CN101280345B - Anion organosilicon emulsion smoothing agent for leather and preparation thereof - Google Patents
Anion organosilicon emulsion smoothing agent for leather and preparation thereof Download PDFInfo
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- CN101280345B CN101280345B CN2008100594485A CN200810059448A CN101280345B CN 101280345 B CN101280345 B CN 101280345B CN 2008100594485 A CN2008100594485 A CN 2008100594485A CN 200810059448 A CN200810059448 A CN 200810059448A CN 101280345 B CN101280345 B CN 101280345B
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Abstract
The invention discloses anion organ silicone mulsion leather slip agent and a preparation method thereof. Most of the prior organ silicon leather slip agent is only provided with amino group and difficult plays the function of durability. The invention adopts anion emulsifier sodium dodecyl benzene sulfonate and nonionic emulsifier fatty alcohol polyoxyethylene ether and takes benzene sulfonic acid as catalyst; the emulsion copolymerization is performed to the coupling agent containing crosslinking functional group, the coupling agent containing amino-hydrocarbon and the organ silicon monomer to prepare anion organ silicon emulsion. The organ silicon emulsion contains sulfhydryl or epoxy group crosslinking functional group and simultaneously contains the amino-hydrocarbon functional group, the slip agent is ensured to have durability by the crosslinking functional group and is ensured to meet the requirements of slipperiness, lubrication and waterproof by the amino-hydrocarbon.
Description
Technical field
The present invention relates to the leather chemical industry field, specifically a kind of anion organosilicon emulsion smoothing agent for leather and preparation method thereof.
Background technology
Organosilicon emulsion smoothing agent for leather is an important industrial chemicals in the process hides process, and it can significantly improve the feel of leather, makes that leather is smooth, glossy, waterproof etc.The performance quality of organosilicon emulsion smoothing agent for leather is mainly reflected in smooth property, weather resistance, water-repellancy, and the leather hand feeling aspect after covering with paint, lacquer, colour wash, etc.At present; Anion organosilicon emulsion as smoothing agent for leather; Because the ionic of its ionic and most leather chemical industry raw material such as finish, pigment paste is identical; So their consistency is better, in use the floating oil phenomenon can not occur, and the shelf stability of anionic organic silicon emulsion is also better.Publication number is that the one Chinese patent application of CN1670223A discloses a kind of waterborne organic silicon smoothing agent for leather and preparation method thereof, and the surface slip agent for preparing through this method only contains amino, is difficult to play the effect of weather resistance.
Summary of the invention
Technical problem to be solved by this invention is to overcome the defective that above-mentioned prior art exists, and provides a kind of and not only has weather resistance but also can satisfy anion organosilicon smoothing agent for leather smooth, glossy, waterproof requirement.
For this reason; The present invention adopts following technical scheme: a kind of anion organosilicon emulsion smoothing agent for leather; It is characterized in that its employing anionic emulsifier X 2073 and nonionic emulsifying agent AEO; With the Phenylsulfonic acid is catalyzer, and the coupling agent that will contain bridging property functional group carries out emulsion copolymerization with the coupling agent and an organosilane monomer that contain the ammonia alkyl, is prepared into anion organosilicon emulsion.Contain sulfydryl or epoxy group(ing) bridging property functional group and ammonia hydrocarbyl functional group in the organic silicon emulsion of the present invention simultaneously, bridging property functional group since it can with amino on the leather fiber take place crosslinked, thereby make this surface slip agent have weather resistance; The ammonia alkyl makes it can satisfy smooth, glossy and waterproof requirement again.
Above-mentioned anion organosilicon emulsion smoothing agent for leather; Raw material and quality percentage composition thereof used during letex polymerization are: an organosilane monomer 15%～17%, contain the coupling agent 0.1%～0.3% of bridging property functional group, and contain the coupling agent 0.2%～0.5% of ammonia alkyl; Phenylsulfonic acid 4.0%～9.0%; X 2073 0.5%～1.0%, AEO 2.0%～3.5%, all the other are deionized water.
Above-mentioned anion organosilicon emulsion smoothing agent for leather, an organosilane monomer are octamethylcyclotetrasiloxane or dimethyl siloxane mixed methylcyclosiloxane; The described coupling agent that contains bridging property functional group is γ-mercapto propyl group methyl dimethoxysilane, γ (2; 3 epoxies)-and propyl trimethoxy silicane or both mixtures, the coupling agent that contains the ammonia alkyl is γ-An Bingjisanyiyangjiguiwan, N-β (aminoethyl)-γ-aminopropyl methyl dimethoxy oxygen alkane silane or both mixtures; EO value (ethylene oxide value) contained in the molecular chain of AEO is 3～25.
The outward appearance of organic silicon emulsion of the present invention is translucent for the band blue light, and solid content is 22～24%, and the pH value is 6.5～7.0.
