CN1297592C - Process for preparing cation composite modified organosilicon emulsion - Google Patents
Process for preparing cation composite modified organosilicon emulsion Download PDFInfo
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- CN1297592C CN1297592C CNB2005100380092A CN200510038009A CN1297592C CN 1297592 C CN1297592 C CN 1297592C CN B2005100380092 A CNB2005100380092 A CN B2005100380092A CN 200510038009 A CN200510038009 A CN 200510038009A CN 1297592 C CN1297592 C CN 1297592C
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- emulsion
- coupling agent
- aminopropyl methyl
- methyl dimethoxysilane
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Abstract
The present invention relates to a preparation method of cation composite modified organosilicon emulsion, which is mainly used for improving the functions of softness and relaxation 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 (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 and a substituting group of the coupling agent are different. The emulsion prepared by the present invention has a solid content of 20% to 22%, and the appearance is semitransparent. The prepared emulsion performs excellent functions of softening and relaxation on fabrics.
Description
Technical field:
The present invention relates to a kind of organic silicon emulsion, especially relate to a kind of cation composite modified organic silicon preparation of microemulsion method.Be mainly used in the softness that improves fabric, lax 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 emulsion of preparation is handled fabric sofetening in this way, lax 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 softness, lax function that handles is provided.
The object of the present invention is achieved like this: a kind of preparation method of cation composite modified organic silicon emulsion, 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 [N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane] with two kinds of different substituents, coupling agent [N-cyclohexyl-γ-aminopropyl methyl dimethoxysilane] carries out the composite emulsion modification by copolymerization with organosilane monomer, made translucent modified emulsion, its preparation method comprises the steps:
A) 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 emulsion raw material total amount and is in the mixed solution of step a): coupling agent [N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane] 0.14%～0.3%, coupling agent [N-cyclohexyl-γ-aminopropyl methyl dimethoxysilane] 0.14%～0.33%, octamethylcyclotetrasiloxane 12%～13%.
The consumption of each raw material of mixed system accounts for the weight percent of emulsion raw material total amount and is in the step b): cetyl trimethyl ammonia chloride 1.9%～2.0%, potassium hydroxide 0.45%～0.5%, nonionic emulsifying agent alkylphenol polyoxyethylene 4.0%～6.2%, the two fat 2.4%～2.5% of oleic acid list, water 76%～80%.
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 two kinds of different functional groups, in conjunction with the advantage of two kinds of coupling agents, the emulsion that makes has fabulous softness, lax function to fabric.
The emulsion of the present invention's preparation, its solid content is 20%～22%, outward appearance is translucent.The emulsion that makes has fabulous softness, lax function to fabric.
Embodiment:
Embodiment 1:
A) 1g coupling agent [N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane], 1g coupling agent [N-cyclohexyl-γ-aminopropyl methyl dimethoxysilane] and 52g octamethylcyclotetrasiloxane are mixed make mixture;
B) with 8g cetyl trimethyl ammonia chloride, 2g potassium hydroxide, the 17g alkylphenol polyoxyethylene, two fat of 10g oleic acid list and 320g 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) 0.3g coupling agent [N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane], 0.68g coupling agent [N-cyclohexyl-γ-aminopropyl methyl dimethoxysilane] and 26g octamethylcyclotetrasiloxane are mixed make mixture;
B) with 4g cetyl trimethyl ammonia chloride, 1g potassium hydroxide, 13g alkylphenol polyoxyethylene, the two fat of 5.2g 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 has fabulous softness, lax function to fabric.
Embodiment 3:
A) 0.60g 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) 4g cetyl trimethyl ammonia chloride, 1g potassium hydroxide, 10g 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, lax function to fabric.
