CN1927910A - Preparation method of amino/epoxy co-modified hydrophilic silicone oil - Google Patents
Preparation method of amino/epoxy co-modified hydrophilic silicone oil Download PDFInfo
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- CN1927910A CN1927910A CN 200610096030 CN200610096030A CN1927910A CN 1927910 A CN1927910 A CN 1927910A CN 200610096030 CN200610096030 CN 200610096030 CN 200610096030 A CN200610096030 A CN 200610096030A CN 1927910 A CN1927910 A CN 1927910A
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Abstract
The present invention relates to preparation process of amino/epoxy co-modified hydrophilic silicone oil, and features that under the action of chain transfer agent and catalyst, silicone oil with low hydrogen content and polyether are first reacted, and amino couplant and epoxy couplant are then introduced to prepare the amino/epoxy co-modified hydrophilic silicone oil. The amino/epoxy co-modified hydrophilic silicone oil has high water solubility and good color, and is used in finishing fabric, and the finished fabric has very low surface tension, water contacting angle greater than 150 deg and excellent hand feeling.
Description
Technical field
The present invention relates to a kind of amino-modified silicone oil emulsion, especially relate to a kind of preparation method of amino/epoxy co-modified hydrophilic silicone oil.Belong to field of chemical technology.
Background technology
The amino-modified silicone oil emulsion is because of its distinctive softness, is widely used in the soft function arrangement of textiles, itself and the crosslinked film forming of fabric, but this film water dissolubility is poor, so when fabric need rearrange, silicon oil membrane was difficult for removing, the performance of returning something for repairs is bad.The CGF hydrophilic silicone oil of supplying on the market, production technique is simple, and good water solubility is hydrophilic level and smooth, can return something for repairs, but its not water-fast washing, no softness.
Summary of the invention
The objective of the invention is to overcome above-mentioned deficiency, provide a kind of hydrophilic, simultaneously can give the preparation method of the amino/epoxy co-modified hydrophilic silicone oil of fabric sofetening performance again.
The object of the present invention is achieved like this: a kind of preparation method of amino/epoxy co-modified hydrophilic silicone oil, it is characterized in that: adopt silicon oil of low hydrogen content and polyethers under chain-transfer agent, catalyst action, to react, introducing contains amino coupling agent and contains the epoxy group(ing) coupling agent again, prepares amino/epoxy co-modified hydrophilic silicon oil.
Concrete preparation method of the present invention is: silicon oil of low hydrogen content, polyethers and Virahol are dropped in the reactor, be warming up to 90 ℃ ± 5 ℃, stirred 3 ± 0.5 hours, be added dropwise to 2% isopropyl alcohol solution of chloroplatinic acid after, stirred 3 hours ± 0.5 hour, be added dropwise to 2% isopropyl alcohol solution of chloroplatinic acid again, restir 3 hours ± 0.5 hour is cooled to 70 ℃ ± 5 ℃, adds to contain amino coupling agent and contain the epoxy group(ing) coupling agent, stirred 3 hours ± 0.5 hour, and got amino/epoxy co-modified silicone oil product after vacuumizing.
Polyethers of the present invention is F-6 or glycidyl allyl ether; Or be the mixed ether of F-6 and glycidyl allyl ether, F-6 accounts for the 0.8-1.2 massfraction of silicon oil of low hydrogen content in the mixed ether, and glycidyl allyl ether accounts for the 0.05-0.08 massfraction of silicon oil of low hydrogen content.
Chain-transfer agent of the present invention is a Virahol, and chain-transfer agent accounts for 0.5 massfraction of silicon oil of low hydrogen content; Catalyzer is 2% isopropyl alcohol solution of chloroplatinic acid.
The present invention uses contains amino coupling agent and can be γ-An Bingjisanyiyangjiguiwan, N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane, N-cyclohexyl-γ-aminopropyl methyl dimethoxysilane, γ-diethylenetriamine propyl group methyl dimethoxysilane, N-(β-aminoethyl)-γ-An Bingjisanjiayangjiguiwan; Containing the epoxy group(ing) coupling agent is δ-aminopropyl triethoxysilane.
