CN110485166A - A kind of organic silicon emulsion increases deep hand feel finishing agent and preparation method, application - Google Patents
A kind of organic silicon emulsion increases deep hand feel finishing agent and preparation method, application Download PDFInfo
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- CN110485166A CN110485166A CN201910923252.4A CN201910923252A CN110485166A CN 110485166 A CN110485166 A CN 110485166A CN 201910923252 A CN201910923252 A CN 201910923252A CN 110485166 A CN110485166 A CN 110485166A
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- organic silicon
- finishing agent
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- hand feel
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- 239000000839 emulsion Substances 0.000 title claims abstract description 29
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 26
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 26
- 239000010703 silicon Substances 0.000 title claims abstract description 26
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 25
- 239000004744 fabric Substances 0.000 claims abstract description 20
- 230000000694 effects Effects 0.000 claims abstract description 18
- 230000001965 increasing effect Effects 0.000 claims abstract description 15
- 239000006210 lotion Substances 0.000 claims abstract description 12
- 239000012530 fluid Substances 0.000 claims abstract description 4
- 229920002545 silicone oil Polymers 0.000 claims description 24
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 17
- 229920002554 vinyl polymer Polymers 0.000 claims description 17
- 238000010792 warming Methods 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 239000003921 oil Substances 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims description 9
- QMMBZOSZCYBCDC-UHFFFAOYSA-N NCCNCCC[SiH](OC(OCC)(OCC)OCC)OC Chemical compound NCCNCCC[SiH](OC(OCC)(OCC)OCC)OC QMMBZOSZCYBCDC-UHFFFAOYSA-N 0.000 claims description 7
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 7
- 238000013019 agitation Methods 0.000 claims description 7
- 238000009835 boiling Methods 0.000 claims description 7
- 230000006837 decompression Effects 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000006185 dispersion Substances 0.000 claims description 7
- PELGKMTVNFFDDL-UHFFFAOYSA-N dodecyl-dimethoxy-methylsilane Chemical compound CCCCCCCCCCCC[Si](C)(OC)OC PELGKMTVNFFDDL-UHFFFAOYSA-N 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 230000009471 action Effects 0.000 claims description 6
- 238000002386 leaching Methods 0.000 claims 1
- 239000004094 surface-active agent Substances 0.000 claims 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 8
- 229910021529 ammonia Inorganic materials 0.000 abstract description 7
- 150000001335 aliphatic alkanes Chemical class 0.000 abstract description 5
- 239000010408 film Substances 0.000 abstract description 5
- 125000005358 mercaptoalkyl group Chemical group 0.000 abstract description 5
- 230000009257 reactivity Effects 0.000 abstract description 4
- 238000009988 textile finishing Methods 0.000 abstract description 4
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 239000013039 cover film Substances 0.000 abstract description 2
- 239000000835 fiber Substances 0.000 abstract description 2
- 238000012650 click reaction Methods 0.000 abstract 1
- -1 amido silicon Chemical compound 0.000 description 15
- 230000008859 change Effects 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 239000004205 dimethyl polysiloxane Substances 0.000 description 6
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 6
- 238000005096 rolling process Methods 0.000 description 6
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 6
- 239000007822 coupling agent Substances 0.000 description 5
- YQGOWXYZDLJBFL-UHFFFAOYSA-N dimethoxysilane Chemical compound CO[SiH2]OC YQGOWXYZDLJBFL-UHFFFAOYSA-N 0.000 description 5
- 239000012224 working solution Substances 0.000 description 5
- 239000000975 dye Substances 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 230000009102 absorption Effects 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000004043 dyeing Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- 238000000655 nuclear magnetic resonance spectrum Methods 0.000 description 2
- 230000005311 nuclear magnetism Effects 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
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 2
