CN101736597A - Preparation of crisp oil lubricating organosilicone coating agent - Google Patents
Preparation of crisp oil lubricating organosilicone coating agent Download PDFInfo
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- CN101736597A CN101736597A CN200810162127A CN200810162127A CN101736597A CN 101736597 A CN101736597 A CN 101736597A CN 200810162127 A CN200810162127 A CN 200810162127A CN 200810162127 A CN200810162127 A CN 200810162127A CN 101736597 A CN101736597 A CN 101736597A
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Abstract
The invention relates to preparation of a crisp oil lubricating organosilicone coating agent. The crisp oil lubricating organosilicone coating agent is mainly used for high-grade handfeel finish of fabrics; the coating agent consists of three compositions: (A) 100 weight parts of mixture comprising the following compositions: (A1) 10 to 80 percent hydroxy silicone oil, (A2) 20 to 50 percent methyl silicone oil and (A3) 1 to 10 percent hydrogen-based silicon oil, (B) 0.1 to 5 weight parts of organic tin catalyst and (C) 0.2 to 2 weight parts of coupling agent containing epoxy groups, sulfhydryls, amidogens, uramidos and other functional groups. The prepared coating agent can endow the coating fabrics with high elastic, crisp, smooth and oil lubricating handfeel.
Description
Technical field:
The present invention relates to a kind of preparation method of SILICONE COATING AGENT, relate in particular to a kind of preparation that can give the SILICONE COATING AGENT of the high-elastic crisp level and smooth glossy feel of holding concurrently of fabric.The invention belongs to the auxiliary chemicals technical field.
Background technology:
Textile coating agent can be given loomage water proof and moisture permeable, fire-retardant, antiultraviolet, performance such as antibiotic, improves the fabric class, has obtained flourish in recent years.Wherein principal item has: polyacrylate coating agent, polyurethane coating agent, pvc coating agent, natural and synthetic rubber coating agent, polytetrafluorethylecoatings coatings agent and SILICONE COATING AGENT etc.
Organosilicon material has that high-low temperature resistant, weather-proof, physiology inertia (skin is not stimulated), interfacial tension are low, silica silicon bond angle reaches many particular performances such as strand is submissive greatly, can give the very strong tearing strength of fabric after the coating as the SILICONE COATING AGENT of base-material, outstanding water vapor permeability, performances such as excellent flexibility and UV resistant.Be widely used for the fabric coating finish of raincoat, umbrella, tarpaulin, navigation clothes, baby pants, fire balloon, ski-wear, protective clothing etc., be subjected to people's attention always.Germany wacker company just develops serial SILICONE COATING AGENT product as far back as the seventies in 20th century, the Dow-corning company of the U.S., GE company thereafter, and the SILICONE COATING AGENT that the company of SHIN-ETSU HANTOTAI of Japan etc. also all releases one after another is separately put on market.In addition, also emerge in multitude of relevant both at home and abroad bibliographical information.As U.S. Pat 4,994,317 disclose a kind of organosilicon fire protection flame retarding coating agent, and the fabric after the coating has the performance of opposing thermal-flame, give the good drapability of fabric, sewing property and aesthetic feeling etc.U.S. Pat 7,059,627 disclose a kind of coating agent that is used for the air bag coating, can improve the high-temperature machinery and the bottom bond properties of air bag.Chinese patent CN1,670,300 preparation methods that disclose a kind of bi-component SILICONE COATING AGENT are mainly used in the fabric waterproof airing function and handle.
Sum up the disclosed document of forefathers as can be known, domestic and international most of SILICONE COATING AGENT is developed in order to give some specific function of fabric.Up to the present, the SILICONE COATING AGENT that is specifically designed to the fabric feeling Feeling Finishing still seldom is seen in bibliographical information, and the coated fabric of excellent handle is to improve one of its key factor of using class, therefore, in the present invention, we will prepare a kind of SILICONE COATING AGENT that can give the high-elastic crisp level and smooth glossy feel of holding concurrently of fabric, to satisfy the domestic and international market needs that day easily increases by molecular structure and prescription design.
