CN100334137C - Process for preparing anion composite modified organic silicon emulsion with softening and anti-shrinking function - Google Patents
Process for preparing anion composite modified organic silicon emulsion with softening and anti-shrinking function Download PDFInfo
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- CN100334137C CN100334137C CNB2005100380016A CN200510038001A CN100334137C CN 100334137 C CN100334137 C CN 100334137C CN B2005100380016 A CNB2005100380016 A CN B2005100380016A CN 200510038001 A CN200510038001 A CN 200510038001A CN 100334137 C CN100334137 C CN 100334137C
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Abstract
The present invention relates to a preparation method of anion composite modified organosilicon emulsion having the functions of softening and shrink prevention, and the emulsion is mainly used for improving the functions of softness and shrink prevention of fabrics. The preparation method is characterized in that fatty alcohol as an anionic emulsifying agent and peregal as an epoxyethane additional product are adopted and compounded with alkylphenol polyoxyethylene as a nonionic emulsifying agent, composite emulsion is copolymerized and modified among a silane coupling agent (gamma-mercaptopropyl methyl dimethoxy silane), a coupling agent (gamma-aminopropyl triethoxy silane) and an organosilicon monomer by using sulfonic acid as a catalyst to obtain the modified emulsion, and a substituting group of the silane coupling agent and a substituting group of the coupling agent are different. The emulsion prepared by the present invention has a solid content of 21% to 23%, and the appearance of the emulsion is milky. The emulsion performs excellent functions of softening, shrink prevention, washability, relaxation and elasticity on protein fabrics.
Description
Technical field:
The present invention relates to a kind of organic silicon emulsion, especially relate to a kind of anion composite modified organic silicon preparation of microemulsion method that softening and anti-shrinking function is arranged.Be mainly used in the softness that improves fabric, the function of anti-shrinking function.Belong to the auxiliary chemicals technical field.
Background technology:
Organic silicon emulsion plays an important role to the feel of improving fabric, function such as shrinkproof, washable in textile industry.At present, the modified organic silicon emulsion as softening agent is made by two-step approach mostly: synthesize amino-modified silicone oil by mass polymerization earlier, carry out microemulsified with suitable emulsifying agent again.The function of the emulsion of preparation processing fabric sofetening, anti-shrinking function is not ideal in this way.
Summary of the invention:
The objective of the invention is to overcome above-mentioned deficiency, a kind of preparation method that fabric has the anion composite modified organic silicon emulsion of softness, anti-shrinking function that handles is provided.
The object of the present invention is achieved like this: a kind of preparation method that the anion composite modified organic silicon emulsion of softening and anti-shrinking function is arranged, it is to adopt anionic emulsifier Fatty Alcohol(C12-C14 and C12-C18) and ethylene oxide adduct paregal O
25Composite with the nonionic emulsifying agent alkylphenol polyoxyethylene, sulfonic acid is catalyzer, silane coupling agent γ-mercapto propyl group methyl dimethoxysilane, coupling agent γ-An Bingjisanyiyangjiguiwan and the organosilane monomer of two kinds of different substituents are carried out the composite emulsion modification by copolymerization, made milky modified emulsion, its preparation method comprises the steps:
A) coupling agent γ-mercapto propyl group methyl dimethoxysilane, coupling agent γ-An Bingjisanyiyangjiguiwan and octamethylcyclotetrasiloxane are mixed by proportioning make mixture;
B) with water, sulfonic acid, Fatty Alcohol(C12-C14 and C12-C18) and ethylene oxide adduct paregal O
25, the two fat of alkylphenol polyoxyethylene, oleic acid list drop in the reactor by proportioning, stir, and are warming up to 50 ℃ ± 5 ℃, are incubated 1 hour ± 0.5 hour;
C) mixture that a) makes is added dropwise to b) system in, keep 60min～120min, slowly be warming up to 70 ℃～80 ℃ then, be incubated 5～6 hours, cooling, neutralization is filtered, discharging, gets the oyster white anion composite modified organic silicon emulsion.