- 229910001948 sodium oxide Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- IGQLTMLBFFIKBR-UHFFFAOYSA-N SCO[Si](OC)(C)CCCO Chemical compound SCO[Si](OC)(C)CCCO IGQLTMLBFFIKBR-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- UDSAIICHUKSCKT-UHFFFAOYSA-N bromophenol blue Chemical compound C1=C(Br)C(O)=C(Br)C=C1C1(C=2C=C(Br)C(O)=C(Br)C=2)C2=CC=CC=C2S(=O)(=O)O1 UDSAIICHUKSCKT-UHFFFAOYSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000002653 sulfanylmethyl group Chemical group [H]SC([H])([H])[*] 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012956 testing procedure Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000005303 weighing 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
-
- 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
- C08G77/44—Block-or graft-polymers containing polysiloxane sequences containing only polysiloxane sequences
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/02—After-treatment
- D06P5/04—After-treatment with organic compounds
- D06P5/08—After-treatment with organic compounds macromolecular
-
- 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
- D06M2200/50—Modified hand or grip properties; Softening compositions
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
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)
- Silicon Polymers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The present invention relates to a kind of organic silicon emulsions to increase deep hand feel finishing agent and preparation method, application, synthesize with reactivity, surface coating increase diffusing reflection function containing long chain alkane, mercapto alkyl, ammonia hydrocarbyl side chain comb shape organosilicon.Since silicone backbone refractive index is low, and ammonia alkyl is had, strong with fabric affinity, long chain alkane increases fabric surface bumps performance after so that finishing agent is formed a film, and increases diffusing reflection, can form rough low refractive index film in fiber surface.There is reactive mercapto alkyl by introducing in organosilicon side chain, be based on sulfydryl-alkene click-reaction, improve its reactivity with vinyl-terminated silicone fluid, form branched silicone lotion.In textile finishing, by framework branched structure, cloth cover film complexity is improved, the increasing depth effect of product is further increased.
Description
Technical field
The invention belongs to textile printing and dyeing processing and final finishing field, and in particular to a kind of deep hand feel finishing of organic silicon emulsion increasing
Agent and preparation method, application.
Background technique
Currently, as China's conventional column industry-textile industry, a large amount of dyestuffs consumption for link of printing and dyeing and a large amount of waste water
It generates and brings heavy burden to environment, resource.With energetically rectification, non-environmental protection dyestuff of the country to dyeing in recent years
Severe monitoring, energy-saving and emission-reduction, to technical transition, raising product competitiveness becomes the extremely urgent task of the sector.In addition,
As the popularization and Arab region of Novel super-thin fabric are to absolutely black pursuit, fabric contaminates deep problem and is increasingly subject to
Pay attention to.Using deep technology is increased, dyestuff can be not only saved, discharge of wastewater is reduced, can also overcome increasing dye dosage that cannot reach
The bathochromic effect problem arrived.
Use on the market at present it is mostly be polyurethane resin finishing agent, acrylic resin finishing agent, Organic fluoride finishing agent and
Organic silicone finishing agent.
Preceding three classes product is since structure limits, and for fabric substantially without slippery, wearability is not high after arrangement, by these three increasings
Fabric after deep product treatment, the final finishing stage, there is still a need for carry out organic silicon hand feeling arrangement again.Esters of acrylic acid product treatment
It is even more abnormal rough after fabric, poor flexibility, poor surface smoothness, the fluorine-containing raw material of Organic fluoride finishing agent also exists economical and environmentally friendly etc.
Problem.
Since organic silicon oxygen bond has rotatory, it is made to readily penetrate through oxygen, nitrogen etc., fabric has soft fluffy after processing
Loose performance and good smooth sense, are widely used in the fabric post-treatment stage, but conventional organic silicon hand feeling finishing agent such as amido silicon oil,
Block silicone oil is generally unable to reach the deep effect of ideal increasing.
Summary of the invention
The purpose of the present invention is to provide it is a kind of it is simple and reasonable, clean and maintenance is easy, cheap and good-quality side is inhaled
Formula smokeless purifier, with overcome the deficiencies in the prior art.
