CN102911363A - Preparation method for nitrogenous silane coupling agent blocked polyether block silicone oil - Google Patents
Preparation method for nitrogenous silane coupling agent blocked polyether block silicone oil Download PDFInfo
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- CN102911363A CN102911363A CN2012104349417A CN201210434941A CN102911363A CN 102911363 A CN102911363 A CN 102911363A CN 2012104349417 A CN2012104349417 A CN 2012104349417A CN 201210434941 A CN201210434941 A CN 201210434941A CN 102911363 A CN102911363 A CN 102911363A
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Abstract
The invention discloses a preparation method for nitrogenous silane coupling agent blocked polyether block silicone oil, which has the advantages of capability of industrialized production, simple technology, low cost and capability of improving current performance. According to the method, the materials by weight part are as follows: 1,000 parts of epoxidized polyether silicon oil with molecular weight of 10,000, 2-6 parts of nitrogenous silane coupling agent and 20 parts of isopropyl alcohol; reaction under 80-85 DEG C is carried out for 3 hours; pressure reduction and vacuum pumping are carried out to achieve that the degree of vacuum is 0.09 Mpa per 30 minutes; a transparent pasty liquid is obtained; and the molar ratio of the epoxy base of the nitrogenous silane coupling agent to that of the epoxidized polyether silicon oil is 1:1. The method has the characteristics of simple technology, convenience in use and realization in mass production.
Description
Technical field
The present invention relates to a kind of preparation method of polyether block silicone oil of nitrogenous silane coupling agent end-blocking.
Background technology
Along with the raising of people's living standard is also more and more higher to the requirement of fine chemical product performance.Past is because the characteristic such as the surfactivity of dimethyl silicone oil is high, chemical stability reaches well high-low temperature resistant and being accepted by people.Because its special reactivity, adsorptivity, cross-linking type are given again in the introducing of epoxide group, so that having had in fields such as fibre finish, resin modified, the antiseized separant of photocuring, paint additives widely, used by epoxide modified silicone oil afterwards.But along with the fast development of science and technology and the end ring oxygen silicone oil product of continually developing of product innovation have substituted the dimethyl-silicon oil production that contains epoxide group gradually.The epoxy silicon oil reactive behavior is high, finishing composition as fabric, can with the reactions such as the hydroxyl of fiber surface, amino, carboxyl, the fabric of giving fabric persistence soft effect, arrangement is washable, not yellowing, the composite use of epoxy silicon oil and amido silicon oil, can also make fiber produce the same feel of similar wool, and have shrinkproof, wrinkle resistant effect.
End ring oxygen silicone oil has following purposes: 1, utilize its flexible smooth, and water-absorbent is used for processing textiles particularly cotton, towel, sheet, underwear etc., the fabric sofetening after the processing, smooth, absorbing sweat is ventilative, and is comfortable and easy to wear.
2, utilize its low surface tension and radiation hardness, ageing-resistant, resistant of high or low temperature can be used as the interior interpolation antifogging agent of plastic greenhouse film, and the plastic greenhouse film of producing (without dripping a film) has well antifog, preventing water drops, good transmittance.
3, as fibre finishing, the static inhibitor of plastics etc. and the release agent of fabric fibre.
4, as defoamer, and the flow agent of some coating.
Existing problems, present polyether block silicone oil can not be realized suitability for industrialized production, complex process, the problems such as production cost height, simultaneously the performance of each side is abundant not, and existing performance capability a little less than.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of can suitability for industrialized production, technique is simple, cost is low, improves the preparation method of polyether block silicone oil of the nitrogenous silane coupling agent end-blocking of existing performance.Molecular weight is 10000 end ring oxygen polyether silicone oil when being 100 parts by weight, and nitrogenous one type of silane coupling agent is 2-6 part, 20 parts of Virahols, and 80-85 degree reaction 3 hours, decompression vacuum pumping, described vacuum tightness is 0.09Mpa30 minute, gets transparent thick liquid; The mol ratio of the epoxy group(ing) in described nitrogenous one type of silane coupling agent and the end ring oxygen polyether silicone oil is 1:1.
This product can be used as intermediate or directly uses has good effect.
Described nitrogenous one type of silane coupling agent can be one or more mixtures in N-β-aminoethyl-γ-aminopropyl methyl dimethoxysilane, N-ring ethyl-γ-aminopropyl methyl dimethoxysilane, γ-divinyl triammonium propyl group methyl dimethoxysilane, N-β-aminoethyl-γ-aminopropyl methyltrimethoxy silane, γ-piperazinyl propyl group methyl dimethoxysilane, γ-aminopropyl triethoxysilane, the N-γ dimethylamino-γ γ-aminopropyl methyl dimethoxysilane.
Have according to above-described preparation method that technique is simple, easy to use, the characteristics such as accomplish scale production.
Embodiment
Embodiment 1:
Molecular weight is 10000 end ring oxygen polyether silicone oil during by weight for 100kg, and N-β-aminoethyl-γ-aminopropyl methyl dimethoxysilane is 4.27kg, Virahol 20kg, 80-85 degree reaction 3 hours, decompression vacuum pumping, described vacuum tightness is 0.09Mpa30 minute, gets transparent thick liquid.
Embodiment 2:
Molecular weight is 10000 end ring oxygen polyether silicone oil during by weight for 100kg, and γ-aminopropyl triethoxysilane is 4.56kg, Virahol 20kg, 80-85 degree reaction 3 hours, decompression vacuum pumping, described vacuum tightness is 0.09Mpa30 minute, gets transparent thick liquid.
