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Addition-type liquid fluorosilicone rubber inhibitor and preparation method thereof

A technology of rubber inhibitor and liquid fluorosilicone, which is applied in the field of rubber materials, can solve the problems of inhibitor volatilization loss and poor compatibility of fluorosilicone rubber system, and achieve the effect of solving volatilization loss, good compatibility and remarkable effect

Active Publication Date: 2022-05-27
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

[0006] Aiming at the deficiencies in the prior art, the present invention provides an addition-type liquid fluorosilicone rubber inhibitor and its preparation method, which can effectively solve the problems of the volatilization loss of the inhibitor and poor compatibility with the fluorosilicone rubber system.

Method used

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  • Addition-type liquid fluorosilicone rubber inhibitor and preparation method thereof
  • Addition-type liquid fluorosilicone rubber inhibitor and preparation method thereof
  • Addition-type liquid fluorosilicone rubber inhibitor and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] An additively molded liquid fluorosilicone rubber inhibitor with the following structure:

[0050]

[0051] The preparation steps are as follows:

[0052] (1) Under the protection of nitrogen, to the reactor equipped with mechanical stirring, thermometer, condensing tube, drip funnel added 1340g tetramethyldisiloxane, 1500g toluene and 12.6g tri (pentafluorophenyl) borane, open the stirring and heat up to 40 °C, and then slowly add 1764g 2-methyl-3-butyne-2-ol to the kettle for dehydrogenation reaction, during the drip addition of a large amount of exothermic heat, by the drip acceleration of the kettle temperature regulation, maintain the reaction temperature of the entire drip process of 40 °C ~ 50 °C, After the drop addition, continue stirring the reaction for 1h;

[0053] (2) Reduce the reaction system to room temperature and add 76g of hydrotallite [Mg] to the kettle 6 Al 2 (OH) 16 CO 3 .4H 2 O] and 80 g of diatomaceous earth stirred to neutralize for 2 h, and then n...

Embodiment 2

[0057] An additively molded liquid fluorosilicone rubber inhibitor with the following structure:

[0058]

[0059] The preparation steps are as follows:

[0060] (1) Under the protection of nitrogen, add 1340g of tetramethyldisiloxane, 2000g of toluene and 17.5g of tris(pentafluorophenyl) borane to the reactor equipped with mechanical stirring, thermometer, condensing tube, and drip funnel, turn on stirring and heat up to 40 °C, and then slowly add 1848g of 2-methyl-3-butyne-2-ol to the kettle for dehydrogenation reaction, during the drop-addition of a large amount of exothermic heat, through the drop acceleration of the kettle temperature regulation, maintain the reaction temperature of the entire drip process of 40 °C ~ 50 °C, After the drop addition, continue stirring the reaction for 2h;

[0061] (2) Reduce the reaction system to room temperature and add 105g of hydrotallite [Mg] to the kettle 6 Al 2 (OH) 16 CO 3 .4H 2 O] and 100 g of diatomaceous earth stirred to neutralize...

Embodiment 3

[0064] An additively molded liquid fluorosilicone rubber inhibitor with the following structure:

[0065]

[0066] The preparation steps are as follows:

[0067] (1) To the reactor equipped with mechanical stirring, thermometer, condensing tube was added 468g trimethyltris(3,3,3-trifluoropropyl) cyclotrisiloxane (D 3 F) and 268g tetramethyldisiloxane, stirred evenly, using an ice water bath to reduce the kettle temperature to 10 °C ~ 15 °C Then slowly add 3.6g of trifluoromethanesulfonic acid to the kettle for cationic catalytic ring-opening polymerization reaction, reaction exothermic, cooling in an ice water bath, after the end of the punching temperature, maintain 10 °C ~ 20 °C to continue stirring the reaction for 2h; then add 3.2g of sodium bicarbonate to the kettle to mix the reaction for 3h and filter and filter, collect filtrate; at a pressure of -0.09MPa, heat up to 160 °C to remove unreacted raw materials and small molecules with low boiling point, cool down, and give ...

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Abstract

The invention discloses an addition-type liquid fluorosilicone rubber inhibitor and a preparation method thereof. The inhibitor is prepared by dehydrogenating a Lewis acid-catalyzed hydrogen-containing fluorosiloxane oligomer and methyl butynol. It is fully compatible with the fluorosilicone rubber system during use, and has the advantage of not being volatile even in a high-temperature environment, and has a good inhibitory effect, which effectively solves the problems of volatile loss of inhibitors and poor compatibility with the system , which gives the addition-type liquid fluorosilicone rubber sufficient operating time, and also improves the storage stability of the product. The fluorosilicone rubber product prepared by it has a smooth surface and excellent performance.

Description

Technical field [0001] The present invention relates to the technical field of rubber materials, specifically to an additively molded liquid fluorosilicone rubber inhibitor and a preparation method thereof. Background [0002] The compounding liquid fluorosilicone rubber is an elastomer with vinyl-containing polyfluorosilicone as the base glue, and the oligosiloxane containing silicone hydrogen as the crosslinking agent, under the action of platinum catalyst, the three-dimensional network structure is formed by the hydrogen addition reaction of silicon. In practice, reaction inhibitors are often needed to modulate the rate of vulcanization and give sufficient operability time for construction. Generally speaking, in order to meet the requirements of perfusion, calendering, coating and injection molding and other processes, the two-component compounding liquid fluorosilicone rubber needs at least four hours of operability time at room temperature after the two components are mixed...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/5419C08L83/08C08G77/04C08G77/24C07F7/18
CPCC08K5/5419C08L83/08C08G77/045C08G77/24C07F7/1804C07F7/188C08L2205/025
Inventor 于鹏飞解乐福田志钢杜辉邵军强侯志伟王华杰
Owner 新元化学(山东)股份有限公司
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