Summary of the invention:
The present invention seeks to: in this SILICONE COATING AGENT constituent, utilize dehydrogenation reaction between containing hydrogen silicone oil and the hydroxy silicon oil, can in the fabric coating procedure, form fine and close crosslinked organosilicon epithelium, give fabric and very scrape crisp feel.And utilize the flexible smooth of organosilicon strand excellence, give fabric face smooth glossy feel again simultaneously.On this basis, adjust by Molecular Structure Design and prescription, the crosslink density of optimization organosilicon epithelium, cross-linked structure etc. finally can obtain the required feel style in multiple market.
The present invention relates to a kind of preparation of crisp oil lubricating organosilicone coating agent, wherein comprise following three components and relevant consumption:
(A) component: the mixture that comprises following component of 100 weight portions: (A1) 10%～80% hydroxy silicon oil, (A2) 20%～50% methyl-silicone oil, (A3) 1%～10% hydrogeneous basic silicone oil, (B) component: the organotin catalysts of 0.1～5 weight portion.(C) component: the coupling agent that contains functional groups such as epoxy radicals, sulfydryl, amino, urea groups of 0.2-2 weight portion.
The mixing of component A, B, C adopts following technology to carry out: in stirred autoclave, add hydroxy silicon oil, methyl-silicone oil successively, start stirring, be warming up to 60～80 ℃ again, stirred 0.5～1 hour, and fully behind the mixing, be cooled to room temperature, add containing hydrogen silicone oil again, continue to stir discharging 0.5 hour.
Among the component A, hydroxy silicon oil is as one of component of dehydrogenation reaction, and the size of its consumption and molecular weight directly influence the compactness extent of organosilicon epithelium, thus the influence curing elasticity and the crisp sense of coating afterwards, its consumption range of choice is 10%～80%, preferred 20%～70%; The viscosity range of choice is 5000～1500000mPa.s, preferred 50000～1000000mPa.s.
Among the component A, containing hydrogen silicone oil is another component of dehydrogenation reaction, and the content of its consumption and protium directly influences the compactness extent of organosilicon epithelium, thereby influences the elasticity and the crisp sense of solidified coating, and its consumption range of choice is 1%～10%, preferred 2%～7%; Its hydrogen content range of choice is 0.1%～1.6%, preferred 0.4%～1.6%.
Among the component A, though methyl-silicone oil does not have reactive group, play the organosilicon epithelium after plasticising is solidified, regulate the effect of crisp and glossy comprehensive feel, its consumption range of choice is 10%～50%, preferred 15%～40%; Its viscosity range of choice is 5000～1000000mPa.s, preferred 50000-500000mPa.s.
Component A is as the colloid of coating agent, in the fabric coating process, suitable viscosity plays a key effect to its film forming on fabric, to make coated fabric possess more high-elastic crisp feel and form the complete organic silicon coat that does not trickle, the viscosity requirement of knifing in the therefore comprehensive fabric coating process, the range of viscosities of component A mixture is 30000～500000mPa.s, preferred 80000～300000mPa.s.
B component is the organotin catalysts of catalytic dehydrogenating reaction, and the consumption increase will promote the degree of depth of dehydrogenation reaction in the coating, increases the density of organosilicon epithelium, thereby improves crisp feel.Specifically can select dibutyl tin laurate, dibutyltin diacetate, two (2 ethyl hexanoic acid) dibutyl tin etc. for use.Amount ranges is 0.1～5 weight portion (the A components of relative 100 weight portions), preferred 0.5～3 weight portion.
Component C can select coupling agents such as 3-glycidyl ether oxygen base propyl trimethoxy silicane, 3-mercaptopropyl trimethoxysilane, 3-aminopropyl trimethoxysilane, 3-(2-aminoethyl)-aminopropyl trimethoxysilane, 3-urea groups propyl trimethoxy silicane for use for promoting the tackifier of coating agent and adhering fabric.Amount ranges is 0.2～2 weight portion (the A components of relative 100 weight portions), preferred 0.5～1 weight portion.
The specific embodiment:
Describe the present invention in detail below in conjunction with embodiment, wherein the coating agent of directly estimating the present invention preparation by artificial digital palpation for examination of trauma is coated in the feel style on the fabric, in following example ranges, 1 representative is the poorest, 5 the representative best, other and the like (crisp sense of wherein undressed blank cloth and glossy sense all are decided to be 1 grade).
