CN102093562B - Preparation method of low-yellowing negative ion-modified organic silicon emulsion - Google Patents
Preparation method of low-yellowing negative ion-modified organic silicon emulsion Download PDFInfo
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- CN102093562B CN102093562B CN200910231660XA CN200910231660A CN102093562B CN 102093562 B CN102093562 B CN 102093562B CN 200910231660X A CN200910231660X A CN 200910231660XA CN 200910231660 A CN200910231660 A CN 200910231660A CN 102093562 B CN102093562 B CN 102093562B
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Abstract
The invention relates to a preparation method of a low-yellowing negative ion-modified organic silicon emulsion. The emulsion is mainly used for enhancing the flexibility and the wearability of a light color fabric and almost has no influence on the chromatic light of the fabric simultaneously. The method comprises the following steps of: compounding a negative ion emulsifier, polyethylene glycol PEG400 and nonionic emulsifier fatty alcohol polyoxyethylene ether; and performing emulsion polymerization on N,N-dimethyl aminopropyl aminopropyl methyl dimethoxy silane, gamma-aminopropyl triethoxy silane and an organic silicon monomer by taking sulfoacid as a catalyst to obtain a modified emulsion. The modified emulsion prepared by the invention has the solid content between 21 percent and 25 percent, and is a blue-light semitransparent emulsion. The emulsion has excellent flexibility and wearability on a light-colored fabric and almost has no influence on the chromatic light of the fabric simultaneously.
Description
Technical field
The present invention relates to a kind of organic silicon emulsion, especially relate to the preparation method of the anion-modified organosilicon emulsion of a kind of low-yellowing.This emulsion has fabulous softness, wear behavior to light fabric, and the coloured light to fabric does not almost have influence simultaneously.
Background technology
Organic silicon emulsion plays an important role to feel, the shrinkproof performance of improving fabric 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 through mass polymerization earlier, carry out microemulsified with suitable emulsifying agent again.After the emulsion of preparation was handled fabric in this way, feel existed not enough, in use made light fabric the appearance of many-sided unstable situation such as xanthochromia, floating oil occur easily simultaneously.
Summary of the invention
Technical problem to be solved by this invention is: provide a kind of processing fabric to have softness, wear behavior, simultaneously the coloured light of fabric is not almost had the preparation method of the anion-modified organosilicon emulsion of low-yellowing of influence.
For solving the problems of the technologies described above; The technical scheme that the present invention adopted is: the preparation method of the anion-modified organosilicon emulsion of low-yellowing, this method adopt anionic emulsifier, polyoxyethylene glycol PEG400 and nonionic emulsifying agent AEO composite, and sulfonic acid is catalyzer; N; N-dimethyl aminopropyl aminopropyl methyl dimethoxysilane, γ-An Bingjisanyiyangjiguiwan and an organosilane monomer carry out emulsion copolymerization, have made hydrophilically modified emulsion, its preparation method following steps:
1) with N, N-dimethyl aminopropyl aminopropyl methyl dimethoxysilane, γ-An Bingjisanyiyangjiguiwan and an organosilane monomer octamethylcyclotetrasiloxane mix by proportioning, process mixture;
2) with deionized water, sulfonic acid, polyoxyethylene glycol PEG400, AEO drops in the reaction kettle by proportioning, stirs, and is warming up to 60 ℃ ± 5 ℃, is incubated 1.5 hours;
3) mixture that step 1) is made is added dropwise to step 2) system in, be controlled in 90min~120min and dropwise, slowly be warming up to 78 ℃~82 ℃ then; Be incubated 5~6 hours; Cooling, neutralization is filtered, discharging, obtains the anion-modified organic silicon emulsion of low-yellowing.
The consumption of each raw material accounts for the weight percent of emulsion total amount and is in the mixed solution of step 1): N, N-dimethyl aminopropyl aminopropyl methyl dimethoxysilane 0.3%, γ-An Bingjisanyiyangjiguiwan 0.1%%, octamethylcyclotetrasiloxane 17%;
Step 2) consumption of each raw material accounts for the weight percent of emulsion total amount and is in the mixed system: deionized water 78%, and sulfonic acid 3.6%, AEO 0.5%, polyoxyethylene glycol PEG400 are 0.5%.
The invention has the beneficial effects as follows: the organic silicon emulsion that makes through preparation method of the present invention; Its solid content is 21~25%; Outward appearance is the translucent emulsion of band blue light, and this emulsion has fabulous softness, wear behavior to light fabric, and the coloured light to fabric does not almost have influence simultaneously.
Embodiment
Through specific embodiment the present invention is further described below, but the present invention is not limited to following embodiment.
Embodiment one:
1) with 1.5g N, N-dimethyl aminopropyl aminopropyl methyl dimethoxysilane, 0.6g γ-An Bingjisanyiyangjiguiwan and 108g octamethylcyclotetrasiloxane mix by proportioning and process mixture;
2) with the 456g deionized water, 21g sulfonic acid, 2.1g polyoxyethylene glycol PEG400, the 4.8g AEO drops in the reaction kettle by proportioning, stirs, and is warming up to 64 ℃, is incubated 1.5 hours;
3) will be added dropwise to step 2 by the mixture that step 1) makes) system in, be controlled in the 120min and dropwise, slowly be warming up to 82 ℃ then, be incubated 5.3 hours; Cooling then, neutralization is filtered, discharging, obtains the anion-modified organic silicon emulsion of low-yellowing.
