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Preparation method of fluorosilicon oil with high-efficiency defoaming performance

A fluorine-containing silicone oil, defoaming technology, applied in chemical instruments and methods, foam dispersion/prevention, dissolution, etc., can solve the problems of inapplicable oil phase system, low surface free energy, weak defoaming performance of silicone oil, etc. Good defoaming and anti-foaming effect, high surface energy effect

Active Publication Date: 2010-07-21
JIANGSU SAIOUXINYUE DEFOAMER
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Silicone oil is used as a defoamer due to its low surface free energy, but the long-term defoaming performance of silicone oil is weak when used alone, and it cannot be used in oil phase systems due to its certain solubility

Method used

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  • Preparation method of fluorosilicon oil with high-efficiency defoaming performance
  • Preparation method of fluorosilicon oil with high-efficiency defoaming performance
  • Preparation method of fluorosilicon oil with high-efficiency defoaming performance

Examples

Experimental program
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Effect test

Embodiment 1

[0023] ① In this example, acrylic acid and 1H, 1H, 2H, 2H-perfluorodecyl alcohol were used as raw materials to synthesize 1H, 1H, 2H, 2H-perfluorodecyl alcohol acrylate:

[0024] A 500ml four-necked flask is equipped with stirring, thermometer, reflux condenser and constant pressure addition funnel respectively. According to the weight ratio, add 40 parts of 1H, 1H, 2H, 2H-perfluorodecanol, 10 parts of acrylic acid and 50 parts of Solvent toluene, use 2 parts of concentrated sulfuric acid as catalyst, react at reflux temperature 90°C for 5.5h; neutralize the reaction product with sodium bicarbonate after the reaction, wash with water until neutral, then dry with anhydrous sodium sulfate, and finally depressurize Distillation to obtain 1H, 1H, 2H, 2H-perfluorodecyl alcohol acrylate; the product is a light yellow transparent liquid with a yield of 68%; product analysis results: FT-IR (KBr), v / cm -1 : 1272(v C-F ), 1638 (v C＝C ), 1728 (v C＝O ), 1189 (v C-O ), 2926 (v- CH2- )...

Embodiment 2

[0033] According to the reaction method provided in Example 1, 1H, 1H, 2H, 2H-perfluorodecylcarbonylpropyl-methyl silicone oil was synthesized; in the esterification reaction, 30 parts of 1H, 1H, 2H, 2H-perfluoro Decyl alcohol, 5 parts of acrylic acid and 55 parts of solvent benzene, with 1 part of methanesulfonic acid as a catalyst, reacted at a reflux temperature of 110°C for 5 hours, and the yield was 60%; the addition reaction was reacted at 130°C for 3 hours, and the yield was 75% %; for the cyclization reaction, 20 parts of fluorine-containing dichlorosilane and 10 parts of calcium oxide were reacted for 2 hours; for the ring-opening reaction, the reaction was carried out at 80° C. for 12 hours, and the yield was 77%.

Embodiment 3

[0035] According to the reaction method provided in Example 1, 1H, 1H, 2H, 2H-perfluorodecylcarbonylpropyl-methyl silicone oil was synthesized; in the esterification reaction, 50 parts of 1H, 1H, 2H, 2H-perfluoro Decyl alcohol, 15 parts of acrylic acid and 45 parts of solvent thionyl chloride, with 4 parts of cyclohexane as a catalyst, reacted at a reflux temperature of 70°C for 6 hours, and the yield was 62%; among them, the addition reaction was carried out at 80°C for 7 hours, The yield is 76%; among them, cyclization reaction, 26 parts of fluorine-containing dichlorosilane, and 10 parts of manganese dioxide are reacted for 3 hours; among them, the ring-opening reaction is reacted at 90° C. for 10 hours, and the yield is 80%.

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Abstract

The invention discloses fluorosilicon oil with a high-efficiency defoaming performance and a preparation method thereof. Acroleic acid and fluorine-containing fatty alcohol generate esterification reaction under the effect of a catalyst to synthesize fluorine-containing fatty alcohol acrylate; the fluorine-containing fatty alcohol acrylate and dichloromethyl silane generate silicon hydrogen addition reaction to obtain fluorine-containing dichlorosilane; the fluorine-containing dichlorosilane and dimethyl dichlorosilane generate dechlorination cyclization reaction under the effect of a metal oxide; and finally, under the effect of a blocking agent hexamethyl disiloxane, the fluorosilicon oil is obtained by ring-opening polymerization reaction. The fluorosilicon oil has low surface tension and good defoaming and foam inhibiting effects as an oil defoamer.

Description

technical field [0001] The invention relates to a preparation method of fluorine-containing silicone oil with high-efficiency defoaming performance, and belongs to the technical field of special polymer materials in chemical synthesis. Background technique [0002] Silicone oil is used as a defoamer because of its low surface free energy, but the long-term defoaming performance of silicone oil is weak when used alone, and it cannot be used in oil phase systems due to its certain solubility. Since the fluorocarbon group has lower surface free energy, such as poly(1H, 1H, 2H, 2H-heptadecafluorodecane) methylsiloxane film material, the surface energy is only 7.0mN / m, so the use of fluorocarbon The fluorine-containing silicone oil obtained by substituting part or all of the methyl group of the side chain of the silicone oil has better defoaming performance; moreover, the fluorocarbon group is insoluble in the oil phase system, so that the fluorine-containing silicone oil can be ...

Claims

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Application Information

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IPC IPC(8): B01F17/54B01D19/04C09K23/54
Inventor 杨柏忠
Owner JIANGSU SAIOUXINYUE DEFOAMER
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