The present invention the technical solution to solve the technical problem is that: a kind of organic silicon emulsion increases deep hand feel finishing agent, and structure is such as
Under:
Above-mentioned organic silicon emulsion increases the preparation method of deep hand feel finishing agent, comprising the following steps: 1) system of comb shape organosilicon
It is standby: to use linear body, dodecyl methyl dimethoxysilane, mercapto hydroxypropyl methyl dimethoxysilane, N- β-aminoethyl-γ-
Aminopropyltriethoxy dimethoxysilane is raw material, under basic catalyst effect, 0.5~4h of prepolymerization reaction, vacuum decompression reaction 1~
10h obtains having compared with strong affinity, soft, the organic silanol terminated polydimethylsiloxane of the deep preferable comb shape of effect of increasing；2) branched silicone lotion
Preparation: comb shape organosilicon is added in the four-hole boiling flask equipped with thermometer, is warming up to 50~70 DEG C, triethanolamine catalyst is made
Under, vinyl silicone oil is added in substep, is stirred to react 30 minutes to 2 hours, is obtained branched structure organic silicone oil；It is living that surface is added
Property agent, under high velocity agitation be added deionized water carry out emulsion dispersion, obtain branched structure organic silicon emulsion.
Above-mentioned organic silicon emulsion increases the application of deep hand feel finishing agent: applying in textile finishing, the organic silicon emulsion increases
The finishing fluid concentration of deep hand feel finishing agent is not less than 20g/L, technique for applying is: an immersing and rolling --- 100 DEG C drying --- 150 DEG C
~180 DEG C of * 90s thermal finalizations.
The beneficial effects of the present invention are:
The present invention passes through the reaction ratio of control ammonia alkyl coupling agent, mercapto alkyl coupling agent, long chain alkane coupling agent, linear body
Example, the design of silicone molecule amount size and the selection of emulsifying process, generate the combed organosilicon of specific main chain.In order to further mention
Its high darkening effect on the fabric, introduces vinyl silicone oil and the synthesizing branched organosilicon of comb shape organosilicon reaction, optimization and collation
The formula of agent investigates the performances such as increasing depth effect and the feel of its collated rear fabric.
The present invention designs and synthesizes and provides reactivity, surface coating increase diffusing reflection function containing long chain alkane, mercapto hydrocarbon
The comb shape organosilicon of base, ammonia hydrocarbyl side chain.Since silicone backbone refractive index is low, and ammonia alkyl is had, with fabric affinity
By force, increase fabric surface bumps performance after long chain alkane makes finishing agent form a film, increase diffusing reflection, can be formed in fiber surface recessed
The low refractive index film of convex injustice.There is reactive mercapto alkyl by introducing in organosilicon side chain, clicked based on sulfydryl-alkene anti-
It answers, improves its reactivity with vinyl-terminated silicone fluid, form branched silicone lotion.In textile finishing, pass through framework branching
Structure improves cloth cover film complexity, further increases the increasing depth effect of product.
The fabric of organosilicon obtained through the invention increases deep hand feel finishing agent and remains the excellent smooth feel of organosilicon,
Excellent increasing depth effect is also obtained, it is possible to reduce the increasing depths reason of process before textile finishing, it is economic and environment-friendly, there is very high quotient
Industry value.
To sum up, raw material of the present invention is easy to get, and preparation process is simple, and industrialization is at low cost, low for equipment requirements；Pass through sulfydryl-
Double bond click chemistry reaction construction branched structure organosilicon, is swift in response；Pass through sulfydryl-double bond construction branched structure and long-chain
Alkyl structure cooperation manufacture concave-convex effect organic film, increases deep ratio up to 30%；It is not fluorine-containing, it is environmentally protective, and solve existing
The shortcomings that deep-dyeing agent feel is poor, needs subsequent hand feel finishing.
Detailed description of the invention
Fig. 1 is the H of comb shape modification organic silicon oil of the invention1NMR spectra.
Fig. 2 is the H of comb shape modification organic silicon oil of the invention1NMR spectra partial enlarged view.
In attached drawing, abscissa indicates chemical shift, and ordinate indicates peak intensity.
Specific embodiment
The embodiments described below with reference to the accompanying drawings are exemplary, for explaining only the invention, and should not be understood as
Limitation of the present invention.