The consumption of each raw material accounts for the weight percent of raw material total amount and is in the mixed solution of step a): coupling agent γ-mercapto propyl group methyl dimethoxysilane 0.1%～0.2%, coupling agent γ-An Bingjisanyiyangjiguiwan 0.2%～0.4%, octamethylcyclotetrasiloxane 16%～17%;
The consumption of each raw material of mixed system accounts for the weight percent of raw material total amount and is in the step b): water 75%～80%, sulfonic acid 2.5%～3.5%, alkylphenol polyoxyethylene 0.5%～1.0%, oleic acid list two fat 0.9%～1.2%, Fatty Alcohol(C12-C14 and C12-C18) and ethylene oxide adduct paregal Os
250.1%～0.25%.
The silane coupling agent of the strong reactive behavior of coupling agent γ-mercapto propyl group methyl dimethoxysilane a kind of containing-SH.It can give particularly woollens anti-shrinking function of fabric.
The coupling agent γ-An Bingjisanyiyangjiguiwan is the mono amino silane coupling agent of using always, is the important source material of textile auxiliary.
With the silane coupling agent compound modified organic silicon emulsion of these two kinds of different functional groups, in conjunction with the advantage of two kinds of coupling agents, the emulsion that makes has fabulous softness, anti-shrinking function to fabric.
The emulsion of the present invention's preparation, its solid content is 21%～23%, appearance milky white.This emulsion has fabulous softness, shrinkproof, washable elasticity function to the protein fabric.
Embodiment:
Embodiment 1:
A) 0.5g coupling agent γ-mercapto propyl group methyl dimethoxysilane, 1.5g coupling agent γ-An Bingjisanyiyangjiguiwan and 67g octamethylcyclotetrasiloxane are mixed make mixture;
B) with 312g water, 12g sulfonic acid, 2g alkylphenol polyoxyethylene, the two fat of 4g oleic acid list and 0.8g Fatty Alcohol(C12-C14 and C12-C18) and ethylene oxide adduct paregal O
25Drop in the there-necked flask, begin then to stir, be warmed up to 50 ℃, be incubated 1 hour;
C) mixture that a) makes is added dropwise to b) system in, keep 120min, slowly be warming up to 75 ℃ then, be incubated 6 hours, fast cooling to 40 ℃, neutralization is filtered, discharging, must the oyster white anion composite modified organic silicon emulsion.This emulsion can make protein fabric sofetening, shrinkproof.
Embodiment 2:
A) 0.7g coupling agent γ-mercapto propyl group methyl dimethoxysilane, 1.4g coupling agent γ-An Bingjisanyiyangjiguiwan and 67g octamethylcyclotetrasiloxane are mixed make mixture;
B) with 312g water, 12g sulfonic acid, 2g alkylphenol polyoxyethylene, the two fat of 4g oleic acid list and 0.8g ethylene oxide adduct paregal O
25Drop in the there-necked flask, begin then to stir, be warmed up to 55 ℃, be incubated 1.5 hours;
C) mixture that a) makes is added dropwise to b) system in, keep 60min, slowly heat up then
To 80 ℃, be incubated 5 hours, fast cooling to 40 ℃, neutralization is filtered, discharging, the oyster white anion composite modified organic silicon emulsion.This emulsion can make protein fabric sofetening, shrinkproof, loose bullet.
Embodiment 3:
A) 0.8g coupling agent γ-mercapto propyl group methyl dimethoxysilane, 1g coupling agent γ-An Bingjisanyiyangjiguiwan and 67g octamethylcyclotetrasiloxane are mixed make mixture;
B) with 312g water, 12g sulfonic acid, 2g alkylphenol polyoxyethylene, the two fat of 4g oleic acid list and 0.8g ethylene oxide adduct paregal O
25Drop in the there-necked flask, begin then to stir, be warmed up to 50 ℃, be incubated 0.5 hour;
C) mixture that a) makes is added dropwise to b) system in, keep 120min, slowly heat up then
To 70 ℃, be incubated 6 hours, fast cooling to 40 ℃, neutralization is filtered, discharging, the oyster white anion composite modified organic silicon emulsion.This emulsion can make protein fabric sofetening, shrinkproof, loose bullet.