The fabric that the amino/epoxy co-modified sillicon oil treatment of the present invention's preparation goes out has extremely low surface tension, spends greater than 150 with the contact angle of water.Therefore show superior feel.The silicone oil good water solubility of preparation, the color color and luster is good.The existing good flexibility of the fabric of putting in order out, fluffiness, smooth property can be returned something for repairs again, not brightness reversion.
Embodiment
Embodiment 1:
With silicon oil of low hydrogen content 38kg, 36kgF-6,2.3kg glycidyl allyl ether, the 19kg Virahol drops in the reactor, is warming up to 90 ℃, stirs 3 hours, after being added dropwise to 2% the isopropyl alcohol solution of chloroplatinic acid that contains 50g, stirred 3 hours, and be added dropwise to 2% the isopropyl alcohol solution of chloroplatinic acid that contains 50g again, restir 3 hours.Be cooled to 70 ℃, add γ-An Bingjisanyiyangjiguiwan, N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane, N-cyclohexyl-γ-aminopropyl methyl dimethoxysilane, γ-diethylenetriamine propyl group methyl dimethoxysilane or N-(β-aminoethyl)-γ-An Bingjisanjiayangjiguiwan 2.0kg, δ-aminopropyl triethoxysilane 2.1kg, stirred 3 hours, and got amino/epoxy co-modified silicone oil product after vacuumizing.
Embodiment 2: embodiment 2 is that with the difference of embodiment 1 polyethers adopts the F-6 of 38.3kg separately, and all the other are all with embodiment 1.
Embodiment 3: embodiment 3 is that with the difference of embodiment 1 polyethers adopts the glycidyl allyl ether of 38.3kg separately, and all the other are all with embodiment 1.
Claims (5)
1, a kind of preparation method of amino/epoxy co-modified hydrophilic silicone oil, it is characterized in that: adopt silicon oil of low hydrogen content and polyethers under chain-transfer agent, catalyst action, to react, introducing contains amino coupling agent and contains the epoxy group(ing) coupling agent again, prepares amino/epoxy co-modified hydrophilic silicon oil.
2, the preparation method of a kind of amino/epoxy co-modified hydrophilic silicone oil according to claim 1, it is characterized in that: with silicon oil of low hydrogen content, polyethers and Virahol drop in the reactor, be warming up to 90 ℃ ± 5 ℃, stirred 3 ± 0.5 hours, after being added dropwise to 2% isopropyl alcohol solution of chloroplatinic acid, stirred 3 hours ± 0.5 hour, be added dropwise to 2% isopropyl alcohol solution of chloroplatinic acid again, restir 3 hours ± 0.5 hour, be cooled to 70 ℃ ± 5 ℃, adding contains amino coupling agent and contains the epoxy group(ing) coupling agent, stirs 3 hours ± 0.5 hour, gets amino/epoxy co-modified silicone oil product after vacuumizing.
3, the preparation method of a kind of amino/epoxy co-modified hydrophilic silicone oil according to claim 1 and 2 is characterized in that: described polyethers is F-6 or glycidyl allyl ether; Or be the mixed ether of F-6 and glycidyl allyl ether, F-6 accounts for the 0.8-1.2 massfraction of silicon oil of low hydrogen content in the mixed ether, and glycidyl allyl ether accounts for the 0.05-0.08 massfraction of silicon oil of low hydrogen content.
4, the preparation method of a kind of amino/epoxy co-modified hydrophilic silicone oil according to claim 1 and 2 is characterized in that: described chain-transfer agent is a Virahol, and chain-transfer agent accounts for 0.5 massfraction of silicon oil of low hydrogen content; Described catalyzer is 2% isopropyl alcohol solution of chloroplatinic acid.