Another object of the present invention is to provide the preparation method of above-mentioned organosilicon emulsion smoothing agent for leather, and its concrete steps are following:
A) will contain the mixed mixture that gets of the coupling agent of bridging property functional group, the coupling agent that contains the ammonia alkyl and an organosilane monomer;
B) deionized water, X 2073, Phenylsulfonic acid, AEO are dropped in the reaction kettle, start and stir, be warming up to 50 ℃ ± 5 ℃, insulation 1h ± 0.5h;
C) mixture that a) makes is dropped to b) system in, the dropping time is 60min～120min, slowly is warming up to 70～85 ℃ then, insulation 4～6h, cooling, neutralization is filtered, discharging, anion organosilicon emulsion.
The present invention has following beneficial effect: the smoothing agent for leather that makes contains sulfydryl or epoxy group(ing) bridging property functional group and ammonia hydrocarbyl functional group simultaneously, makes this surface slip agent both have weather resistance, can satisfy smooth, glossy and waterproof requirement again; The nonionic emulsifying agent AEO that is adopted does not contain the material (APEOs) of any TX10 class, and is easy to biological degradation, compliance with environmental protection requirements.
Below in conjunction with embodiment the present invention is further described.
Embodiment
Embodiment 1
Preparing method of the present invention is following:
A) with 1.0 kilograms of γ-mercapto propyl group methyl dimethoxysilane, 5.0 kilograms of γ-An Bingjisanyiyangjiguiwans and 170.0 kilograms of octamethylcyclotetrasiloxanes mix processes mixture;
B) with 780.0 kilograms of deionized waters, 5.0 kilograms of X 2073es, 90.0 kilograms of Phenylsulfonic acids, 20 kilograms of AEOs (AEO-3), 15.0 kilograms of paregal Os are fed in the reaction kettle, open then and stir, and are warming up to 50 ℃;
C) mixture that a) makes is dropped to b) system in, the dropping time is 120min, slowly is warming up to 85 ℃ then, insulation 4h is cooled to 50 ℃, neutralization is filtered, discharging, anion organosilicon emulsion smoothing agent for leather.
Embodiment 2
Preparing method of the present invention is following:
A) with 1.0 kilograms of γ (2,3 epoxy)-propyl trimethoxy silicane, 4.0 kilograms of γ-An Bingjisanyiyangjiguiwans and 170.0 kilograms of octamethylcyclotetrasiloxanes mix processes mixture;
B) with 760.0 kilograms of deionized waters, 7.5 kilograms of X 2073es, 80.0 kilograms of Phenylsulfonic acids, 15.0 kilograms of AEOs (AEO-7), 10.0 kilograms of paregal Os are fed in the reaction kettle, open then and stir, and are warming up to 50 ℃;
C) mixture that a) makes is dropped to b) system in, the dropping time is 120min, slowly is warming up to 80 ℃ then, insulation 5h is cooled to 50 ℃, neutralization is filtered, discharging, anion organosilicon emulsion smoothing agent for leather.
Embodiment 3
Preparing method of the present invention is following:
A) with 3.0 kilograms of γ (2,3 epoxy)-propyl trimethoxy silicane, 2.0 kilograms of N-β (aminoethyl)-γ-aminopropyl methyl dimethoxy oxygen alkane silane and 150.0 kilograms of dimethyl siloxane mixed methylcyclosiloxanes mix processes mixture;
B) with 730.0 kilograms of deionized waters, 10.0 kilograms of X 2073es, 40.0 kilograms of Phenylsulfonic acids, 10.0 kilograms of AEOs (AEO-9), 15.0 kilograms of paregal Os are fed in the reaction kettle, open then and stir, and are warming up to 50 ℃;
C) mixture that a) makes is dropped to b) system in, the dropping time is 60min, slowly is warming up to 75 ℃ then, insulation 6h is cooled to 50 ℃, neutralization is filtered, discharging, anion organosilicon emulsion smoothing agent for leather.
Embodiment 4
Preparing method of the present invention is following:
A) with 3.0 kilograms of γ-mercapto propyl group methyl dimethoxysilane, 5.0 kilograms of N-β (aminoethyl)-γ-aminopropyl methyl dimethoxy oxygen alkane silane and 160.0 kilograms of dimethyl siloxane mixed methylcyclosiloxanes mix processes mixture;
B) with 750.0 kilograms of deionized waters, 5.0 kilograms of X 2073es, 70.0 kilograms of Phenylsulfonic acids, 15 kilograms of AEOs (AEO-9), 12.5 kilograms of paregal Os are fed in the reaction kettle, open then and stir, and are warming up to 50 ℃;
C) mixture that a) makes is dropped to b) system in, the dropping time is 90min, slowly is warming up to 80 ℃ then, insulation 5h is cooled to 50 ℃, neutralization is filtered, discharging, anion organosilicon emulsion smoothing agent for leather.