Embodiment 1:
In the 20L stirred autoclave, the hydroxy silicon oil, the 5kg viscosity 69495mPa.s methyl-silicone oil that add 10kg viscosity 54593mPa.s successively, start stirring, be warming up to 80 ℃ again, stirred 1 hour, fully behind the mixing, be cooled to room temperature, the containing hydrogen silicone oil that adds 1kg content amount 1.6% again continues to stir discharging 0.5 hour.
With the A component of above-mentioned preparation, take out 10kg, add the glacial acetic acid of 0.1kg earlier, mixing is allocated 0.2kg dibutyl tin laurate and 0.07kg3-mercaptopropyl trimethoxysilane again into, mixing, hardened coating is put into baking oven, and 170 ℃ of baking 1min go out sample, estimate.
Evaluation result; Crisp sense: 5 grades; Glossy sense; 2 grades.
Embodiment 2:
In 20L electrical heating stirred autoclave, the hydroxy silicon oil, the 5kg viscosity 269495mPa.s methyl-silicone oil that add 10kg viscosity 194593mPa.s successively, start stirring, be warming up to 80 ℃ again, stirred 1 hour, fully behind the mixing, be cooled to room temperature, the containing hydrogen silicone oil that adds 1kg content amount 1.6% again continues to stir discharging 0.5 hour.
With the A component of above-mentioned preparation, take out 10kg, add the glacial acetic acid of 0.1kg earlier, mixing is allocated 0.2kg dibutyl tin laurate and 0.07kg3-mercaptopropyl trimethoxysilane again into, mixing, hardened coating is put into baking oven, and 170 ℃ of baking 1min go out sample, estimate.
Evaluation result; Crisp sense: 4 grades; Glossy sense; 4 grades.
Embodiment 3:
In 20L electrical heating stirred autoclave, the hydroxy silicon oil, the 5kg viscosity 69495mPa.s methyl-silicone oil that add 10kg viscosity 54593mPa.s successively, start stirring, be warming up to 80 ℃ again, stirred 1 hour, fully behind the mixing, be cooled to room temperature, the containing hydrogen silicone oil that adds 1kg content amount 1.6% again continues to stir discharging 0.5 hour.
With the A component of above-mentioned preparation, take out 10kg, add the glacial acetic acid of 0.1kg earlier, mixing is allocated 0.05kg dibutyl tin laurate and 0.07kg3-mercaptopropyl trimethoxysilane again into, mixing, hardened coating is put into baking oven, and 170 ℃ of baking 1min go out sample, estimate.
Evaluation result; Crisp sense: 3 grades; Glossy sense; 5 grades.
Embodiment 4:
In 20L electrical heating stirred autoclave, the hydroxy silicon oil, the 9kg viscosity 818376mPa.s methyl-silicone oil that add 6kg viscosity 68373mPa.s successively, start stirring, be warming up to 80 ℃ again, stirred 1 hour, fully behind the mixing, be cooled to room temperature, the containing hydrogen silicone oil that adds 0.8kg content amount 1.0% again continues to stir discharging 0.5 hour.
With the A component of above-mentioned preparation, take out 10kg, add the glacial acetic acid of 0.1kg earlier, mixing, allocate 0.2kg dibutyl tin laurate and 0.06kg3-glycidyl ether oxygen base propyl trimethoxy silicane again into, mixing, hardened coating is put into baking oven, 170 ℃ of baking 1min go out sample, estimate.
Evaluation result; Crisp sense: 4 grades; Glossy sense; 5 grades.
Claims (8)
1. the preparation of a crisp oil lubricating organosilicone coating agent is characterized in that comprising following three components and relevant consumption:
(A) component: the mixture that comprises following component of 100 weight portions: (A1) 10%～80% hydroxy silicon oil, (A2) 20%～50% methyl-silicone oil, (A3) 1%～10% hydrogeneous basic silicone oil, (B) component: the organotin catalysts of 0.1～5 weight portion.(C) component: the coupling agent that contains functional groups such as epoxy radicals, sulfydryl, amino, urea groups of 0.2-2 weight portion.
2. the preparation of a kind of crisp oil lubricating organosilicone coating agent according to claim 1, it is characterized in that in the A component that the mixing of three raw materials adopts following technology to carry out: in stirred autoclave, add hydroxy silicon oil, methyl-silicone oil successively, start stirring, be warming up to 60～80 ℃ again, stirred 0.5～1 hour, fully behind the mixing, be cooled to room temperature, add containing hydrogen silicone oil again, continue to stir discharging 0.5 hour.