5, the preparation method of a kind of amino/epoxy co-modified hydrophilic silicone oil according to claim 1 and 2, it is characterized in that: the described amino coupling agent that contains is a γ-An Bingjisanyiyangjiguiwan, N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane, N-cyclohexyl-γ-aminopropyl methyl dimethoxysilane, γ-diethylenetriamine propyl group methyl dimethoxysilane or N-(β-aminoethyl)-γ-An Bingjisanjiayangjiguiwan; Containing the epoxy group(ing) coupling agent is δ-aminopropyl triethoxysilane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 200610096030 CN1927910A (en) | 2006-09-14 | 2006-09-14 | Preparation method of amino/epoxy co-modified hydrophilic silicone oil |
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| CN 200610096030 CN1927910A (en) | 2006-09-14 | 2006-09-14 | Preparation method of amino/epoxy co-modified hydrophilic silicone oil |
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| CN1927910A true CN1927910A (en) | 2007-03-14 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101497697B (en) * | 2008-07-11 | 2011-05-18 | 浙江传化股份有限公司 | Preparation of block water-soluble silicon oil |
| CN102250358A (en) * | 2011-05-18 | 2011-11-23 | 黄山市强力化工有限公司 | Block type amino polyether modified silicone oil and preparation method thereof |
| CN101503515B (en) * | 2009-03-04 | 2012-01-18 | 深圳天鼎精细化工制造有限公司 | Method for synthesizing hydrophile amino silicon oil |
| CN102432887A (en) * | 2011-08-12 | 2012-05-02 | 浙江精业生化有限公司 | Preparation method of polyester-modified silica gel |
| CN103193984A (en) * | 2012-01-04 | 2013-07-10 | 安徽科光新材料有限公司 | Hydrophilic aminosilicon oil, and preparation method and uses thereof |
| CN103333339A (en) * | 2013-06-04 | 2013-10-02 | 黄山市强力化工有限公司 | Method for preparing hydroxyl-terminated phenyl amino polyether modified silicone oil |
| CN115652641A (en) * | 2022-10-13 | 2023-01-31 | 英德市东鸿化工科技有限公司 | Preparation method and application of raising agent |
-
2006
- 2006-09-14 CN CN 200610096030 patent/CN1927910A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101497697B (en) * | 2008-07-11 | 2011-05-18 | 浙江传化股份有限公司 | Preparation of block water-soluble silicon oil |
| CN101503515B (en) * | 2009-03-04 | 2012-01-18 | 深圳天鼎精细化工制造有限公司 | Method for synthesizing hydrophile amino silicon oil |
| CN102250358A (en) * | 2011-05-18 | 2011-11-23 | 黄山市强力化工有限公司 | Block type amino polyether modified silicone oil and preparation method thereof |
| CN102250358B (en) * | 2011-05-18 | 2012-09-05 | 黄山市强力化工有限公司 | Block type amino polyether modified silicone oil and preparation method thereof |
| CN102432887A (en) * | 2011-08-12 | 2012-05-02 | 浙江精业生化有限公司 | Preparation method of polyester-modified silica gel |
| CN102432887B (en) * | 2011-08-12 | 2013-03-27 | 绍兴县震东化工有限公司 | Preparation method of polyester-modified silica gel |
| CN103193984A (en) * | 2012-01-04 | 2013-07-10 | 安徽科光新材料有限公司 | Hydrophilic aminosilicon oil, and preparation method and uses thereof |
| CN103333339A (en) * | 2013-06-04 | 2013-10-02 | 黄山市强力化工有限公司 | Method for preparing hydroxyl-terminated phenyl amino polyether modified silicone oil |
| CN103333339B (en) * | 2013-06-04 | 2016-08-10 | 黄山市强力化工有限公司 | A kind of hydroxy-end capped phenyl amino polyether modified silicon oil |
| CN115652641A (en) * | 2022-10-13 | 2023-01-31 | 英德市东鸿化工科技有限公司 | Preparation method and application of raising agent |
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