The above only is preferred embodiment of the present invention.Every foundation technical spirit of the present invention all falls in protection scope of the present invention any simple modification, equivalent variations and modification that above embodiment did.
Claims (7)
1. anion organosilicon emulsion smoothing agent for leather; It is characterized in that its employing anionic emulsifier X 2073 and nonionic emulsifying agent AEO; With the Phenylsulfonic acid is catalyzer; The coupling agent that will contain bridging property functional group carries out emulsion copolymerization with the coupling agent and an organosilane monomer that contain the ammonia alkyl, makes anion organosilicon emulsion; The described coupling agent that contains the ammonia alkyl is a γ-An Bingjisanyiyangjiguiwan.
2. anion organosilicon emulsion smoothing agent for leather according to claim 1; Raw material and quality percentage composition thereof used when it is characterized in that letex polymerization are: an organosilane monomer 15%～17%, contain the coupling agent 0.1%～0.3% of bridging property functional group, and contain the coupling agent 0.2%～0.5% of ammonia alkyl; Phenylsulfonic acid 4.0%～9.0%; X 2073 0.5%～1.0%, AEO 2.0%～3.5%, all the other are deionized water.
3. anion organosilicon emulsion smoothing agent for leather according to claim 1 is characterized in that an organosilane monomer is octamethylcyclotetrasiloxane or dimethyl siloxane mixed methylcyclosiloxane.
4. anion organosilicon emulsion smoothing agent for leather according to claim 1 is characterized in that the said coupling agent that contains bridging property functional group is γ-mercapto propyl group methyl dimethoxysilane, γ (2,3 epoxy)-propyl trimethoxy silicane or both mixtures.
5. anion organosilicon emulsion smoothing agent for leather according to claim 1 is characterized in that EO value contained in the molecular chain of AEO is 3～25.
6. anion organosilicon emulsion smoothing agent for leather according to claim 1 is characterized in that the outward appearance of emulsion is translucent for the band blue light, and solid content is 22～24%, and the pH value is 6.5～7.0.
7. according to the preparation method of each described smoothing agent for leather of claim 1-6, its step is following:
A) will contain the mixed mixture that gets of the coupling agent of bridging property functional group, the coupling agent that contains the ammonia alkyl and an organosilane monomer;
B) deionized water, X 2073, Phenylsulfonic acid, AEO are dropped in the reaction kettle, start and stir, be warming up to 50 ℃ ± 5 ℃, insulation 1h ± 0.5h;
C) mixture that a) makes is dropped to b) system in, the dropping time is 60min～120min, slowly is warming up to 70～85 ℃ then, insulation 4～6h, cooling, neutralization is filtered, discharging, anion organosilicon emulsion.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008100594485A CN101280345B (en) | 2008-01-22 | 2008-01-22 | Anion organosilicon emulsion smoothing agent for leather and preparation thereof |
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| CN2008100594485A CN101280345B (en) | 2008-01-22 | 2008-01-22 | Anion organosilicon emulsion smoothing agent for leather and preparation thereof |
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| CN101280345B true CN101280345B (en) | 2012-04-25 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102190964B (en) * | 2011-03-02 | 2013-06-26 | 江苏雪豹日化有限公司 | Leather long-acting brightening agent and processing method thereof |
| CN104004204B (en) * | 2014-05-12 | 2016-06-22 | 华南理工大学 | A kind of sulfonate type dianion emulsifying agent containing epoxide group and preparation method thereof |
| CN105111932B (en) * | 2015-08-26 | 2018-06-05 | 日照东润有机硅股份有限公司 | A kind of production method of response type waterproofing agent of organosilicon |
| 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 |
| CN113072705B (en) * | 2021-03-19 | 2022-06-24 | 常州市嘉诺有机硅有限公司 | Epoxy silane modified organic silicon emulsion and synthetic method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1683437A (en) * | 2005-03-07 | 2005-10-19 | 华明扬 | Process for preparing anion composite modified organic silicon emulsion with softening, slipping and elastic function |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1683437A (en) * | 2005-03-07 | 2005-10-19 | 华明扬 | Process for preparing anion composite modified organic silicon emulsion with softening, slipping and elastic function |
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Address after: 311215 Xiaoshan economic and Technological Development Zone, Hangzhou, Zhejiang Patentee after: The mass of Limited by Share Ltd Address before: 311215 Xiaoshan economic and Technological Development Zone, Hangzhou, Zhejiang Patentee before: Chuanhua Co., Ltd., Zhejiang |
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Effective date of registration: 20170428 Address after: 311215 Xiaoshan economic and Technological Development Zone, Xiaoshan District, Zhejiang, Hangzhou Co-patentee after: Hangzhou Transfer Fine Chemical Co., Ltd. Patentee after: The mass of Limited by Share Ltd Address before: 311215 Xiaoshan economic and Technological Development Zone, Hangzhou, Zhejiang Patentee before: The mass of Limited by Share Ltd |