Embodiment 1
(1) preparation of comb shape organosilicon: by linear body 500g, dodecyl methyl dimethoxysilane 12g, mercapto propyl first
Base dimethoxysilane 5g, N- β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane 5g are raw material, are warming up to 80 DEG C, hydrogen-oxygen
Change under sodium 0.2g effect, prepolymerization reaction 0.5h, vacuum decompression reacts 2h, obtains the organic silanol terminated polydimethylsiloxane of comb shape.
(2) preparation of branched silicone lotion: 500g comb shape organosilicon is added in the four-hole boiling flask equipped with thermometer,
It is warming up to 50 DEG C, under triethanolamine catalyst action, is added in three times, the ethylene of 4.07g molecular weight 500g/mmol is added every time
Base silicone oil (such as vinyl is excessive, then comb shape organosilicon is added in vinyl silicone oil), is stirred to react 30 minutes, obtains branching knot
Structure organic silicone oil.AEO-7 of the oil quality than 30% is added, deionized water is added under high velocity agitation and carries out emulsion dispersion, obtains
Branched structure organic silicon emulsion.
(3) branched silicone emulsion applications technique: being 20g/L working solution, an immersing and rolling -- 100 DEG C of drying -- by concentration
150 DEG C of thermal finalizations in * 90 seconds.
Embodiment 2
(1) preparation of comb shape organosilicon: by linear body 500g, dodecyl methyl dimethoxysilane 12g, mercapto propyl first
Base dimethoxysilane 5g, N- β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane 5g are raw material, are warming up to 80 DEG C, hydrogen-oxygen
Change under sodium 0.2g effect, prepolymerization reaction 0.5h, vacuum decompression reacts 2h, obtains the organic silanol terminated polydimethylsiloxane of comb shape.
(2) preparation of branched silicone lotion: 500g comb shape organosilicon is added in the four-hole boiling flask equipped with thermometer,
It is warming up to 50 DEG C, under triethanolamine catalyst action, is added in three times, the vinyl of 2g molecular weight 500g/mmol is added every time
Silicone oil (such as vinyl is excessive, then comb shape organosilicon is added in vinyl silicone oil), is stirred to react 30 minutes, obtains branched structure
Organic silicone oil.AEO-7 of the oil quality than 20% is added, deionized water is added under high velocity agitation and carries out emulsion dispersion, is propped up
Change structural silicone lotion.
(3) branched silicone emulsion applications technique: being 20g/L working solution, an immersing and rolling -- 100 DEG C of drying -- by concentration
150 DEG C of thermal finalizations in * 90 seconds.
Embodiment 3
(1) preparation of comb shape organosilicon: by linear body 500g, dodecyl methyl dimethoxysilane 12g, mercapto propyl first
Base dimethoxysilane 5g, N- β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane 5g are raw material, are warming up to 80 DEG C, hydrogen-oxygen
Change under sodium 0.2g effect, prepolymerization reaction 0.5h, vacuum decompression reacts 2h, obtains the organic silanol terminated polydimethylsiloxane of comb shape.
(2) preparation of branched silicone lotion: the vinyl silicone oil of 18g molecular weight 500g/mmol is added to equipped with temperature
It spends in the four-hole boiling flask of meter, is warming up to 50 DEG C, under triethanolamine catalyst action, be added in three times, 167g comb shape is added every time
Organosilicon (such as vinyl is excessive, then comb shape organosilicon is added in vinyl silicone oil), is stirred to react 30 minutes, obtains branching knot
Structure organic silicone oil.AEO-7 of the oil quality than 30% is added, deionized water is added under high velocity agitation and carries out emulsion dispersion, obtains
Branched structure organic silicon emulsion.
(3) branched silicone emulsion applications technique: being 20g/L working solution, an immersing and rolling -- 100 DEG C of drying -- by concentration
150 DEG C of thermal finalizations in * 90 seconds.
Embodiment 4
(1) preparation of comb shape organosilicon: by linear body 500g, dodecyl methyl dimethoxysilane 12g, mercapto propyl first
Base dimethoxysilane 5g, N- β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane 12g are raw material, are warming up to 80 DEG C, hydrogen
Under sodium oxide molybdena 0.2g effect, prepolymerization reaction 1h, vacuum decompression reacts 2h, obtains the organic silanol terminated polydimethylsiloxane of comb shape.
