CN100334136C - Process for preparing anion composite modified organic silicon emulsion with softening, slipping and elastic function - Google Patents
Process for preparing anion composite modified organic silicon emulsion with softening, slipping and elastic function Download PDFInfo
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- CN100334136C CN100334136C CNB2005100380001A CN200510038000A CN100334136C CN 100334136 C CN100334136 C CN 100334136C CN B2005100380001 A CNB2005100380001 A CN B2005100380001A CN 200510038000 A CN200510038000 A CN 200510038000A CN 100334136 C CN100334136 C CN 100334136C
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- Prior art keywords
- emulsion
- coupling agent
- methyl dimethoxysilane
- softening
- organic silicon
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- 239000000839 emulsion Substances 0.000 title claims abstract description 33
- 239000002131 composite material Substances 0.000 title claims abstract description 18
- 150000001450 anions Chemical class 0.000 title claims abstract description 13
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims description 16
- 229910052710 silicon Inorganic materials 0.000 title claims description 16
- 239000010703 silicon Substances 0.000 title claims description 16
- 238000004519 manufacturing process Methods 0.000 title 1
- 239000007822 coupling agent Substances 0.000 claims abstract description 21
- -1 polyoxyethylene Polymers 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- MQWFLKHKWJMCEN-UHFFFAOYSA-N n'-[3-[dimethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical compound CO[Si](C)(OC)CCCNCCN MQWFLKHKWJMCEN-UHFFFAOYSA-N 0.000 claims abstract description 11
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims abstract description 10
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims abstract description 10
- 150000002191 fatty alcohols Chemical class 0.000 claims abstract description 8
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 7
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 5
- 239000000178 monomer Substances 0.000 claims abstract description 3
- PKTOVQRKCNPVKY-UHFFFAOYSA-N dimethoxy(methyl)silicon Chemical compound CO[Si](C)OC PKTOVQRKCNPVKY-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 8
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 7
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 7
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 7
- 239000005642 Oleic acid Substances 0.000 claims description 7
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 7
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 7
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 claims description 7
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 5
- 238000006386 neutralization reaction Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000012874 anionic emulsifier Substances 0.000 claims description 2
- 238000007334 copolymerization reaction Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 230000004048 modification Effects 0.000 claims description 2
- 238000012986 modification Methods 0.000 claims description 2
- 150000001282 organosilanes Chemical class 0.000 claims description 2
- 125000001424 substituent group Chemical group 0.000 claims description 2
- 239000004744 fabric Substances 0.000 abstract description 13
- 102000004169 proteins and genes Human genes 0.000 abstract description 5
- 108090000623 proteins and genes Proteins 0.000 abstract description 5
- 239000007787 solid Substances 0.000 abstract description 2
- IKYAJDOSWUATPI-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propane-1-thiol Chemical compound CO[Si](C)(OC)CCCS IKYAJDOSWUATPI-UHFFFAOYSA-N 0.000 abstract 1
- 125000000129 anionic group Chemical group 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 abstract 1
- 229920000191 poly(N-vinyl pyrrolidone) Polymers 0.000 abstract 1
- 230000002265 prevention Effects 0.000 abstract 1
- 241000237502 Ostreidae Species 0.000 description 4
- 235000020636 oyster Nutrition 0.000 description 4
- 239000004902 Softening Agent Substances 0.000 description 1
- 230000001588 bifunctional effect Effects 0.000 description 1
- 238000012662 bulk polymerization Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Landscapes
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Silicon Polymers (AREA)
Abstract
The present invention relates to a preparation method of an anion 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 fatty alcohol as an anionic emulsifying agent and peregal O25 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 (N-(beta-aminoethyl)-gamma-aminopropyl methyl dimethoxy silane), a coupling agent (gamma-mercaptopropyl methyl dimethoxy 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 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, 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 anion composite modified organic silicon emulsion of softness, smooth, elasticity 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, slipping and elastic 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 N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane, coupling agent γ-mercapto propyl group methyl dimethoxysilane 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 N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane, coupling agent γ-mercapto propyl group methyl dimethoxysilane 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 N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane 0.2%～0.4%, coupling agent γ-mercapto propyl group methyl dimethoxysilane 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%.
Coupling agent N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane is a kind of silane coupling agent of bifunctional diamine.It can give fabric super soft feel(ing).
Coupling agent γ-mercapto propyl group methyl dimethoxysilane is the silane coupling agent of the strong reactive behavior of a kind of containing-SH.It can give particularly woollens anti-shrinking function of fabric.
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) 0.4g coupling agent N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane, 0.2g coupling agent γ-mercapto propyl group methyl dimethoxysilane and 16.7g octamethylcyclotetrasiloxane are mixed make mixture;
B) with 78g water, 3g sulfonic acid, 0.5g alkylphenol polyoxyethylene, the two fat of 1g oleic acid list and 0.2g 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, loose bullet.
Embodiment 2:
A) 0.9g coupling agent N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane, 1.8g coupling agent γ-mercapto propyl group methyl dimethoxysilane and 66.8g octamethylcyclotetrasiloxane are mixed make mixture;
B) with 312g water, 12g sulfonic acid, 2g alkylphenol polyoxyethylene, the two fat of 4.8g 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 be warming up to 80 ℃ then, be incubated 5 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, loose bullet.
Embodiment 3:
A) 1.7g coupling agent N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane, 1.7g coupling agent γ-mercapto propyl group methyl dimethoxysilane and 83.5g octamethylcyclotetrasiloxane are mixed make mixture;
B) with 390g water, 15g sulfonic acid, 2.5g alkylphenol polyoxyethylene, the two fat of 4.5g oleic acid list and 1g 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 be warming up to 70 ℃ 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, loose bullet.
Claims (2)
1, a kind of preparation method that the anion composite modified organic silicon emulsion of softening, slipping and elastic 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 N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane, coupling agent γ-mercapto propyl group methyl dimethoxysilane 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 N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane, coupling agent γ-mercapto propyl group methyl dimethoxysilane 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, 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 N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane 0.2%～0.4%, coupling agent γ-mercapto propyl group methyl dimethoxysilane 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%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100380001A CN100334136C (en) | 2005-03-07 | 2005-03-07 | Process for preparing anion composite modified organic silicon emulsion with softening, slipping and elastic function |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100380001A CN100334136C (en) | 2005-03-07 | 2005-03-07 | Process for preparing anion composite modified organic silicon emulsion with softening, slipping and elastic function |
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| Publication Number | Publication Date |
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| CN1683437A CN1683437A (en) | 2005-10-19 |
| CN100334136C true CN100334136C (en) | 2007-08-29 |
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| CNB2005100380001A Expired - Fee Related CN100334136C (en) | 2005-03-07 | 2005-03-07 | Process for preparing anion composite modified organic silicon emulsion with softening, slipping and elastic function |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101280345B (en) * | 2008-01-22 | 2012-04-25 | 浙江传化股份有限公司 | Anionic organic silicon emulsion leather slip agent and preparation method thereof |
| 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 CNB2005100380001A patent/CN100334136C/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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