 DEG C, insulation reaction
5h adds trifluoro propyl methyl cyclotrisiloxane and basic catalyst, stirs 25min, is warming up to 140 DEG C, insulation reaction
2.5h, reaction are cooled to 90 DEG C after viscosity reaches requirement, are added and increase deep promotor and end-capping reagent, the reaction was continued 2h, have kept the temperature
1.5h is vacuumized after, is cooled to 60 DEG C of blowings to get sliding bullet and is increased deep crude oil；
Each component is by percentage to the quality in crude oil are as follows: octamethylcy-clotetrasiloxane: 70%, amino silicane coupling agent:
10%, basic catalyst: 3%, the deep promotor of increasing: 4.5%, trifluoro propyl methyl cyclotrisiloxane: 5%, end-capping reagent: 0.5%,
Water: 7%.
The basic catalyst being wherein added for the first time includes potassium hydroxide, and second of basic catalyst being added includes tetramethyl
Base ammonium hydroxide, the potassium hydroxide account for the 65% of basic catalyst total weight, and it is total that tetramethylammonium hydroxide accounts for basic catalyst
The 35% of weight.
Increase deep promotor using the deep promotor 280 of the produced increasing of Shaoxing nine divisions of China in remote antiquity Science and Technology Ltd..
S3: emulsification of crude oil, emulsifier and crude oil according to certain mass than carrying out high speed shearing emulsification, while stirring plus water,
It is added the 15% of total Water, triethylamine and N, N- dimethylethanolamine is added, stirs to system phase inversion, is slowly added into remaining water
Amount, stirs while adding, and glacial acetic acid regulation system pH to 6.7 is added, obtains the milky white organic silicon rigidity-increasing depth finishing agent with blue light.
Each component is in parts by weight in product are as follows: crude oil: 40 parts, emulsifier: and 15 parts, water: 33 parts, glacial acetic acid: 8 parts, three
Ethamine: 3 parts, N, N- dimethylethanolamine: 8 parts.
Embodiment 2- embodiment 5 the difference from embodiment 1 is that, each substance of step 1 amino silicane coupling agent is with quality
Percentages are as follows:
Embodiment 6- embodiment 9 the difference from embodiment 1 is that, each substance in step 1 emulsifier is with mass percent
Meter is as follows:
Embodiment 10- embodiment 13 the difference from embodiment 1 is that, each substance in step 1 end-capping reagent is with quality percentage
It is as follows: than meter
Embodiment 14- embodiment 17 the difference from embodiment 1 is that, each component is as follows in parts by weight in step 2 crude oil
Table:
Embodiment 18- embodiment 21 the difference from embodiment 1 is that, the weight hundred of each component in step 2 basic catalyst
Ratio is divided to be as follows:
Embodiment 22- embodiment 25 the difference from embodiment 1 is that, it is each in step 3 product
Component is as follows: in parts by weight
Embodiment 26- embodiment 29 the difference from embodiment 1 is that, preliminary warming temperature is as follows in the synthesis of step 2 crude oil
Table:
| Embodiment | Embodiment 26 | Embodiment 27 | Embodiment 28 | Embodiment 29 |
| Temperature/DEG C | 70 | 75 | 85 | 90 |
Embodiment 30- embodiment 33 the difference from embodiment 1 is that, step 2 crude oil synthesis in be added trifluoro propyl methyl
Warming temperature is as follows: after cyclotrisiloxane
| Embodiment | Embodiment 30 | Embodiment 31 | Embodiment 32 | Embodiment 33 |
| Temperature/DEG C | 130 | 135 | 145 | 150 |
Embodiment 34- embodiment 37 the difference from embodiment 1 is that, the temperature that tentatively cools down is as follows in the synthesis of step 2 crude oil
Table:
| Embodiment | Embodiment 34 | Embodiment 35 | Embodiment 36 | Embodiment 37 |
| Temperature/DEG C | 80 | 85 | 95 | 100 |
Embodiment 38- embodiment 41 the difference from embodiment 1 is that, be added in the synthesis of step 2 crude oil increase deep promotor and
The temperature that cools down after end-capping reagent is as follows:
| Embodiment | Embodiment 38 | Embodiment 39 | Embodiment 40 | Embodiment 41 |
| Temperature/DEG C | 50 | 55 | 65 | 70 |
Embodiment 42- embodiment 45 the difference from embodiment 1 is that, first time amount of water and total in step 3 emulsification of crude oil
The percentage of water is as follows:
| Embodiment | Embodiment 42 | Embodiment 43 | Embodiment 44 | Embodiment 45 |
| Amount of water | 10% | 13% | 17% | 20% |
Embodiment 46- embodiment 49 the difference from embodiment 1 is that, pH value is as follows: in step 3 emulsification of crude oil
| Embodiment | Embodiment 46 | Embodiment 47 | Embodiment 48 | Embodiment 49 |
| PH value | 6.5 | 6.6 | 6.8 | 6.9 |
Comparative example 1: use Gao Zhenghong, Xie Hongde " preparation and its application of deep dyeing promoter silicone acrylate " (2006,
Printing and dyeing assistant, the 8th phase of volume 23) in prepare machine Si acrylate deep-dyeing agent.