(2) preparation of branched silicone lotion: 500g comb shape organosilicon is added in the four-hole boiling flask equipped with thermometer,
It is warming up to 50 DEG C, under triethanolamine catalyst action, is added in three times, the vinyl of 2g molecular weight 500g/mmol is added every time
Silicone oil (such as vinyl is excessive, then comb shape organosilicon is added in vinyl silicone oil), is stirred to react 30 minutes, obtains branched structure
Organic silicone oil.AEO-7 of the oil quality than 20% is added, deionized water is added under high velocity agitation and carries out emulsion dispersion, is propped up
Change structural silicone lotion.
(3) branched silicone emulsion applications technique: being 20g/L working solution, an immersing and rolling -- 100 DEG C of drying -- by concentration
150 DEG C of thermal finalizations in * 90 seconds.
Embodiment 5
(1) preparation of comb shape organosilicon: by linear body 500g, dodecyl methyl dimethoxysilane 12g, mercapto propyl first
Base dimethoxysilane 2g, N- β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane 12g are raw material, are warming up to 80 DEG C, hydrogen
Under sodium oxide molybdena 0.2g effect, prepolymerization reaction 1h, vacuum decompression reacts 2h, obtains the organic silanol terminated polydimethylsiloxane of comb shape.
(2) preparation of branched silicone lotion: 500g comb shape organosilicon is added in the four-hole boiling flask equipped with thermometer,
It is warming up to 50 DEG C, under triethanolamine catalyst action, is added in three times, the vinyl of 1g molecular weight 1000g/mmol is added every time
Silicone oil (such as vinyl is excessive, then comb shape organosilicon is added in vinyl silicone oil), is stirred to react 40 minutes, obtains branched structure
Organic silicone oil.AEO-7 of the oil quality than 40% is added, deionized water is added under high velocity agitation and carries out emulsion dispersion, is propped up
Change structural silicone lotion.
(3) branched silicone emulsion applications technique: being 20g/L working solution, an immersing and rolling -- 100 DEG C of drying -- by concentration
150 DEG C of thermal finalizations in * 90 seconds.
By protonating the amino of silicone oil and sulfydryl in glacial acetic acid, generates salt hydrochloric acid standard solution and refer in bromophenol blue
Show and is titrated under agent, the total value of available amino and sulfydryl.Ammonia value+sulfydryl value=v*C/m, wherein C is hydrochloric acid standard solution
Equivalent concentration 0.1, v become hydrochloric acid volume used in yellow from blue for titration solution, and m is that silicone oil quality is titrated needed for weighing.
In order to verify through pectination silicone oil structure synthesized by the present invention, nuclear-magnetism test is carried out.
Referring to Fig. 1-2, from H1-NMR spectrogram 1-2 as it can be seen that there is strong-CH in δ=1.3ppm or so2Methylene absorption peak,
Appearance-CH near 0.88ppm3There is Si-CH in methyl peak, 0.1ppm3Silicon methyl peak.Since chain alkyl chain length is longer and silicon
Methyl content is higher, therefore silicon methyl Si-CH in silicone oil3And methylene-CH2The intensity of absorption peak is significantly greater than other absorptions
Peak.Amplify δ be at 1.5~4ppm nuclear-magnetism peak as it can be seen that visible Si-CH at δ=1.3ppm2Phenylsilylene peak, δ be 1.6ppm and
1.7ppm distinguishes the Si-CH in visible mercapto alkyl coupling agent and ammonia alkyl coupling agent structure2-CH2, δ, which is at 2.5ppm, is-
CH2NHCH2CH2NH2And CH2-SH。
In order to verify the increasing depth effect of the textile after branched silicone of the present invention increases deep hand feel finishing agent processing, dE
Value and the deep ratio of increasing indicate.
