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A kind of preparation method of organosilicon styrene-acrylic microemulsion

A technology for organosilicon benzene and microemulsion, which is applied in the field of preparation of organosilicon styrene acrylic miniemulsion, can solve the problems of high price, complicated process, the preparation process of organosilicon styrene acrylic miniemulsion needs to be improved, etc., and achieves an improved compatibility. Effect

Active Publication Date: 2017-12-15
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the coagulation rate of 5.5% is still relatively high in practical applications, and the preparation process of silicone styrene-acrylic microemulsion needs to be improved.
[0005] In the preparation of silicone styrene-acrylic microemulsion, commonly used silicone monomers are: (1) cyclosiloxane, such as octamethylcyclotetrasiloxane (D 4 ), vinyl cyclosiloxane (D 4vi ), which generally requires ring-opening under acid or base catalysis and then polymerized with acrylate, the process is more complicated; (2) organosiloxane monomers containing polymerization activity, such as 3-(methacryloyloxy)propyl trimethyl Oxysilane (MEMO), 3-(methacryloyloxy)propyltriethoxysilane, vinyltriisopropoxysilane, vinyltriethoxysilane, can be directly copolymerized with acrylate monomers, but The price is relatively expensive, which restricts the increase of the silicone content in the silicone styrene-acrylic microemulsion from the cost, and limits the improvement of the comprehensive performance of the silicone styrene-acrylic emulsion

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] (1) Styrene, n-butyl acrylate, methyltrimethoxysilane and 3-(methacryloyloxy)propyltrimethoxysilane are used in a molar ratio of 2:1:0.92:0.08 and 2wt.% (mass The fractions are based on the total mass of the monomers, the same below) Hexadecane is added together into a single-necked flask equipped with magnetic stirring, and stirred for more than 1 hour to completely dissolve the stabilizer and become an oil phase mixture;

[0042] (2) Add 2.1wt.% sodium dodecyl sulfate (SDS) and 1.4wt.% OP-10 together with deionized water whose mass is 1.5 times the total mass of monomers into a four-necked flask equipped with magnetic stirring , stirred for more than 1 hour to become an aqueous phase mixture;

[0043] (3) The oil phase mixture is gradually added dropwise to the water phase mixture, and the hydrolysis reaction of the organic silicon and the emulsification process of the whole mixture are carried out simultaneously at 30° C., and the hydrolysis and emulsification time i...

Embodiment 2

[0048] (1) Styrene, butyl acrylate, methyltrimethoxysilane and 3-(methacryloyloxy)propyltrimethoxysilane are mixed according to the molar ratio of 2:1:0.92:0.08 and 1wt.% hexadecane With 1wt.% methyl methacrylate-n-butyl acrylate-siloxane random copolymer (Mn=4600g / mol, PDI=1.17PS:BA(mol)=2:1,3-(methacryloyl Oxygen) propyltrimethoxysilane content is 20mol%) is added together in the one-necked flask equipped with magnetic stirring, stirs more than 1 hour, makes stabilizer dissolve completely, becomes oily phase mixture;

[0049] (2) Add 2.1wt.% sodium dodecyl sulfate (SDS) and 1.4wt.% OP-10 together with deionized water whose mass is 1.2 times the total mass of monomers into a four-necked flask equipped with magnetic stirring , stirred for more than 1 hour to become an aqueous phase mixture;

[0050] (3) The oil phase mixture is gradually added dropwise to the water phase mixture, and the hydrolysis reaction of the organic silicon and the emulsification process of the whole mi...

Embodiment 3

[0055] (1) Styrene, n-butyl acrylate, methyltriethoxysilane and 3-(methacryloyloxy)propyltrimethoxysilane are mixed according to the molar ratio of 2:1:0.71:0.08 and 1wt.% ten Hexane and 1wt.% methyl methacrylate-n-butyl acrylate-siloxane random copolymer (Mn=4600g / mol, PDI=1.17, PS:BA(mol)=2:1,3-(form Acryloyloxy) propyltrimethoxysilane content is 20mol%) together into a single-necked flask equipped with a magnetic stirrer, stirred for more than 1 hour, so that the stabilizer is completely dissolved to become an oil phase mixture;

[0056] (2) Add 2.1wt.% sodium dodecyl sulfate (SDS) and 1.4wt.% OP-10 together with deionized water whose mass is 1.2 times the total mass of monomers into a four-necked flask equipped with magnetic stirring , stirred for more than 1 hour to become an aqueous phase mixture;

[0057] (3) The oil phase mixture is gradually added dropwise to the water phase mixture, and the hydrolysis reaction of the organosilicon and the emulsification process of t...

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Abstract

The invention discloses a preparation method of a silicone styrene-acrylic microemulsion, which comprises mixing styrene, an acrylic ester monomer, a silicone monomer and a stabilizer, and stirring until completely dissolved to obtain an oil phase mixture; mixing the emulsifier Dissolved with water, stirred evenly to obtain a water phase mixture; organosilicon monomers include non-functional organosilicon monomers and functional organosilicon monomers, wherein the non-functional organosilicon monomers are methyltrimethyl(ethyl)oxy At least one of silane, propyltrimethyl(ethyl)oxysilane or phenyltrimethyl(ethyl)oxysilane; the oil phase mixture is added to the water phase mixture, and after hydrolysis-emulsification reaction, ultrafine emulsification is carried out, The mixed solution is subjected to mini-emulsion polymerization under an oxygen-free condition of 60-100°C to obtain a silicone styrene-acrylic emulsion. Both the silicon content and the solid content of the organosilicon styrene-acrylic miniemulsion prepared by the invention are relatively high, and the aggregation rate can be reduced to less than 1%.

Description

technical field [0001] The invention relates to the technical field of emulsion preparation, in particular to a method for preparing an organosilicon styrene-acrylic miniemulsion. Background technique [0002] Styrene-acrylic emulsion (styrene-acrylate emulsion) is a system that has been studied more in emulsion polymerization, and it is also one of the top ten non-crosslinked emulsions with important industrial application value in the world today. As an important intermediate chemical product, styrene-acrylic emulsion has a very wide range of uses. It is mainly used as architectural coatings, metal surface latex coatings, floor coatings, paper adhesives, adhesives, plastic processing additives, etc. Although styrene-acrylic emulsion is cheap, its weather resistance is average, and its outdoor application is still limited. [0003] Silicone-modified styrene-acrylic emulsion is referred to as silicone-styrene-acrylic emulsion. Silicone has excellent properties such as anti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F212/08C08F220/18C08F230/08C08F220/28C08F2/26C08F2/30
Inventor 范宏张先伟王颖欣李伯耿
Owner ZHEJIANG UNIV
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