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Preparation method of vinyl-terminated fluorosilicone oil

A technology of vinyl-terminated and fluorine-terminated silicone oil, which is applied in the field of organic silicon industry, can solve problems such as poor end-capping effect and many organic solvents, and achieve the effects of overcoming compatibility problems, fast reaction speed and high product purity

Active Publication Date: 2019-03-29
GUANGZHOU DAOLIN SYNTHETIC MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Aiming at the deficiencies in the prior art, the present invention provides a method for preparing vinyl-terminated fluorosilicone oil in order to solve the problem that the current vinyl-terminated fluorosilicone oil has poor sealing effect and needs to use more organic solvents. The method is effective for the preparation of vinyl-terminated polymethyltrifluoropropylsiloxane

Method used

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  • Preparation method of vinyl-terminated fluorosilicone oil
  • Preparation method of vinyl-terminated fluorosilicone oil
  • Preparation method of vinyl-terminated fluorosilicone oil

Examples

Experimental program
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Effect test

Embodiment 1

[0039] (1) Add 121g (1mol) Me 2 ViSiCl and 422g (0.9mol) D 3 F , and then add 4.22g of pyridine-N-oxide, stir and react at 40°C for 36h, then pass through excess dimethylamine to react for 24h at 20°C under stirring conditions, until no HCl is released, and then filter to remove the generated ammonium salt to obtain 482g of blocking agent c1.

[0040] (2) In a 1L three-necked flask equipped with a magnetic stirrer, a thermometer and a condenser tube, add 200 g (about 0.25 mol) of hydroxyl-terminated polymethyltrifluoropropylsiloxane with a viscosity of 100 mPa·s and 320 g (about 0.52 mol) The end-capping agent c1 obtained above is mixed and stirred to obtain a transparent and clear liquid, and then the upper end of the condenser tube is connected to a vacuum system, and the reaction is fully stirred at 20°C and 400mmHg pressure for 1h, 29 Si-NMR test shows that there is no Si-OH residue. The reaction system is heated up to 180°C under the pressure of 1mmHg and kept for 2h, ...

Embodiment 2

[0042] (1) Add 121g (1mol) Me 2 ViSiCl and 375g (0.8mol) D 3 F , and then add 7.5g of tri-n-butylphosphine oxide, stir and react at 90°C for 2h, then pass through excess dimethylamine to react for 18h at 70°C under stirring conditions, until no HCl is released, and then filter to remove the formed ammonium salt to obtain 426g of blocking agent c2.

[0043] (2) In a 1L three-necked flask equipped with mechanical stirring, a thermometer and a condenser tube, add 300g (about 0.083mol) of hydroxyl-terminated polymethyltrifluoropropylsiloxane with a viscosity of 600mPa·s and 142g (about 0.25mol) mol) The end-capping agent c2 obtained above is mixed and stirred to obtain a transparent and clear liquid, and then the upper end of the condenser tube is connected to a vacuum system, and the reaction is fully stirred at 60°C and 100mmHg pressure for 2h, 29 Si-NMR test shows that there is no Si-OH residue. The reaction system is heated to 180°C under the pressure of 1mmHg and kept for ...

Embodiment 3

[0045] (1) Add 121g (1mol) Me 2 ViSiCl and 399g (0.85mol) D 3 F , and then add 20g of triphenylphosphine oxide, stir and react at 70°C for 6h, then pass through excess dimethylamine to react for 4h at 100°C under stirring conditions, until no HCl is released, and then filter to remove the generated ammonium salt, That is, 435g of blocking agent c3 was obtained.

[0046] (2) In a 1L three-necked flask equipped with mechanical stirring, a thermometer and a condenser tube, add 300g (about 0.060mol) of hydroxyl-terminated polymethyltrifluoropropylsiloxane with a viscosity of 1500mPa·s and 120g (about 0.24 mol) The end-capping agent c3 obtained above is mixed and stirred to obtain a transparent and clear liquid, and then the upper end of the condenser tube is connected to a vacuum system, and the reaction is fully stirred and reacted at 80 ° C and 600 mmHg pressure for 3 hours, 29 Si-NMR test shows that there is no Si-OH residue. Finally, the reaction system is heated up to 180°...

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Abstract

The invention provides a preparation method of vinyl-terminated fluorosilicone oil, and particularly relates to a preparation method of a vinyl-terminated methyl trifluoropropyl polysiloxane. According to the invention, a vinyl silicon-nitrogen oligomer containing methyl trifluoropropyl silicon oxide chains is adopted as an end-capping reagent to react with hydroxyl-terminated fluorosilicone oil to prepare the vinyl-terminated fluorosilicone oil, so that a homogeneous reaction can be realized without using an organic solvent, and meanwhile, an appropriate vacuum degree is used for promoting escape of byproducts of ammonia gas or dimethylamine gas. The preparation method has the advantages of high reaction speed, high product purity, high yield and the like, and particularly has advantagesin preparing the vinyl-terminated fluorosilicone oil with viscosity of 1500-100000 mPa*s.

Description

technical field [0001] The invention relates to the technical field of organosilicon industry, in particular to a preparation method of vinyl-terminated polymethyltrifluoropropylsiloxane. Background technique [0002] With the rapid development of the national economy, organic fluorosilicon materials represented by fluorosilicone oil and fluorosilicone rubber have gained more and more attention because of their excellent oil resistance, solvent resistance and chemical resistance, as well as their outstanding low surface energy characteristics. It is widely used, and its preparation technology has also been more in-depth research. Vinyl-terminated fluorosilicone oil is an important class of fluorosilicone materials. In addition to the lubricating, water-repellent, oil-repellent, mold release, defoaming and anti-fouling properties of ordinary fluorosilicone oils, it is also a good choice for the preparation of addition-type liquid fluorosilicone rubber. important raw material...

Claims

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Application Information

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IPC IPC(8): C08G77/388C08G77/385
CPCC08G77/385C08G77/388
Inventor 王跃林胡应乾冯钦邦谌绍林吴利民
Owner GUANGZHOU DAOLIN SYNTHETIC MATERIALS CO LTD