Comparative example 2: with 1 difference of comparative example, deep treated cloth will be increased with G2B amino-silicone oil softening agent and do softness
Post-processing.
Comparative example 3: choosing the brightening agent that too paj is knitted is city's quarry sampling.
Product in embodiment 1 and in comparative example 1-3 is performed the following operation:
Fabric: bright and beautiful cotton Rome fabric；
Product dosage: 20g/L (30% lotion, Rome fabric)；
Technique: it pads (second dipping and rolling, pick-up 75%) → sizing (180 DEG C of Rome fabric, 90s) → resurgence, colour examining, comment
Determine feel.
Instrument: M-6 type forming machine (Jing Chuan Machinery Co., Ltd., Shaoxin City), RJ-350 III type padding machine (Shanghai double leaf industry
Co., Ltd).
Increase deep effect: fabric being folded 4 layers, color depth K/S value is tested, tests 8 points, be averaged.Increase deep effect
It is indicated using deep rate is increased, calculation method is as follows:
Increase preceding fabric K/S value × 100% of deep rate=(fabric K/S value before fabric K/S value-arrangement after arrangement)/arrangement.
Fabric tear strength test: deep to increasing according to ASTMD1424 standard on the digital tearing instrument of YG (B) 033D type
The tearing brute force of treated bright and beautiful cotton Rome fabric is measured.
Colour fastness to rubbing: by GB/T3920 " textile color stability test colour fastness to rubbing " to increasing deep treated brocade
Dry, the fastness to wet rubbing of cotton Rome fabric are tested, and with GB/T251 " textile color stability test evaluation staining grey
Scale " evaluation.
Fastness to soaping: after managing by GB/T3921-2008 " textile color stability test color fastness to washing " increasing depths
Bright and beautiful cotton Rome fabric soaping fastness tested, and with GB/T251 " the grey tinctorial pattern of textile color stability test evaluation staining
Card " and GB/T250 " textile color stability test evaluation discoloration gray scale " evaluation.
The comparison of feel: felt by way of being touched with hand the fluffy degree after fabric treating, pliability, resilience,
The composite factors such as smooth degree are evaluated, and feel is divided into 5 each grades, and the higher the better for rank, and 5 grades preferably, 1 grade of minimum, table
Middle feel level data has being obtained with hand touch evaluation for experience technician by five.
It can obtain from upper table: be compared by embodiment 1, comparative example 1, original cloth, although esters of acrylic acid deep-dyeing agent can
So that cloth achievees the purpose that increase depth, but the feel of cloth cannot be improved, the cloth after this deep-dyeing agent has been handled after cloth
Expecting feel ratio, deep treated that cloth feel is worse without increasing.
It is compared, will be carried out after the cloth after having been handled with esters of acrylic acid deep-dyeing agent by embodiment 1 and comparative example 2
Soft final finishing, cloth feel are still less than the cloth feel handled with products obtained therefrom of the present invention, and it is poor to increase deep effect.
It is compared by embodiment 1 and comparative example 3, the increasing depth effect and feel of products obtained therefrom of the present invention are adopted better than market
Sample.
In summary.Products obtained therefrom of the present invention have it is preferable increase deep effect, increased that deep treated that cloth has is higher
Color fastness and preferable mechanical strength, effectively improve the service performance of cloth.
Comparative example 4:
Compare with embodiment 1, step 1 configures in amino silicane coupling agent, and each raw material is in amino silicane coupling agent with quality hundred
Ratio is divided to be calculated as: 3- (2- aminoethyl)-aminopropyl triethoxysilane: 40%, phosphate ester starch: 15%, Yi Jishui: 45%；
Comparative example 5:
Compare with embodiment 1, step 1 configures in amino silicane coupling agent, and each raw material is in amino silicane coupling agent with quality hundred
Ratio is divided to be calculated as: 3- (2- aminoethyl)-aminopropyl triethoxysilane: 40%, polyetheramine: 15%, Yi Jishui: 45%,
Comparative example 6:
Compare with embodiment 1, step 1 configures in amino silicane coupling agent, and each raw material is in amino silicane coupling agent with quality hundred
Ratio is divided to be calculated as: 3- (2- aminoethyl)-aminopropyl triethoxysilane: 40%, Yi Jishui: 60%.