Claims (2)
1, a kind of preparation method of cation composite modified organic silicon emulsion, 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 [N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane], the coupling agent [N-cyclohexyl-γ-aminopropyl methyl dimethoxysilane] of two kinds of different substituents are carried out the composite emulsion modification by copolymerization with organosilane monomer, made translucent modified emulsion, its preparation method comprises the steps:
A) 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 warmed 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, kept 5～6 hours, cooling, neutralization is filtered, discharging, gets translucent cation composite modified organic silicon emulsion.
2, the preparation method of a kind of cation composite modified organic silicon emulsion according to claim 1 is characterized in that:
The consumption of each raw material accounts for the weight percent of emulsion raw material total amount and is in the mixed solution of step a): coupling agent [N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane] 0.14%～0.3%, coupling agent [N-cyclohexyl-γ-aminopropyl methyl dimethoxysilane] 0.14%～0.33%, octamethylcyclotetrasiloxane (D
4) 12%～13%.
The consumption of each raw material of mixed system accounts for the weight percent of emulsion raw material total amount and is in the step b): cetyl trimethyl ammonia chloride 1.9%～2.0%, potassium hydroxide 0.45%～0.5%, nonionic emulsifying agent alkylphenol polyoxyethylene 4.0%～6.2%, the two fat 2.4%～2.5% of oleic acid list, water 76%～80%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100380092A CN1297592C (en) | 2005-03-07 | 2005-03-07 | Process for preparing cation composite modified organosilicon emulsion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100380092A CN1297592C (en) | 2005-03-07 | 2005-03-07 | Process for preparing cation composite modified organosilicon emulsion |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1670058A CN1670058A (en) | 2005-09-21 |
| CN1297592C true CN1297592C (en) | 2007-01-31 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB2005100380092A Expired - Fee Related CN1297592C (en) | 2005-03-07 | 2005-03-07 | Process for preparing cation composite modified organosilicon emulsion |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102002162B (en) * | 2010-08-10 | 2012-07-25 | 佛山市顺德区德美瓦克有机硅有限公司 | Cation amino silicone oil micro-emulsion and preparation method thereof |
| CN106118071A (en) * | 2016-07-11 | 2016-11-16 | 宁波富纳新材料科技有限公司 | A kind of preparation method of guanidinesalt modified amido organic silicon emulsion |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4935464A (en) * | 1987-04-30 | 1990-06-19 | Toray Silicone Company Limited | Organopolysiloxane microemulsion, process for its production and application thereof |
| CN1169489A (en) * | 1996-06-21 | 1998-01-07 | 上饶燎原精细化工实业公司 | Method for making finishing agent for multi-amino silicone high-elasticity fabric |
| JPH10147716A (en) * | 1996-10-16 | 1998-06-02 | Dow Corning Corp | Silicone emulsion |
-
2005
- 2005-03-07 CN CNB2005100380092A patent/CN1297592C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4935464A (en) * | 1987-04-30 | 1990-06-19 | Toray Silicone Company Limited | Organopolysiloxane microemulsion, process for its production and application thereof |
| CN1169489A (en) * | 1996-06-21 | 1998-01-07 | 上饶燎原精细化工实业公司 | Method for making finishing agent for multi-amino silicone high-elasticity fabric |
| JPH10147716A (en) * | 1996-10-16 | 1998-06-02 | Dow Corning Corp | Silicone emulsion |
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| CN1670058A (en) | 2005-09-21 |
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Assignee: Jiangyin Ruco Technology Co., Ltd. Assignor: Hua Mingyang Contract fulfillment period: 2009.4.10 to 2014.4.10 contract change Contract record no.: 2009320000802 Denomination of invention: Prepn process of cation compounded and modified organosilicon emulsion with relaxation shrink resisting function Granted publication date: 20070131 License type: Exclusive license Record date: 2009.5.6 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2009.4.10 TO 2014.4.10; CHANGE OF CONTRACT Name of requester: JIANGYIN CITY NUOKE SCIENCE CO., LTD. Effective date: 20090506 |
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Granted publication date: 20070131 Termination date: 20160307 |