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Novel fluorinated silicone rubber additive as well as preparation method and application thereof

A technology of fluorosilicone rubber and additives, applied in chemical instruments and methods, silicone organic compounds, organic chemistry, etc., can solve the problems of increasing dosage, resilience, small compression set, and rubber becoming brittle, etc. The effect of cross-linking reaction, improving reaction probability, and increasing vulcanization activity

Active Publication Date: 2020-09-01
新元化学(山东)股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the addition amount of the above-mentioned additives is 5-10% of the fluorosilicone raw rubber, not only the amount is large, but also its function in the formula is only to promote the crosslinking of the raw rubber, and it cannot establish the chemical relationship between white carbon black and raw rubber. Connection, which has little effect on improving performance such as resilience and compression set
[0005] Most of the currently used vinyl additives are adsorbed or reacted to silica. Vinyl siloxane on silica has poor compatibility with fluorosilicone raw rubber, and the reaction is difficult, so it is necessary to increase the dosage. , but too much vinyl will easily cause unnecessary crosslinking and make the rubber brittle. The existing methods and additives cannot solve this problem well.

Method used

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  • Novel fluorinated silicone rubber additive as well as preparation method and application thereof
  • Novel fluorinated silicone rubber additive as well as preparation method and application thereof
  • Novel fluorinated silicone rubber additive as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] A preparation method of a novel fluorosilicone rubber additive, comprising the steps of:

[0050] (1) Preparation of Trifluoropropyl Allyl Methyl Chlorosilane

[0051] Add dried THF1000g, trifluoropropylmethyldichlorosilane 1265g, 80g Mg scraps and 0.5g iodine to remove the oxide layer in the reactor with mechanical stirring, constant pressure dropping funnel, thermometer and spherical condenser, Stir and mix evenly; take 790g of dry THF and 228g of allyl chloride and mix them evenly and add them to the constant pressure dropping funnel. 30~40℃, the dropping time is 3h, after the dropping is completed, react at 30~40℃ for 1h; After filtration, the filtrate was rectified and purified with a reflux ratio of 7:1, and the fraction at 63-65°C / 10.1kPa was cut off to obtain trifluoropropylallylmethylchlorosilane with a purity of 99.0% and a yield of 84%.

[0052] (2) Preparation of bis(trifluoropropyl)bis(allyl)dimethyldisilazane

[0053] Add 400g of n-hexane and 200g of tr...

Embodiment 2

[0058] A preparation method of a novel fluorosilicone rubber additive, comprising the steps of:

[0059] (1) Preparation of Trifluoropropyl Allyl Methyl Chlorosilane

[0060] Add dried THF1000g, trifluoropropylmethyldichlorosilane 1265g, 80g Mg scraps and 0.5g iodine to remove the oxide layer in the reactor with mechanical stirring, constant pressure dropping funnel, thermometer and spherical condenser, Stir and mix evenly; take 790g of dry THF and 363g of propylene bromide and mix them evenly and add them to the constant pressure dropping funnel. At 30-40°C, the dropping time is 3h. After the dropwise addition, react at 30-40°C for 1h; After filtration, the filtrate was rectified and purified with a reflux ratio of 7:1, and the fraction at 63-65°C / 10.1kPa was cut off to obtain trifluoropropylallylmethylchlorosilane with a purity of 98.7% and a yield of 81%.

[0061] (2) Preparation of bis(trifluoropropyl)bis(allyl)dimethyldisilazane

[0062] Add 500g of cyclohexane and 200...

Embodiment 3

[0064] A preparation method of a novel fluorosilicone rubber additive, comprising the steps of:

[0065] (1) Preparation of Trifluoropropyl Allyl Methyl Chlorosilane

[0066] Add dried THF1000g, trifluoropropylmethyldichlorosilane 1265g, 54g Mg chips and 0.5g iodine to remove the oxide layer in the reactor with mechanical stirring, constant pressure dropping funnel, thermometer, and spherical condenser, Stir and mix evenly; take 500g of dry THF and 153g of allyl chloride and mix them evenly, and then add them to the constant pressure dropping funnel. At 30-40°C, the dropping time is 3h. After the dropping is completed, react at 30-40°C for 1h; After filtration, the filtrate was purified by rectification at a reflux ratio of 7:1, and the fraction at 63-65°C / 10.1kPa was cut off to obtain trifluoropropylallylmethylchlorosilane with a purity of 99.4% and a yield of 89%.

[0067] (2) Preparation of bis(trifluoropropyl)bis(allyl)dimethyldisilazane

[0068] Add 600g of toluene and...

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Abstract

The invention provides a novel fluorinated silicone rubber additive as well as a preparation method and application thereof, and the preparation method comprises the following steps: in the presence of a solvent, reacting trifluoropropyl methyl dichlorosilane, magnesium chips and halopropene, adding a complex breaker after the reaction is finished, filtering, and rectifying to obtain trifluoropropyl allyl methyl chlorosilane; mixing trifluoropropyl allyl methyl chlorosilane with a non-polar solvent, introducing ammonia gas to react, and finally filtering and carrying out reduced pressure distillation to obtain di (trifluoropropyl) di (allyl) dimethyl disilazane. The novel fluorinated silicone rubber additive disclosed by the invention has the advantages that the effect of a structured control agent can be achieved; meanwhile, the compatibility of the white carbon black and the fluorosilicone raw rubber can be improved, a cross-linking reaction with a cross-linking point on the fluorosilicone raw rubber is easier to occur, chemical bond connection is formed between the white carbon black and the fluorosilicone raw rubber, and the elasticity and oil resistance of the fluorosilicone rubber are improved under the condition that the use amount is very small.

Description

technical field [0001] The invention relates to a novel fluorosilicone rubber additive and its preparation method and application, in particular to a preparation method of bis(trifluoropropyl)bis(allyl)dimethyldisilazane, which belongs to organosilicon technology field. Background technique [0002] Fluorosilicone rubber is a vinyl silicone rubber containing trifluoropropyl group in the side chain. It has excellent high and low temperature resistance, weather resistance, oil resistance and solvent resistance. It is widely used in gaskets, aerospace, automotive, machinery, chemical and other fields. Rubber products such as sealing rings, hoses, etc. [0003] The formula of fluorosilicone rubber mainly includes fluorosilicone raw rubber, fillers, additives and other materials, among which fluorosilicone rubber additives include structural control agents and functional additives, etc., and structural control agents include hydroxyfluorosilicone oil, silazane, di Phenylsilaned...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/10C07F7/20C08L83/08C08L83/04C08K13/02C08K3/36C08K5/5445
CPCC07F7/10C07F7/20C08L83/08C08L2205/025C08L2205/03C08L83/04C08K13/02C08K3/36C08K5/544
Inventor 田志钢杜辉解乐福刘晓敏林峰张威邵军强
Owner 新元化学(山东)股份有限公司
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