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Preparation method for organosilicone acrylate

A technology of acrylate and silicone, which is applied in the field of silicone acrylate preparation, can solve the problems of product impurity, single acrylate group, difficulty in meeting the requirements of defoamer dispersibility and defoaming, etc. To achieve the effect of improving smoothness

Active Publication Date: 2014-08-27
SHANGHAI PHICHEM MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] In the above four preparation methods, CH-containing 2 =CMeCOOC 3 h 6 The silane is used as a raw material, and the silane is prone to self-polymerization or copolymerization under the conditions of addition and condensation reactions, resulting in a variety of substances, resulting in impure products, and the grafted acrylate group is single and unchanged, making it difficult to achieve defoaming agent Requirements for good dispersibility and defoaming

Method used

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  • Preparation method for organosilicone acrylate
  • Preparation method for organosilicone acrylate
  • Preparation method for organosilicone acrylate

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preparation example Construction

[0028] The embodiment of the present invention provides a method for preparing silicone acrylate, the preparation method comprising:

[0029] Step 1 Preparation of epoxy hydrocarbon-based silicone: In the presence of inert gas, catalyst, polymerization inhibitor and epoxy stabilizer, low-hydrogen silicone oil and unsaturated epoxy compound are reacted at 60-100°C for 0.5-2 hours, and then distilled to obtain Epoxy hydrocarbon-based silicone, wherein the molar ratio of the silicon-hydrogen bond of the low-hydrogen silicone oil to the carbon-carbon double bond of the unsaturated epoxy compound is 1:(1~2);

[0030] Step 2 Preparation of silicone acrylate: in the presence of air, esterification reaction catalyst, polymerization inhibitor and antioxidant, react the epoxy hydrocarbon-based silicone with unsaturated carboxylic acid at 60-100°C for 10-25 hours , to obtain silicone acrylate, wherein the molar ratio of the epoxy group of the epoxy alkyl silicone to the carboxyl group of...

Embodiment 1

[0050] The embodiment of the present invention provides a method for preparing silicone acrylate, the method comprising:

[0051] Add 12g of high hydrogen-containing silicone oil (hydrogen content 1.5%, viscosity 30cst), 2g of hexamethyldisiloxane (MM), 90g of octamethyldisiloxane (MM) into a 500ml three-necked reaction flask equipped with mechanical stirring, condenser and thermometer Tetrasiloxane (D4) and 2g concentrated sulfuric acid, control the temperature of the oil bath at 40°C, and stir for 6h. Pour the mixed solution into a separatory funnel, let it stand for half an hour, separate and remove the yellow acid solution at the bottom layer, pour the upper layer liquid into a reaction bottle, and neutralize it with 3.4 g of sodium bicarbonate powder. Distill at 110°C and 1.3kPa to remove low-boiling substances, and finally filter to obtain a colorless and transparent low-hydrogen silicone oil with a relative molecular weight of 12,000.

[0052] Weigh 55.87g of the above...

Embodiment 2

[0057] The embodiment of the present invention provides a method for preparing silicone acrylate, the method comprising:

[0058] Add 18g of high hydrogen-containing silicone oil (hydrogen content 1.0%, viscosity 50cst), 4.6gMM, 77.4gD4 and 10g of strongly acidic macroporous cationic resin to a 500ml three-necked reaction flask equipped with mechanical stirring, condenser, and thermometer, and control the oil bath The temperature was at 80°C and stirred for 8h. After filtration, take the filtrate, and distill off low boiling point substances at 110°C and 1.3kPa to obtain a colorless and transparent low-hydrogen silicone oil with a relative molecular weight of 8,000.

[0059] The preparation steps of epoxy hydrocarbon-based silicone and silicone acrylate are the same as in Example 1. The product is a brownish-yellow transparent liquid, and its infrared absorption spectrum confirms that it is silicone acrylate, and its molecular structure is as follows:

[0060]

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Abstract

The invention discloses a preparation method for organosilicone acrylate, and belongs to the preparation field of coating defoamer. The method comprises two steps of preparing an epoxy organosilicone intermediate by reacting low hydrogen-containing silicone oil and an unsaturated epoxy compound; and then preparing organosilicone acrylate by reacting the obtained epoxy organosilicone intermediate and unsaturated carboxylic acid. Compared with a conventional synthetic method for organosilicone acrylate, the method provided by the invention prevents phenomena of self-polymerization and copolymerization of bi-functional monomers, obtains a series of organosilicone acrylate containing different side chain acrylic ester groups by selecting different raw materials and reaction conditions, overcomes the disadvantage that side chain acrylic ester groups are constant, meets the requirements for good defoaming property and good levelling property of the organosilicone acrylate defoamer in an ultraviolet-curable coating system.

Description

technical field [0001] The invention relates to the field of preparation of defoamers, in particular to a preparation method of organosilicon acrylate. Background technique [0002] Due to its rapid prototyping, environmental protection and excellent performance, UV-curable coatings have achieved rapid development in recent years and have been quickly applied to various industrial fields. The main components of UV-curable coatings generally include photoinitiators, reactive diluents, oligomers and various additives such as leveling agents, dispersants, defoamers, etc., among which defoamers can play a role in defoaming and foam suppression. The addition of defoamers will directly affect the film-forming effect of UV-curable coatings during use. [0003] Silicone acrylate defoamers participate in the curing process of the coating system, which is beneficial to improve the recoatability and scratch resistance of the cured coating. Research hotspots. In the prior art, the sy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/38C08G77/12C09D11/101C09D7/12
Inventor 江彭胜曹松
Owner SHANGHAI PHICHEM MATERIAL CO LTD
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