Testing procedure: needing the test sample of 3 pieces of 180*180mm (7*7in.), needed before test by it at 21 ± 1 DEG C of temperature,
The standard environment relative humidity of relative humidity 65 ± 2% at least 4 hours.In addition, each sample is required comprising all differences in fabric
The horizontal and vertical yarn of specification.Be placed in the production of UltraScan company, the U.S., on the color difference meter of model VIS, read dE value and
Increase deep ratio.Every piece of cloth is surveyed three points and is averaged, and same sample takes three pieces of cloth average values.
Embodiment increases deep grade form
| Number | dE | Increase deep ratio |
| Embodiment 1 | 2.53 | 32 |
| Embodiment 2 | 2.24 | 29 |
| Embodiment 3 | 2.26 | 29 |
| Embodiment 4 | 2.17 | 28 |
| Embodiment 5 | 2.31 | 30 |
The foregoing is merely preferred embodiments of the invention, actually each specific raw material cited by the present invention and each original
Bound, the section value of material, and bound, the section value of technological parameter (such as temperature, time) can realize this hair
It is bright, embodiment numerous to list herein.
Although an embodiment of the present invention has been shown and described, those skilled in the art should understand that: not
A variety of change, modification, replacement and modification can be carried out to these embodiments in the case where being detached from the principle of the present invention and objective, this
The range of invention is limited by claim and its equivalent replacement, without creative work improvements introduced etc., should all include
Within protection scope of the present invention.
Claims (3)
1. a kind of organic silicon emulsion increases deep hand feel finishing agent, it is characterised in that: the organic silicon emulsion increases deep hand feel finishing agent
Structure is as follows:
2. organic silicon emulsion increases the preparation method of deep hand feel finishing agent according to claim 1, it is characterised in that including following
Step:
1) linear body, dodecyl methyl dimethoxysilane, mercapto hydroxypropyl methyl dimethoxy the preparation of comb shape organosilicon: are used
Silane, N- β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane are raw material, under basic catalyst effect, prepolymerization reaction 0.5
~4h, vacuum decompression react 1~10h, obtain having compared with strong affinity, soft, the preferable comb shape organosilicon silicon of the deep effect of increasing
Oil；
2) preparation of branched silicone lotion: comb shape organosilicon is added in the four-hole boiling flask equipped with thermometer, is warming up to 50
~70 DEG C, under triethanolamine catalyst action, vinyl silicone oil is added in substep, is stirred to react 30 minutes to 2 hours, is obtained branching
Structural silicone oil；Surfactant is added, deionized water is added under high velocity agitation and carries out emulsion dispersion, obtains branched structure
Organic silicon emulsion.
3. organic silicon emulsion increases the application of deep hand feel finishing agent according to claim 1, it is characterised in that: apply whole in fabric
In reason, the finishing fluid concentration that the organic silicon emulsion increases deep hand feel finishing agent is not less than 20g/L, and technique for applying is: 1) leaching one
It rolls；2) 100 DEG C of drying；3) 150 DEG C~180 DEG C * 90s thermal finalizations.
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| CN111116920A (en) * | 2019-12-26 | 2020-05-08 | 福建省晋江新德美化工有限公司 | Branched polyamino long-chain alkyl polysiloxane, waterproof soft organic silicon finishing agent and preparation method thereof |
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| CN114541145A (en) * | 2019-09-27 | 2022-05-27 | 佛山市顺德区德美瓦克有机硅有限公司 | Application of organic silicon emulsion hand feeling deepening finishing agent |
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Address after: 528305 No.9, Keyuan 2nd Road, high tech Zone (Ronggui), Shunde District, Foshan City, Guangdong Province Patentee after: Guangdong Demei Organic Silicon Co.,Ltd. Country or region after: China Address before: 528305 No.9, Keyuan 2nd Road, high tech Zone (Ronggui), Shunde District, Foshan City, Guangdong Province Patentee before: WACKER DYMATIC SILICONES (SHUNDE) CO.,LTD. Country or region before: China |