CN100334133C - Process for preparing cation composite modified organic silicon emulsion with softening, slipping and elastic function - Google Patents
Process for preparing cation composite modified organic silicon emulsion with softening, slipping and elastic function Download PDFInfo
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- CN100334133C CN100334133C CNB2005100380069A CN200510038006A CN100334133C CN 100334133 C CN100334133 C CN 100334133C CN B2005100380069 A CNB2005100380069 A CN B2005100380069A CN 200510038006 A CN200510038006 A CN 200510038006A CN 100334133 C CN100334133 C CN 100334133C
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- methyl dimethoxysilane
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Abstract
The present invention relates to a preparation method of cation composite modified organosilicon emulsion having the functions of softening, smoothening and elasticity. The emulsion is mainly used for improving the functions of softness, smoothness and elasticity of fabrics. The preparation method is characterized in that cetyl trimethyl ammonium chloride as a cationic emulsifying agent is adopted and compounded with alkylphenol polyoxyethylene as a nonionic emulsifying agent, composite emulsion is copolymerized and modified among a silane coupling agent (gamma-aminopropyl triethoxy silane), a coupling agent (N-(beta-aminoethyl)-gamma-aminopropyl methyl dimethoxy silane), a coupling agent (N-cyclohexyl-gamma-aminopropyl methyl dimethoxy silane) and an organosilicon monomer by using potassium hydroxide as a catalyst to obtain the semitransparent modified emulsion, and a substituting group of the silane coupling agent, a substituting group of the second coupling agent and a substituting group of the third coupling agent are different. The appearance of the emulsion prepared by the present invention is semitransparent, and the emulsion performs excellent functions of softening and elasticity on fabrics.
Description
Technical field:
The present invention relates to a kind of organic silicon emulsion, especially relate to a kind of preparation method that the cation composite modified organic silicon emulsion of softening, slipping and elastic function is arranged.Be mainly used in the softness, smooth, the elasticity function that improve fabric.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.In this way the emulsion of preparation handle fabric sofetening, smooth, elasticity function is not ideal.
Summary of the invention:
The objective of the invention is to overcome above-mentioned deficiency, a kind of preparation method that fabric has the cation composite modified organic silicon emulsion of softening, slipping and elastic function that handles is provided.
The object of the present invention is achieved like this: a kind of preparation method that the cation composite modified organic silicon emulsion of softening, slipping and elastic function is arranged, it is to adopt cationic emulsifier cetyl trimethyl ammonia chloride, composite with the nonionic emulsifying agent alkylphenol polyoxyethylene, potassium hydroxide is catalyzer, silane coupling agent γ-An Bingjisanyiyangjiguiwan with three kinds of different substituents, coupling agent N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane, coupling agent N-cyclohexyl-γ-aminopropyl methyl dimethoxysilane and organosilane monomer carry out the composite emulsion modification by copolymerization, made translucent modified emulsion, its preparation method comprises the steps:
A) coupling agent γ-An Bingjisanyiyangjiguiwan, coupling agent N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane, coupling agent N-cyclohexyl-γ-aminopropyl methyl dimethoxysilane and octamethylcyclotetrasiloxane are mixed by proportioning make mixture;
B) cationic emulsifier cetyl trimethyl ammonia chloride, catalyzer potassium hydroxide, nonionic emulsifying agent alkylphenol polyoxyethylene, the two fat of oleic acid list and water are dropped in the reactor by proportioning, begin then to stir, be warming up to 50 ℃ ± 5 ℃;
C) mixture that a) makes is added dropwise to b) system in, keep 60min～120min, slowly be warming up to 80 ℃～85 ℃ then, be incubated 5～6 hours, cooling, neutralization is filtered, discharging, gets translucent cation 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-An Bingjisanyiyangjiguiwan 0.1%～0.3%, coupling agent N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane 0.10%～0.14%, coupling agent N-cyclohexyl-γ-aminopropyl methyl dimethoxysilane 0.10%～0.14%, octamethylcyclotetrasiloxane 12%～13%;
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): cetyl trimethyl ammonia chloride 1.4%～1.5%, potassium hydroxide 0.45%～0.5%, alkylphenol polyoxyethylene 3.9%～7.1%, the two fat 2.4%～4.3% of oleic acid list, water 75%～80%.
The coupling agent γ-An Bingjisanyiyangjiguiwan is the mono amino silane coupling agent of using always.
Coupling agent N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane is a kind of silane coupling agent of two functional group's diamines.It can give fabric super soft feel(ing).
Coupling agent N-cyclohexyl-γ-aminopropyl methyl dimethoxysilane is a kind of silane coupling agent of two functional group's monoamines.Its specific functional groups can give the sense of fabric particularly soft, fabulous whiteness and better hydrophilicity.
With the silane coupling agent compound modified organic silicon emulsion of these three kinds of different functional groups, in conjunction with the advantage of three kinds of coupling agents, the emulsion that makes has fabulous softness, smooth, elasticity function to fabric.