Comparative example 7:
Compare with embodiment 1, each component is in parts by weight in step 3 emulsification of crude oil, in product are as follows: crude oil: 40, emulsifier:
15, water: 36, glacial acetic acid: 8, N, N- dimethylethanolamine: 8.
Product in embodiment 1 and in comparative example 4-7 is performed the following operation:
Fabric: bright and beautiful cotton Rome fabric；
Product dosage: 20g/L (30% lotion, Rome fabric)；
Technique: it pads (second dipping and rolling, pick-up 75%) → sizing (180 DEG C of Rome fabric, 90s) → resurgence, colour examining, comment
Determine feel.
Instrument: NDJ-8S type rotational viscometer (Shanghai Ji Tai Electronic Science and Technology Co., Ltd.), M-6 type forming machine (Shaoxin City
Jing Chuan Machinery Co., Ltd.), III type padding machine of RJ-350 (Shanghai double leaf Industrial Co., Ltd.).
Viscosity: it is tested at (25 ± 1) DEG C with rotational viscometer.
Final product: being configured to 10% aqueous solution by stability, is fitted into matched centrifuge tube, and centrifuge speed is set
For 3000r/min, it is centrifuged 30min, whether observation lotion is layered, and it is such as not stratified, indicate that emulsion intercalation method is good.
Increase deep effect: fabric being folded 4 layers, color depth K/S value is tested, tests 8 points, be averaged.Increase deep effect
It is indicated using deep rate is increased, calculation method is as follows:
Increase preceding fabric K/S value × 100% of deep rate=(fabric K/S value before fabric K/S value-arrangement after arrangement)/arrangement.
The comparison of feel: felt by way of being touched with hand the fluffy degree after fabric treating, pliability, resilience,
The composite factors such as smooth degree and coolness are evaluated, and feel is divided into 5 each grades, the higher the better for rank, and 5 grades are preferably, and 1
Grade is minimum, and feel level data has being obtained with hand touch evaluation for experience technician by five in table.
| Detection project | Viscosity/mPas | Centrifugal stability | Increase depth rate/% | Sliding elasticity |
| Embodiment 1 | 138500 | Without separating into | 38.6% | 5 |
| Comparative example 4 | 127000 | Without separating into | 30.1% | 4.5 |
| Comparative example 5 | 132000 | Without separating into | 31.9% | 4.5 |
| Comparative example 6 | 100000 | It is divided into | 26.9% | 4 |
| Comparative example 7 | 124500 | It is divided into | 27.1% | 4 |
It can be obtained from upper table: triethylamine is added, amido silicon oil emulsifying effectiveness can be improved, the emulsion particle diameter made is small, steady
Calmly, the phenomenon that and being not in floating oil.Polyetheramine is added and the emulsifying effectiveness of product can be improved in phosphate ester starch, makes product more
Stablize.And product of the invention keeps the sliding elasticity of cloth more preferable, can assign cloth better feel.
This specific embodiment is only explanation of the invention, is not limitation of the present invention, those skilled in the art
Member can according to need the modification that not creative contribution is made to the present embodiment after reading this specification, but as long as at this
All by the protection of Patent Law in the scope of the claims of invention.
Claims (9)
1. a kind of organic silicon rigidity-increasing depth finishing agent, which is characterized in that the product includes following raw material: increasing deep crude oil: 30-
50 parts, emulsifier: 10-20 parts, water: 25-40 parts, glacial acetic acid: 5-10 parts；
The deep crude oil of the increasing includes following raw material and its mass percent: octamethylcy-clotetrasiloxane: 55-85%, and amino silane is even
Joining agent: 5-20%, basic catalyst: 1-10% increases deep promotor: 1-10%, water: 1-10%.
2. organic silicon rigidity-increasing depth finishing agent according to claim 1, which is characterized in that the product also includes following parts by weight
Raw material: triethylamine: 1-5 parts, N, N- dimethylethanolamine: 5-10 parts.
3. organic silicon rigidity-increasing depth finishing agent according to claim 1 or 2, which is characterized in that the deep crude oil of the increasing includes following
Raw material and its mass percent: octamethylcy-clotetrasiloxane: 60-80%, amino silicane coupling agent: 8-15%, basic catalyst: 1-
5%, increase deep promotor: 3-6%, trifluoro propyl methyl cyclotrisiloxane: 1-10%, end-capping reagent: 0.5-1%, water: 4-10%.
4. organic silicon rigidity-increasing depth finishing agent according to claim 3, which is characterized in that the end-capping reagent include following raw material and
Its mass percent: hexamethyldisiloxane: 30-50%, 3- chloro-2-hydroxypropyl-trimethyl ammonium chloride: 20-40%, isopropanol:
20-40%。
5. organic silicon rigidity-increasing depth finishing agent according to claim 1 or 4, which is characterized in that the amino silicane coupling agent packet
Containing following raw material and its mass percent: 3- (2- aminoethyl)-aminopropyl triethoxysilane: 30-50%, polyetheramine: 10-
20%, phosphate ester starch: 10-20%, water: 20-40%.
