Inorganic nano SiO2 hybrid organic silicon fluoride-free waterproof agent and preparation method thereof

A fluorine-free water repellent and inorganic nano technology, which is applied in the field of textile dyeing auxiliaries, can solve the problems of limited use of fluorine-containing water repellants, poor fabric feel, complicated preparation methods, etc., and achieves obvious waterproof effect, improved washing resistance, Guaranteed long-lasting results

Active Publication Date: 2020-11-10
科凯精细化工(上海)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The waterproof effect of fluorine-containing finishing agents is the most obvious, but perfluorooctane sulfonyl compounds (PFOS) and perfluorooctanoic acid compounds (PFOA) are the most indispensable sources of raw materials for fluorine-containing waterproofing agents. Due to the international ban on PFOS and PFOA , many fluorocarbon waterproof finishing agents on the market are gradually being eliminated, and the use of fluorine-containing waterproofing agents is bound to be limited. Therefore, finding waterproof finishing additives that can replace organic fluorine has become an urgent problem to be solved in the industry
[0004] For fluorine-free waterproof finishing agents, people have made various attempts and explorations, but some fluorine-free waterproof finishing agents and their preparation methods all have some places that need to be improved, especially after the waterproof finishing of textiles, the fabric's feel becomes worse, Washing resistance needs to be improved. In addition, the preparation method is relatively complicated, and the process route needs to be simplified.

Method used

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  • Inorganic nano SiO2 hybrid organic silicon fluoride-free waterproof agent and preparation method thereof
  • Inorganic nano SiO2 hybrid organic silicon fluoride-free waterproof agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Add 81.4g octamethylcyclotetrasiloxane linear body, 0.12g tetramethylammonium hydroxide and 8.36g distilled water into the reaction vessel, stir, heat up to 85°C for 2 hours, cool down to 60°C, add 1.5gN-β- (Aminoethyl)-γ-aminopropylmethyldimethoxysilane, 8.4g hexadecyltrimethoxysilane and 0.22g tetramethylammonium hydroxide, heat up to 120°C, react for 2h, cool down and reduce pressure Low boilers are removed by distillation to obtain cross-linked long-chain alkyl / amino co-modified silicone;

[0038] In another reaction vessel, add 2.53g nanometer SiO in 27.60g toluene simultaneously 2 (average particle size is 80nm), ultrasonically disperse at room temperature for 30min to obtain a uniform suspension, then add 1.93g of coupling agent γ-(2,3-glycidyloxy)propyltrimethoxysilane, ultrasonically Disperse for 5 minutes, then magnetically stir and reflux for 6 hours under the reaction condition of 90°C, centrifuge at high speed, wash several times and then dry to obtain epo...

Embodiment 2

[0041] Add 85.4g octamethylcyclotetrasiloxane linear body, 0.12g tetramethylammonium hydroxide and 3.56g distilled water into the reaction vessel, stir, heat up to 90°C for 2.5h, cool down to 60°C, add 1.4gN-β -(Aminoethyl)-γ-aminopropylmethyldimethoxysilane, 9.3g hexadecyltrimethoxysilane and 0.22g tetramethylammonium hydroxide, heated up to 130°C, reacted for 1h, cooled down Pressure distillation to remove low boilers to obtain cross-linked long-chain alkyl / amino co-modified organosilicon;

[0042] In another reaction vessel, add 2.18g nanometer SiO in 28.4g toluene simultaneously 2 (average particle size is 80nm), ultrasonically disperse at room temperature for 30min to obtain a uniform suspension, then add 1.91g coupling agent γ-(2,3-glycidyloxy)propyltrimethoxysilane to it, ultrasonically Disperse for 5 minutes, then magnetically stir and reflux for 6 hours under the reaction condition of 90°C, centrifuge at high speed, wash several times and then dry to obtain epoxy-mod...

Embodiment 3

[0046] Add 86.2g octamethylcyclotetrasiloxane linear body, 0.12g tetramethylammonium hydroxide and 3.26g distilled water into the reaction vessel, stir, raise the temperature to 95°C for 2 hours, cool down to 60°C, add 0.8g N-β- (Aminoethyl)-γ-aminopropylmethyldimethoxysilane, 9.4g hexadecyltrimethoxysilane and 0.22g tetramethylammonium hydroxide, heat up to 120°C, react for 2h, cool down and reduce pressure Low boilers are removed by distillation to obtain cross-linked long-chain alkyl / amino co-modified silicone;

[0047] In another reaction vessel, add 2.42g nanometer SiO in 28.4g toluene simultaneously 2 (average particle size is 80nm), ultrasonically disperse at room temperature for 30min to obtain a uniform suspension, then add 1.32g coupling agent γ-(2,3-glycidyloxy)propyltrimethoxysilane to it, ultrasonically Disperse for 5 minutes, then magnetically stir and reflux for 6 hours under the reaction condition of 90°C, centrifuge at high speed, wash several times and then ...

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Abstract

The invention discloses an inorganic nano SiO2 hybrid organic silicon fluoride-free waterproof agent and a preparation method thereof. The preparation method comprises the following steps of introducing a long carbon chain group and a reactive amino group into an organic silicon side chain by adopting an alkaline equilibrium reaction to prepare cross-linked long-chain alkyl/amino co-modified organic silicon; putting nano SiO2 into methylbenzene for ultrasonic treatment, and performing modifying by using a silane coupling agent to prepare epoxy modified nano SiO2; enabling the prepared cross-linked long-chain alkyl/amino co-modified organic silicon and epoxy modified nano SiO2 to react in solvent isopropanol, so as to obtain inorganic nano SiO2 hybrid long-chain alkyl organic silicon; and emulsifying the inorganic nano SiO2 hybrid long-chain alkyl organic silicon with water to obtain the inorganic nano SiO2 hybrid organic silicon fluoride-free waterproof agent. The preparation method provided by the invention is clear in route and simple, can be used for preparation without special and complex equipment, is used for waterproof finishing of cotton fabrics, enables the fabrics to be soft in hand feeling, can enable the fabrics to have an excellent waterproof effect, and has relatively good durability.

Description

technical field [0001] The invention belongs to the technical field of textile dyeing auxiliaries, in particular to an inorganic nano-SiO 2 Hybrid organosilicon fluorine-free waterproofing agent and its preparation method. Background technique [0002] With the continuous improvement of the quality of life and the rapid development of the textile industry, people have higher and higher requirements for the variety and performance of fabrics. Traditional textiles can no longer meet people's growing needs. People's requirements for the performance of fabrics are also constantly improving. They are no longer limited to basic functions such as warmth and comfort as in the past, but also require clothing to have other additional functions, including moisture permeability, perspiration, anti-wrinkle, easy decontamination, UV protection, Antibacterial, antistatic and other functionalized textiles. Therefore, domestic and foreign textile industry workers are committed to developin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D06M15/643D06M11/79C08G77/26D06M101/06
CPCD06M15/6436D06M11/79C08G77/26D06M2200/12D06M2200/50D06M2101/06
Inventor 张达王慧荣张萍苏梦婷
Owner 科凯精细化工(上海)有限公司
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