The preparation method of silicone acrylic miniemulsion

A technology of micro-emulsion and silicon-acrylic micro-emulsion, which is applied in the field of preparation of silicon-acrylic micro-emulsion, can solve the problems of high price, limit the comprehensive performance of polyacrylate emulsion, and restrict the content of organic silicon in silicon-acrylic micro-emulsion, so as to improve the compatibility Effect

Active Publication Date: 2017-03-01
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 silicon acrylic miniemulsion needs to be improved.
[0004] In the preparation of silicone acrylic miniemulsion, commonly used organosilicon 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 acrylic microemulsion from the cost, and limits the improvement of the comprehensive performance of the polyacrylate emulsion

Method used

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  • The preparation method of silicone acrylic miniemulsion
  • The preparation method of silicone acrylic miniemulsion
  • The preparation method of silicone acrylic miniemulsion

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] (1) Methyl methacrylate (MMA), butyl acrylate (BA), methyltrimethoxysilane (MTMS) and 3-(methacryloyloxy)propyltrimethoxysilane (MEMO) according to mole Ratio 2:1:0.92:0.08 and 2wt.% (the mass fraction is based on the total mass of the monomer, the same below) hexadecane was added to a single-necked flask equipped with magnetic stirring, and stirred for more than 1 hour to completely dissolve the stabilizer , becoming an oil phase mixture;

[0045] (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;

[0046] (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 emu...

Embodiment 2

[0051] (1) Methyl methacrylate (MMA), butyl acrylate (BA), methyltrimethoxysilane (MTMS) and 3-(methacryloyloxy)propyltrimethoxysilane (MEMO) according to mole Ratio 2:1:0.92:0.08 with 1wt.% hexadecane and 1wt.% methyl methacrylate-n-butyl acrylate-siloxane random copolymer (Mn=3000g / mol, PDI=1.11, MMA: BA (mol)=2:1, 3-(methacryloyloxy)propyltrimethoxysilane content is 20mol%) were added together into a single-necked flask equipped with magnetic stirring, and stirred for more than 1 hour to make the stabilizer completely dissolve and become an oil phase mixture;

[0052] (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;

[0053] (3) The oil phase mixture is gradually added dropwise to the water phase mixture, and the hydrolysis reaction of the organic silicon a...

Embodiment 3

[0058] (1) Methyl methacrylate (MMA), butyl acrylate (BA), methyltriethoxysilane (MTES) and 3-(methacryloyloxy)propyltrimethoxysilane (MEMO) according to Molar ratio 2:1:0.71:0.08 with 1wt.% hexadecane and 1wt.% methyl methacrylate-n-butyl acrylate-siloxane random copolymer (Mn=3000g / mol, PDI=1.11, MMA : BA (mol) = 2: 1, 3-(methacryloyloxy) propyltrimethoxysilane content is 20mol%) add together in the one-necked flask equipped with magnetic stirring, stir more than 1 hour, make stabilizer Dissolve completely and become an oil phase mixture;

[0059] (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;

[0060] (3) The oil phase mixture is gradually added dropwise to the water phase mixture, and the hydrolysis reaction of the organosilicon and the emulsification pr...

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Abstract

The invention discloses a preparation method for silicone-acrylic miniemulsion. The preparation method comprises the following steps: mixing acrylate monomers, organosilicone monomers and a stabilizer, stirring until complete dissolution, and obtaining an oil-phase mixture, wherein the organosilicone monomers include non-functional organosilicone monomers and functional organosilicone monomers, and the non-functional organosilicone monomers include methyltrimeth(eth)oxysilane, propyltrimeth(eth)oxysilane or phenyltrimeth(eth)oxysilane; dissolving an emulsifier and water, and stirring uniformly to obtain a water-phase mixture; adding the oil-phase mixture into the water-phase mixture, producing a hydrolysis-emulsification reaction, performing ultrasonic miniemulsification, and producing a miniemulsion polymerization reaction of a mixed solution in an oxygen-free condition at 50-70 DEG C to obtain the silicone-acrylic emulsion. The preparation method is used for performing miniemulsion polymerization on a monomer system consisting of the non-functional organosilicone monomers, the functional organosilicone monomers and the acrylate monomers, the prepared silicone-acrylic miniemulsion is relatively high in both silicon content and solid content, and the coagulation rate can be reduced to 0%.

Description

technical field [0001] The invention relates to the technical field of emulsion preparation, in particular to a method for preparing a silicon acrylic miniemulsion. Background technique [0002] Polyacrylate emulsion has excellent anti-aging, film-forming properties, chemical resistance, transparency and mechanical properties, etc., and the raw material price is low, and the synthesis process is relatively simple, so it has been widely used in the coating industry. Especially water-based polyacrylate coatings, which use polyacrylate as the base material and water as the solvent or dispersion medium, are widely used in the construction field because of their safe use and no pollution to the environment. However, with the rapid development of the coatings industry, for practical applications, polyacrylate coatings still have some shortcomings, such as poor water resistance, friction resistance, and weather resistance, which affect the effect of decoration and protection. In o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/14C08F220/18C08F220/28C08F230/08C08F2/30
Inventor 范宏张先伟王颖欣李伯耿
Owner ZHEJIANG UNIV
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