6. organic silicon rigidity-increasing depth finishing agent according to claim 1 or 5, which is characterized in that the basic catalyst includes hydrogen
One or more of potassium oxide, sodium hydroxide, tetramethyl oxyammonia.
7. organic silicon rigidity-increasing depth finishing agent according to claim 1 or 6, which is characterized in that the emulsifier includes following original
Material and its mass percent: different tridecanol polyoxyethylene ether: 20-45%, Castor Oil Phosphate Ester Salt: 20-40%, polyoxyethylene glycerol
Ether: 20-30%, isopropanol: 10-20%.
8. a kind of preparation method of organic silicon rigidity-increasing depth finishing agent, which comprises the following steps:
S1: configuration amino silicane coupling agent: 3- (2- aminoethyl)-aminopropyl triethoxysilane, polyetheramine, phosphate are formed sediment
Powder and water mix in a reservoir, heating heating, and stir 0.5-1h and obtain amino silicane coupling agent；
Configure emulsifier: by different tridecanol polyoxyethylene ether, Castor Oil Phosphate Ester Salt, polyoxyethylene glycerol ether and isopropanol,
It mixes in a reservoir, heating heating, and stirs 0.5-1h and obtain emulsifier；
Configure end-capping reagent: in a reservoir by hexamethyldisiloxane, 3- chloro-2-hydroxypropyl-trimethyl ammonium chloride and isopropanol
Mixing, stirring 0.5-1h obtain end-capping reagent；
S2: octamethylcy-clotetrasiloxane and amino silicane coupling agent are added equipped with blender and thermometer for the synthesis of crude oil
In three-necked flask, stirring and be warming up to 70-90 DEG C, addition basic catalyst stirs 20-30 min, is warming up to 120-130 DEG C,
Insulation reaction 4-6h is being added trifluoro propyl methyl cyclotrisiloxane and basic catalyst, is stirring 20-30min, be warming up to 130-
150 DEG C, insulation reaction 2-3h, reaction is cooled to 80-100 DEG C after viscosity reaches requirement, is added and increases deep promotor and end-capping reagent,
The reaction was continued 1-3 h vacuumizes 1-2h after the completion of heat preservation, is cooled to 50-70 DEG C of blowing to get sliding bullet and increases deep crude oil；
S3: emulsification of crude oil, emulsifier and crude oil, than carrying out high speed shearing emulsification, while stirring plus water, are added according to certain mass
Triethylamine and N, N- dimethylethanolamine, stirring is added in the 10%-20% of total Water, and system phase inversion is slowly added into surplus water,
It stirs while adding, glacial acetic acid regulation system pH to 6.5-6.9 is added, obtains the milky white organic silicon rigidity-increasing depth finishing agent with blue light.
9. the preparation method of organic silicon rigidity-increasing depth finishing agent according to claim 8, which is characterized in that in the S2 for the first time
The basic catalyst of addition includes potassium hydroxide, and second of basic catalyst being added includes tetramethylammonium hydroxide, the hydrogen
Potassium oxide accounts for the 50-80% of basic catalyst total weight, and tetramethylammonium hydroxide accounts for the 20-50% of basic catalyst total weight.
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| CN113957720A (en) * | 2021-09-27 | 2022-01-21 | 广东仙图科技研究有限公司 | Hydrophilic deepening dust-free silicone oil and preparation method and use method thereof |
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| CN113756102A (en) * | 2021-10-15 | 2021-12-07 | 传清化工(广东)有限公司 | Skin-friendly darkening finishing agent and preparation method thereof |
| CN115262241A (en) * | 2022-06-20 | 2022-11-01 | 广东仙图科技研究有限公司 | Surface treatment method of textile, special hyperchromic repairing agent and preparation method thereof |
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| CN116607329A (en) * | 2023-05-16 | 2023-08-18 | 诸暨市众伟染整有限公司 | Fabric deepening agent and preparation method and application thereof |
| CN117248378A (en) * | 2023-09-20 | 2023-12-19 | 广东创新精细化工实业有限公司 | Deepened silicone oil emulsion, preparation method thereof and application of deepened silicone oil emulsion in vulcanized black and dark fabric |
| CN117248378B (en) * | 2023-09-20 | 2024-04-16 | 广东创新精细化工实业有限公司 | Deepened silicone oil emulsion, preparation method thereof and application of deepened silicone oil emulsion in vulcanized black and dark fabric |
| CN119736798A (en) * | 2024-12-25 | 2025-04-01 | 广东协佳化学有限公司 | A kind of silicone oil emulsion and preparation method thereof |
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