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A kind of long-chain alkylphenyl fluorosilicone oil and its preparation method

A technology of long-chain alkylbenzene and fluorosilicone oil, which is applied in the field of synthesis of long-chain alkylphenyl fluorosilicone oil, and can solve the problem of poor compatibility between fluorosilicone lubricating oil and synthetic oil or mineral oil, and thermal performance that cannot meet the scope of use. , Difficult to compound and use, etc., to achieve the effect of low cost, easy control, and low viscosity

Active Publication Date: 2019-01-29
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The purpose of this patent is to synthesize a high-performance fluorosilicone lubricating oil, but in the process of using it as a lubricating oil, it is necessary for the silicone oil to have good heat resistance. The thermal stability of the silicone oil synthesized by this method is better than that of ordinary dimethyl Silicone oil, but the thermal performance still cannot meet the use range of higher temperature, and its thermal stability still needs to be further improved
When compounded with other synthetic oils or mineral oils, the fluorosilicone lubricating oil synthesized by this method has poor compatibility with synthetic oils or mineral oils, and it is easy to separate and difficult to compound.

Method used

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  • A kind of long-chain alkylphenyl fluorosilicone oil and its preparation method
  • A kind of long-chain alkylphenyl fluorosilicone oil and its preparation method
  • A kind of long-chain alkylphenyl fluorosilicone oil and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] in N 2 Under protection, in a 100ml dry three-necked flask equipped with a reflux condensing device, a thermometer, and a magnetic stirrer, add dodecylphenyltrifluoropropyl co-modified siloxane mixed rings (self-made, the quality of fluorine Fraction is 20%, phenyl mass fraction is 8%, dodecyl mass fraction is 5%) 40g, octamethylcyclotetrasiloxane 20g, hexamethyldisiloxane 1.93g, 98% concentrated sulfuric acid 2.4 g, react at 25°C for 24 hours, after the reaction, add 4.15g of sodium bicarbonate to fully stir and neutralize, remove the solid salt in it by high-speed centrifugation, and remove it by distillation at a vacuum degree of -0.096Mpa and a system temperature of 200°C for 2 hours Among them, unreacted raw materials and low boilers can be used to obtain dodecylphenyl fluorosilicone oil.

[0037] The dodecylphenyl fluorosilicone oil prepared in this implementation is a clear and transparent liquid with a molecular weight of 5300g / mol, wherein the fluorine content...

Embodiment 2

[0040] in N 2 Under protection, in a 100ml dry three-necked flask equipped with a reflux condensing device, a thermometer, and a magnetic stirrer, add dodecylphenyltrifluoropropyl co-modified siloxane mixed rings (self-made, the quality of fluorine Fraction is 10%, phenyl mass fraction is 15%, dodecyl mass fraction is 5%) 40g, octamethylcyclotetrasiloxane 20g, hexamethyldisiloxane 0.32g, tetramethylhydroxide Ammonium 0.012g, react at 70°C for 12 hours, heat up to 170°C for 30 minutes after the reaction, decompose tetramethylammonium hydroxide, and remove it by distillation at a vacuum degree of -0.096Mpa and a system temperature of 200°C for 2 hours Dodecylphenyl fluorosilicone oil can be obtained from unreacted raw materials and low boilers.

[0041] The dodecylphenyl fluorosilicone oil prepared in this implementation is a clear and transparent liquid with a molecular weight of 35000g / mol, wherein the fluorine content is 5.86%, the phenyl content is 9.68%, and the dodecyl co...

Embodiment 3

[0044] in N 2 Under protection, in a 100ml dry three-necked flask equipped with a reflux condensing device, a thermometer, and a magnetic stirrer, add dodecylphenyltrifluoropropyl co-modified siloxane mixed rings (self-made, the quality of fluorine Fraction is 20%, phenyl mass fraction is 8%, dodecyl mass fraction is 5%) 40g, octamethylcyclotetrasiloxane 20g, tetramethyldiethylsiloxane 0.14g, tetramethyl Ammonium hydroxide 0.006g, react at 70°C for 12 hours, heat up to 170°C for 30 minutes after the reaction, decompose tetramethylammonium hydroxide, and distill for 2 hours at a vacuum degree of -0.096Mpa and a system temperature of 200°C Dodecylphenyl fluorosilicone oil can be obtained by removing unreacted raw materials and low boilers.

[0045] The dodecylphenyl fluorosilicone oil prepared in this implementation is a clear and transparent liquid with a molecular weight of 83000g / mol, wherein the fluorine content is 13.12%, the phenyl content is 4.87%, and the dodecyl conten...

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Abstract

The invention discloses long-chain alkyl phenyl fluorosilicone oil and a preparation method thereof. The preparation method comprises the following steps: under the protection of inert gas, a self-made polyfunctional group substituted hybrid siloxane ring body is used as a reaction raw material, a corresponding end-capping reagent is added, and a strong acid or strong base ring-opening reaction is carried out to prepare high-molecular-weight long-chain alkyl phenyl fluorosilicone oil. The preparation method is low in cost and mild in reaction condition, the molecular structure and organic group content of the product are easy to control, the organic group in the synthesized product is more uniform in distribution, the synthesized product is low in viscosity and good in heat resistance, and the lubricating property requirements within a wide temperature range are met; at the same time, the long-chain alkyl phenyl fluorosilicone oil can be used as an additive and used in a compounding manner with the synthetic oil or mineral oil, so that the lubricating properties of the synthetic oil or mineral oil are improved.

Description

technical field [0001] The invention relates to a method for synthesizing long-chain alkylphenyl fluorosilicone oil. The ring-opening polymerization of siloxane mixed rings containing long-chain alkyl, phenyl, and fluoroalkyl is catalyzed by strong acid or strong base to control the molecular weight and Molecular weight distribution obtained long-chain alkylphenyl fluorosilicone oil with excellent comprehensive properties. Background technique [0002] Among synthetic lubricating oils, methyl silicone oil has excellent high and low temperature performance, but its poor lubricity affects its application. As we all know, fluorine has the strongest electronegativity among all elements, and it tends to bond strongly with other atoms and attract the bonded electrons, especially the fluorine atom in C-F, as a substituent, shows a strong absorption electronic. If some methyl groups are replaced by fluorine-containing alkyl groups, fluorosilicone lubricating oils for high, low tem...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/24C08G77/06C08G77/08
Inventor 范宏张德琪
Owner ZHEJIANG UNIV
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