Claims (2)
1, a kind of preparation method that the anion composite modified organic silicon emulsion of softening and anti-shrinking function is arranged is characterized in that it is to adopt anionic emulsifier Fatty Alcohol(C12-C14 and C12-C18) and ethylene oxide adduct paregal O
25Composite with the nonionic emulsifying agent alkylphenol polyoxyethylene, sulfonic acid is catalyzer, silane coupling agent γ-mercapto propyl group methyl dimethoxysilane, coupling agent γ-An Bingjisanyiyangjiguiwan and the organosilane monomer of two kinds of different substituents are carried out the composite emulsion modification by copolymerization, made modified emulsion, its preparation method comprises the steps:
A) coupling agent γ-mercapto propyl group methyl dimethoxysilane, coupling agent γ-An Bingjisanyiyangjiguiwan and octamethylcyclotetrasiloxane are mixed by proportioning make mixture;
B) with water, sulfonic acid, Fatty Alcohol(C12-C14 and C12-C18) and ethylene oxide adduct paregal O
25, the two fat of alkylphenol polyoxyethylene, oleic acid list drop in the reactor by proportioning, stir, and are warming up to 50 ℃ ± 5 ℃, are incubated 1 hour ± 0.5 hour;
C) mixture that a) makes is added dropwise to b) system in, keep 60min～120min, slowly be warming up to 70 ℃～80 ℃ then, be incubated 5～6 hours, cooling, neutralization is filtered, discharging, gets anion composite modified organic silicon emulsion.
2, a kind of preparation method that the anion composite modified organic silicon emulsion of softening and anti-shrinking function is arranged according to claim 1 is characterized in that:
The consumption of each raw material accounts for the weight percent of raw material total amount and is in the mixed solution of step a): coupling agent γ-mercapto propyl group methyl dimethoxysilane 0.1%～0.2%, coupling agent γ-An Bingjisanyiyangjiguiwan 0.2%～0.4%, octamethylcyclotetrasiloxane 16%～17%;
The consumption of each raw material of mixed system accounts for the weight percent of raw material total amount and is in the step b): water 75%～80%, sulfonic acid 2.5%～3.5%, alkylphenol polyoxyethylene 0.5%～1.0%, oleic acid list two fat 0.9%～1.2%, Fatty Alcohol(C12-C14 and C12-C18) and ethylene oxide adduct paregal Os
250.1%～0.25%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100380016A CN100334137C (en) | 2005-03-07 | 2005-03-07 | Process for preparing anion composite modified organic silicon emulsion with softening and anti-shrinking function |
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| CNB2005100380016A CN100334137C (en) | 2005-03-07 | 2005-03-07 | Process for preparing anion composite modified organic silicon emulsion with softening and anti-shrinking function |
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| CN1683438A CN1683438A (en) | 2005-10-19 |
| CN100334137C true CN100334137C (en) | 2007-08-29 |
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| CNB2005100380016A Expired - Fee Related CN100334137C (en) | 2005-03-07 | 2005-03-07 | Process for preparing anion composite modified organic silicon emulsion with softening and anti-shrinking function |
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| CN109851791A (en) * | 2018-12-27 | 2019-06-07 | 广东银洋环保新材料有限公司 | A kind of anionic amino modified organic silicon emulsion and the preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1030435A (en) * | 1987-06-25 | 1989-01-18 | 信越化学工业株式会社 | Silicon resin composition |
| CN1405209A (en) * | 2002-11-04 | 2003-03-26 | 东华大学 | Fluoro organosilicon polymer preparation and application |
| US20040242768A1 (en) * | 2003-06-02 | 2004-12-02 | Butts Matthew David | Silicone based flame retardant systems for textiles |
| CN1569925A (en) * | 2004-04-29 | 2005-01-26 | 上海高分子材料研究开发中心 | Novel configuration phenyl methyl silicon oil |
-
2005
- 2005-03-07 CN CNB2005100380016A patent/CN100334137C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1030435A (en) * | 1987-06-25 | 1989-01-18 | 信越化学工业株式会社 | Silicon resin composition |
| CN1405209A (en) * | 2002-11-04 | 2003-03-26 | 东华大学 | Fluoro organosilicon polymer preparation and application |
| US20040242768A1 (en) * | 2003-06-02 | 2004-12-02 | Butts Matthew David | Silicone based flame retardant systems for textiles |
| CN1569925A (en) * | 2004-04-29 | 2005-01-26 | 上海高分子材料研究开发中心 | Novel configuration phenyl methyl silicon oil |
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