3. according to the preparation of claim 1 and 2 described a kind of crisp oil lubricating organosilicone coating agents, it is characterized in that in the A component that the viscosity of hydroxy silicon oil is 5000～1500000mPa.s.
4. according to the preparation of claim 1 and 2 described a kind of crisp oil lubricating organosilicone coating agents, it is characterized in that in the A component that the viscosity of methyl-silicone oil is 5000～1000000mPa.s.
5. according to the preparation of claim 1 and 2 described a kind of crisp oil lubricating organosilicone coating agents, it is characterized in that in the A component that the hydrogen content of containing hydrogen silicone oil is 0.1%～1.6% (percentage by weight).
6. according to the preparation of claim 1 and 2 described a kind of crisp oil lubricating organosilicone coating agents, it is characterized in that A component mixture viscosity is 30000～500000mPa.s.
7. the preparation of a kind of crisp oil lubricating organosilicone coating agent according to claim 1 is characterized in that the B component can select for use dibutyl tin laurate, dibutyltin diacetate, two (2 ethyl hexanoic acid) dibutyl tin etc. as organotin catalysts.
8. the preparation of a kind of crisp oil lubricating organosilicone coating agent according to claim 1 is characterized in that the C component can select for use coupling agents such as 3-glycidyl ether oxygen base propyl trimethoxy silicane, 3-mercaptopropyl trimethoxysilane, 3-aminopropyl trimethoxysilane, 3-(2-aminoethyl)-aminopropyl trimethoxysilane, 3-urea groups propyl trimethoxy silicane as tackifier.
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| CN200810162127A CN101736597A (en) | 2008-11-24 | 2008-11-24 | Preparation of crisp oil lubricating organosilicone coating agent |
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| CN200810162127A CN101736597A (en) | 2008-11-24 | 2008-11-24 | Preparation of crisp oil lubricating organosilicone coating agent |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102965908A (en) * | 2012-11-21 | 2013-03-13 | 际华三五零九纺织有限公司 | Method for radiation curing of pure organic silicone coated fabric by using electron beams |
| CN103898766A (en) * | 2014-02-26 | 2014-07-02 | 巨化集团技术中心 | High-elastic straight organic silicon fabric coating agent and preparation method thereof |
| CN108531075A (en) * | 2018-03-27 | 2018-09-14 | 浙江科技学院 | A kind of preparation method of emulsion-type fabric of organosilicon coating agent |
| CN110437733A (en) * | 2018-05-02 | 2019-11-12 | 深圳Tcl工业研究院有限公司 | A kind of sealing structure and the luminescent device of sealing |
| CN111500067A (en) * | 2020-05-29 | 2020-08-07 | 长兴特殊材料（珠海）有限公司 | Porous organosilicon elastic microsphere and preparation method thereof |
-
2008
- 2008-11-24 CN CN200810162127A patent/CN101736597A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102965908A (en) * | 2012-11-21 | 2013-03-13 | 际华三五零九纺织有限公司 | Method for radiation curing of pure organic silicone coated fabric by using electron beams |
| CN102965908B (en) * | 2012-11-21 | 2015-04-01 | 际华三五零九纺织有限公司 | Method for radiation curing of pure organic silicone coated fabric by using electron beams |
| CN103898766A (en) * | 2014-02-26 | 2014-07-02 | 巨化集团技术中心 | High-elastic straight organic silicon fabric coating agent and preparation method thereof |
| CN108531075A (en) * | 2018-03-27 | 2018-09-14 | 浙江科技学院 | A kind of preparation method of emulsion-type fabric of organosilicon coating agent |
| CN108531075B (en) * | 2018-03-27 | 2020-07-17 | 浙江科技学院 | Preparation method of emulsion type organic silicon fabric coating agent |
| CN110437733A (en) * | 2018-05-02 | 2019-11-12 | 深圳Tcl工业研究院有限公司 | A kind of sealing structure and the luminescent device of sealing |
| CN110437733B (en) * | 2018-05-02 | 2022-04-01 | 深圳Tcl工业研究院有限公司 | Sealing structure and sealed light-emitting device |
| CN111500067A (en) * | 2020-05-29 | 2020-08-07 | 长兴特殊材料（珠海）有限公司 | Porous organosilicon elastic microsphere and preparation method thereof |
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Application publication date: 20100616 |