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Fluorosilicone defoaming agent and preparation method thereof

A fluorosilicone defoamer and defoaming technology, which is applied in the direction of foam dispersion/prevention, can solve the problems that are difficult to meet the needs of industrial production, and achieve suitable for large-scale production, improve defoaming and foam suppression performance, and production operations simple effect

Active Publication Date: 2015-03-25
ZHEJIANG JUHUA HANZHENG NEW MATERIAL +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the silicone defoamer has a certain solubility in the oil phase, and it is difficult to meet the needs of some industrial production as a single silicone defoamer

Method used

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  • Fluorosilicone defoaming agent and preparation method thereof
  • Fluorosilicone defoaming agent and preparation method thereof
  • Fluorosilicone defoaming agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Take the compound of (Formula II) as 1,3,5-trimethyl-1,3,5-tri(3,3,4,4,5,5,6,6,6-nonafluorohexyl)cyclotri Siloxane, take 60g 1,3,5-trimethyl-1,3,5-tris(3,3,4,4,5,5,6,6,6-nonafluorohexyl)cyclotrisiloxane , 20g trifluoropropylmethylcyclotrisiloxane (D 3 F), 20g octamethylcyclotetrasiloxane (D) 4 ) into the 250mL there-necked flask with stirring paddle, thermometer and reflux condensing device, then add 0.8g hexamethyldisiloxane in the there-necked flask, then use the concentrated sulfuric acid (98%) as a catalyst, get 1.0g of concentrated sulfuric acid (98%) was added to the three-necked flask to form a mixed solution. After mixing uniformly, heating to 110 °C for 10 h to obtain a crude product. After the reaction, the crude product was cooled to room temperature, washed with water until neutral, and the low waste in the crude product was removed under reduced pressure to obtain 92 g of a fluorosilicone defoamer. The reaction equation is shown in formula III:

[0031...

Embodiment 2

[0036]Take the compound of (Formula II) as 1,3,5-trimethyl-1,3,5-tris(3,3,4,4,5,5,6,6,7,7,8,8, 9,9,9-tridecafluorooctyl) cyclotrisiloxane, take 60g of 1,3,5-trimethyl-1,3,5-tri(3,3,4,4,5,5,6 ,6,7,7,8,8,9,9,9-tridecafluorooctyl)cyclotrisiloxane, 20g trifluoropropylmethylcyclotrisiloxane (D 3 F), 20g octamethylcyclotetrasiloxane (D) 4 ) into the 250mL there-necked flask with stirring paddle, thermometer and reflux condensing device, then add 0.8g hexamethyldisiloxane in the there-necked flask, then use trifluorosulfonic acid as a catalyst, get 1.0g trifluorosulfonic acid added to the three-necked flask to form a mixed solution. After mixing uniformly, heating to 110 °C for 10 h to obtain a crude product. After the reaction, the crude product was cooled to room temperature, washed with water until neutral, and the low waste in the crude product was removed under reduced pressure to obtain 93 g of a fluorosilicone defoamer.

[0037] The surface tension of the fluorosilicone de...

Embodiment 3

[0041] Take the compound of (Formula II) as 1,3,5-trimethyl-1,3,5-tri(3,3,4,4,5,5,6,6,6-nonafluorohexyl)cyclotri Siloxane, take 25g of 1,3,5-trimethyl-1,3,5-tris(3,3,4,4,5,5,6,6,6-nonafluorohexyl)cyclotrisiloxane , 35g trifluoropropylmethylcyclotrisiloxane (D 3 F), 40g octamethylcyclotetrasiloxane (D) 4 ) into the 250mL there-necked flask with stirring paddle, thermometer and reflux condensing device, then add 1.5g of hexamethyldisiloxane in the there-necked flask, then use trifluorosulfonic acid as a catalyst, get 0.5g of trifluorosulfonic acid added to the three-necked flask to form a mixed solution. After mixing uniformly, heating to 110 °C for 10 h to obtain a crude product. After the reaction, the crude product was cooled to room temperature, washed with water until neutral, and the low waste in the crude product was removed under reduced pressure to obtain 95 g of a fluorosilicone defoamer.

[0042] The surface tension of the fluorosilicone defoamer was 18.9 mN / m mea...

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Abstract

The invention discloses a fluorosilicone defoaming agent, wherein the fluorosilicone defoaming agent has different chain segments of fluoroalkyl. The defoaming agent is low in surface energy, excellent in defoaming property, long in foaming inhibition time, low in addition amount, and especially suitable for defoaming in an oil-based system. The invention further provides a preparation method of the fluorosilicone defoaming agent, and the preparation method comprises the following steps: mixing a compound (shown in the formula II), trifluoropropylmethylcyclotrisiloxane (D3F) and octamethylcyclotetrasiloxane (D4), heating the mixture by taking hexamethyldisiloxane as a blocking agent and inorganic acid or organic acid as a catalyst, and reacting to obtain the fluorosilicone defoaming agent. In preparation, the proportional relation of all components can be optimized to obtain an optimal formula, and the prepared fluorosilicone defoaming agent has excellent defoaming and foaming inhibition properties. In addition, the preparation method is simple, mild in conditions, and suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the technical field of polymer materials in chemical synthesis, in particular to a fluorosilicone defoamer and a preparation method thereof. Background technique [0002] Foaming agent is recognized as the most effective foam elimination method. Compared with alcohol, ether, mineral oil and synthetic oil defoamer, silicone defoamer has low surface energy, excellent chemical stability and high and low temperature resistance. It has become a commonly used defoamer in industry. However, the silicone defoamer has a certain solubility in the oil phase, and it is difficult to meet the needs of some industrial productions by using silicone alone as a defoamer. [0003] At present, the research on organofluorine-modified silicone oil mainly focuses on the fluorine-containing side chain. Organofluorine-modified silicone oil mainly refers to polydimethylsiloxane with fluorine-containing alkyl side chains, and its unique organofluorine ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D19/04
Inventor 向德轩陈欣王树华周强
Owner ZHEJIANG JUHUA HANZHENG NEW MATERIAL
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