Embodiment 3:
Molecular weight is that 10000 end ring oxygen polyether silicone oil is during by weight for 100kg, N-β-aminoethyl-γ-aminopropyl methyl dimethoxysilane is that 2.14kg, γ-aminopropyl triethoxysilane are 2.28 grams, Virahol 20kg, 80-85 degree reaction 3 hours, decompression vacuum pumping, described vacuum tightness is 0.09Mpa30 minute, gets transparent thick liquid.
Claims (2)
1. the preparation method of the polyether block silicone oil of a nitrogenous silane coupling agent end-blocking, it is characterized in that: molecular weight is that 10000 end ring oxygen polyether silicone oil is when being 100 parts by weight, nitrogenous one type of silane coupling agent is 2-6 part, 20 parts of Virahols, 80-85 degree reaction 3 hours, decompression vacuum pumping, described vacuum tightness is 0.09Mpa30 minute, gets transparent thick liquid; The mol ratio of the epoxy group(ing) in described nitrogenous one type of silane coupling agent and the end ring oxygen polyether silicone oil is 1:1.
2. the preparation method of the polyether block silicone oil of a kind of nitrogenous silane coupling agent end-blocking according to claim 1, it is characterized in that: described nitrogenous one type of silane coupling agent is N-β-aminoethyl-γ-aminopropyl methyl dimethoxysilane, N-encircles ethyl-γ-aminopropyl methyl dimethoxysilane, γ-divinyl triammonium propyl group methyl dimethoxysilane, N-β-aminoethyl-γ-aminopropyl methyltrimethoxy silane, γ-piperazinyl propyl group methyl dimethoxysilane, γ-aminopropyl triethoxysilane, one or more mixtures in N-γ dimethylamino-γ γ-aminopropyl methyl dimethoxysilane.
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| CN2012104349417A CN102911363A (en) | 2012-11-02 | 2012-11-02 | Preparation method for nitrogenous silane coupling agent blocked polyether block silicone oil |
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| CN2012104349417A CN102911363A (en) | 2012-11-02 | 2012-11-02 | Preparation method for nitrogenous silane coupling agent blocked polyether block silicone oil |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104031269A (en) * | 2014-05-20 | 2014-09-10 | 江阴市诺科科技有限公司 | Hydrophilic block polyether amino silicone oil with amino branched chain, and preparation method and application thereof |
| CN105694046A (en) * | 2016-02-06 | 2016-06-22 | 浙江汉邦化工有限公司 | Preparation method of highly-branched block polyether-aminosiloxane finishing agent |
| CN106497600A (en) * | 2016-11-16 | 2017-03-15 | 中海油天津化工研究设计院有限公司 | A kind of offshore oilfield Produced Liquid comprehensive treatment agent and preparation method thereof |
| CN107033353A (en) * | 2017-02-21 | 2017-08-11 | 苏州市邦涔高分子科技有限公司 | A kind of preparation method and application of softening agent |
| CN114133573A (en) * | 2021-10-27 | 2022-03-04 | 浙江汉邦新材料股份有限公司 | Environment-friendly odorless hydrophilic organic silicon softening agent for wool tops and preparation method thereof |
| CN116284799A (en) * | 2023-03-09 | 2023-06-23 | 深圳天鼎新材料有限公司 | Organosilicon elastomer prepolymer emulsion softener and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101503515A (en) * | 2009-03-04 | 2009-08-12 | 深圳天鼎精细化工制造有限公司 | Method for synthesizing hydrophile amino silicon oil |
| CN102516549A (en) * | 2011-12-16 | 2012-06-27 | 浙江汉邦化工有限公司 | Method for synthesizing main chain block polyether hydrophilic amino silicone oil |
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2012
- 2012-11-02 CN CN2012104349417A patent/CN102911363A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101503515A (en) * | 2009-03-04 | 2009-08-12 | 深圳天鼎精细化工制造有限公司 | Method for synthesizing hydrophile amino silicon oil |
| CN102516549A (en) * | 2011-12-16 | 2012-06-27 | 浙江汉邦化工有限公司 | Method for synthesizing main chain block polyether hydrophilic amino silicone oil |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104031269A (en) * | 2014-05-20 | 2014-09-10 | 江阴市诺科科技有限公司 | Hydrophilic block polyether amino silicone oil with amino branched chain, and preparation method and application thereof |
| CN105694046A (en) * | 2016-02-06 | 2016-06-22 | 浙江汉邦化工有限公司 | Preparation method of highly-branched block polyether-aminosiloxane finishing agent |
| CN106497600A (en) * | 2016-11-16 | 2017-03-15 | 中海油天津化工研究设计院有限公司 | A kind of offshore oilfield Produced Liquid comprehensive treatment agent and preparation method thereof |
| CN106497600B (en) * | 2016-11-16 | 2018-06-26 | 中海油天津化工研究设计院有限公司 | A kind of offshore oilfield Produced Liquid comprehensive treatment agent and preparation method thereof |
| CN107033353A (en) * | 2017-02-21 | 2017-08-11 | 苏州市邦涔高分子科技有限公司 | A kind of preparation method and application of softening agent |
| CN114133573A (en) * | 2021-10-27 | 2022-03-04 | 浙江汉邦新材料股份有限公司 | Environment-friendly odorless hydrophilic organic silicon softening agent for wool tops and preparation method thereof |
| CN116284799A (en) * | 2023-03-09 | 2023-06-23 | 深圳天鼎新材料有限公司 | Organosilicon elastomer prepolymer emulsion softener and preparation method and application thereof |
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Application publication date: 20130206 |