Embodiment two:
1) with 1.8g N, N-dimethyl aminopropyl aminopropyl methyl dimethoxysilane, the 0.6g γ-An Bingjisanyiyangjiguiwan mixes by proportioning with the 102g octamethylcyclotetrasiloxane and to process mixture;
2) with the 468g deionized water, 21.6g sulfonic acid, 3g polyoxyethylene glycol PEG400, the 3g AEO drops in the reaction kettle by proportioning, stirs, and is warming up to 64 ℃, is incubated 1.5 hours;
3) will be added dropwise to step 2 by the mixture that step 1) makes) system in, be controlled in the 120min and dropwise, slowly be warming up to 80 ℃ then, be incubated 5.9 hours; Cooling then, neutralization is filtered, discharging, obtains the anion-modified organic silicon emulsion of low-yellowing.
Claims (2)
1. the preparation method of the anion-modified organic silicon emulsion of low-yellowing; This method adopts anionic emulsifier, polyoxyethylene glycol PEG400 and nonionic emulsifying agent AEO composite; Sulfonic acid is catalyzer, and with N, N-dimethyl aminopropyl aminopropyl methyl dimethoxysilane, γ-An Bingjisanyiyangjiguiwan and an organosilane monomer carry out emulsion copolymerization; Made modified emulsion, its preparation method comprises the steps:
1) with N, N-dimethyl aminopropyl aminopropyl methyl dimethoxysilane, γ-An Bingjisanyiyangjiguiwan and an organosilane monomer octamethylcyclotetrasiloxane mix by proportioning processes mixture;
2) with deionized water, sulfonic acid, polyoxyethylene glycol PEG400, AEO drops in the reaction kettle by proportioning, stirs, and is warming up to 60 ℃ ± 5 ℃, is incubated 1.5 hours;
3) mixture that step 1) is made is added dropwise to step 2) system in, be controlled in 90min ~ 120min and dropwise, slowly be warming up to 78 ℃ ~ 82 ℃ then; Be incubated 5 ~ 6 hours; Cooling, neutralization is filtered, discharging, obtains the anion-modified organic silicon emulsion of low-yellowing.
2. the preparation method of the anion-modified organic silicon emulsion of low-yellowing according to claim 1 is characterized in that:
The consumption of each raw material accounts for the weight percent of emulsion total amount and is in the mixed solution of step 1): N, N-dimethyl aminopropyl aminopropyl methyl dimethoxysilane 0.3%, γ-An Bingjisanyiyangjiguiwan 0.1%, octamethylcyclotetrasiloxane 17%;
Step 2) consumption of each raw material accounts for the weight percent of emulsion total amount and is in the mixed system: deionized water 78%, and sulfonic acid 3.6%, AEO 0.5%, polyoxyethylene glycol PEG400 are 0.5%.
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Families Citing this family (4)
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CN103194892B (en) * | 2013-04-24 | 2015-05-13 | 广州市番禺区协运来化工用品有限公司 | Anti-yellowing agent |
CN105037730A (en) * | 2015-08-26 | 2015-11-11 | 武汉知睿达新材料有限公司 | Production method of reactive organosilicon softening and smoothing agent for textiles |
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 |
CN111286029A (en) * | 2020-03-15 | 2020-06-16 | 华中师范大学 | High-stability organic silicon emulsion and preparation method and application thereof |
Citations (3)
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DE102004012877A1 (en) * | 2003-12-23 | 2005-07-21 | Ge Bayer Silicones Gmbh & Co. Kg | Formulations containing amino- and/or ammonium-polysiloxane with a low content of hydroxy and alkoxy groups attached to silicon, used in detergent formulations and cosmetics or as textile softeners |
CN1670056A (en) * | 2005-03-07 | 2005-09-21 | 华明扬 | Process for preparing anion composite modified organosilicon emulsion |
CN101550237A (en) * | 2009-05-18 | 2009-10-07 | 安徽德佳有机硅有限公司 | High springback silicone stiffening agent and preparation method thereof |
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Patent Citations (3)
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DE102004012877A1 (en) * | 2003-12-23 | 2005-07-21 | Ge Bayer Silicones Gmbh & Co. Kg | Formulations containing amino- and/or ammonium-polysiloxane with a low content of hydroxy and alkoxy groups attached to silicon, used in detergent formulations and cosmetics or as textile softeners |
CN1670056A (en) * | 2005-03-07 | 2005-09-21 | 华明扬 | Process for preparing anion composite modified organosilicon emulsion |
CN101550237A (en) * | 2009-05-18 | 2009-10-07 | 安徽德佳有机硅有限公司 | High springback silicone stiffening agent and preparation method thereof |
Non-Patent Citations (2)
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有机硅交联剂改性阴离子型氨基硅微乳液的合成与应用;苏华 等;《印染助剂》;20050131;第22卷(第1期);说明书全文 * |
苏华 等.有机硅交联剂改性阴离子型氨基硅微乳液的合成与应用.《印染助剂》.2005,第22卷(第1期),第39-41页. |
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