The emulsion of the present invention's preparation, its solid content is 20%～22%, outward appearance is translucent
Embodiment:
Embodiment 1:
A) 0.6g coupling agent γ-An Bingjisanyiyangjiguiwan, 0.2g coupling agent N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane, 0.2g coupling agent N-cyclohexyl-γ-aminopropyl methyl dimethoxysilane and 26g octamethylcyclotetrasiloxane are mixed make mixture;
B) with 3g cetyl trimethyl ammonia chloride, 1g potassium hydroxide, the 10g alkylphenol polyoxyethylene, two fat of 9g oleic acid list and 160g water drop in the there-necked flask, begin then to stir, and are warmed up to 50 ℃;
C) mixture that a) makes is added dropwise to b) system in, keep 120min, slowly be warming up to 85 ℃ then, be incubated 6 hours, be cooled to 40 ℃, neutralization is filtered, discharging, must translucent cation composite modified organic silicon microemulsion.This emulsion has fabulous softness, lax function to fabric.
Embodiment 2:
A) 0.6g coupling agent γ-An Bingjisanyiyangjiguiwan, 0.2g coupling agent N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane, 0.2g coupling agent N-cyclohexyl-γ-aminopropyl methyl dimethoxysilane and 26g octamethylcyclotetrasiloxane are mixed make mixture;
B) with 3g cetyl trimethyl ammonia chloride, 1g potassium hydroxide, 8g alkylphenol polyoxyethylene, the two fat of 5g oleic acid list and 160g water drop in the there-necked flask, begin then to stir, and are warmed up to 55 ℃;
C) mixture that a) makes is added dropwise to b) system in, keep 60min, slowly be warming up to 90 ℃ then, be incubated 5 hours, be cooled to 40 ℃, neutralization is filtered, discharging, must translucent cation composite modified organic silicon microemulsion.This emulsion is main to fabric sofetening, is with smooth, lax function.
Embodiment 3:
A) 0.3g coupling agent γ-An Bingjisanyiyangjiguiwan, 0.3g coupling agent N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane, 0.3g coupling agent N-cyclohexyl-γ-aminopropyl methyl dimethoxysilane and 26g octamethylcyclotetrasiloxane are mixed make mixture;
B) 3g cetyl trimethyl ammonia chloride, 1g potassium hydroxide, 15g alkylphenol polyoxyethylene, the two fat of 5g oleic acid list and 160g water are dropped in the there-necked flask, begin then to stir, be warmed up to 45 ℃;
C) mixture that a) makes is added dropwise to b) system in, keep 120min, slowly be warming up to 80 ℃ then, kept 6 hours, be cooled to 40 ℃, neutralization is filtered, discharging, must translucent cation composite modified organic silicon microemulsion.This emulsion has fabulous softness, smooth, lax function to fabric.
Claims (2)
1, a kind of preparation method that the cation composite modified organic silicon emulsion of softening, slipping and elastic function is arranged, it is characterized in that it is to adopt cationic emulsifier cetyl trimethyl ammonia chloride, composite with the nonionic emulsifying agent alkylphenol polyoxyethylene, potassium hydroxide is catalyzer, silane coupling agent γ-An Bingjisanyiyangjiguiwan with three kinds of different substituents, coupling agent N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane, coupling agent N-cyclohexyl-γ-aminopropyl methyl dimethoxysilane and organosilane monomer carry out the composite emulsion modification by copolymerization, made translucent modified emulsion, its preparation method comprises the steps:
A) coupling agent γ-An Bingjisanyiyangjiguiwan, coupling agent N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane, coupling agent N-cyclohexyl-γ-aminopropyl methyl dimethoxysilane and octamethylcyclotetrasiloxane are mixed by proportioning make mixture;
B) cationic emulsifier cetyl trimethyl ammonia chloride, catalyzer potassium hydroxide, nonionic emulsifying agent alkylphenol polyoxyethylene, the two fat of oleic acid list and water are dropped in the reactor by proportioning, begin then to stir, be warming up to 50 ℃ ± 5 ℃;
C) mixture that a) makes is added dropwise to b) system in, keep 60min～120min, slowly be warming up to 80 ℃～85 ℃ then, be incubated 5～6 hours, cooling, neutralization is filtered, discharging, gets translucent cation composite modified organic silicon emulsion.
2, a kind of preparation method that the cation composite modified organic silicon emulsion of softening, slipping and elastic 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-An Bingjisanyiyangjiguiwan 0.1%～0.3%, coupling agent N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane 0.10%～0.14%, coupling agent N-cyclohexyl-γ-aminopropyl methyl dimethoxysilane 0.10%～0.14%, octamethylcyclotetrasiloxane 12%～13%;
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): cetyl trimethyl ammonia chloride 1.4%～1.5%, potassium hydroxide 0.45%～0.5%, alkylphenol polyoxyethylene 3.9%～7.1%, the two fat 2.4%～4.3% of oleic acid list, water 75%～80%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100380069A CN100334133C (en) | 2005-03-07 | 2005-03-07 | Process for preparing cation composite modified organic silicon emulsion with softening, slipping and elastic function |
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| CNB2005100380069A CN100334133C (en) | 2005-03-07 | 2005-03-07 | Process for preparing cation composite modified organic silicon emulsion with softening, slipping and elastic function |
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| CN1683434A CN1683434A (en) | 2005-10-19 |
| CN100334133C true CN100334133C (en) | 2007-08-29 |
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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 CNB2005100380069A patent/CN100334133C/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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| CN1683434A (en) | 2005-10-19 |
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