Method for preparing vinyl-functionalized white carbon black for reinforcing methyl vinyl silicone rubber

A technology of methyl vinyl silicon and vinyl functions, which is applied in the field of preparation of vinyl functionalized silica for reinforcement of methyl vinyl silicone rubber, which can solve the problem of poor stability of the adsorption transition layer, affecting product performance, and stress relaxation To improve the reinforcement effect, reduce the number of hydroxyl groups, and improve the hydrophobicity

Active Publication Date: 2013-08-14
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when the white carbon black provided by the prior art is used in silicone rubber, the intermolecular interaction between white carbon black and silicone rubber is generally only physical adsorption, resulting in poor stability of the adsorption transition layer. The molecular chain of silicone rubber will slip, and the macroscopic performance will be stress relaxation, which will affect the performance of the product.

Method used

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  • Method for preparing vinyl-functionalized white carbon black for reinforcing methyl vinyl silicone rubber
  • Method for preparing vinyl-functionalized white carbon black for reinforcing methyl vinyl silicone rubber
  • Method for preparing vinyl-functionalized white carbon black for reinforcing methyl vinyl silicone rubber

Examples

Experimental program
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Effect test

Embodiment 1

[0019] A preparation method of vinyl functionalized white carbon black for methyl vinyl silicone rubber reinforcement, the preparation steps are: tetraethyl orthosilicate: catalyst ammonia water: solvent absolute ethanol: modifier undecenyl alcohol is 6 : The volume ratio of 3:1:1, mixed ethyl orthosilicate, catalyst ammonia water (0.75mol / L), solvent absolute ethanol and modifier undecenyl alcohol, reacted at 65°C for 1.5h, and then Filtration, the solid obtained after filtration is washed with absolute ethanol as a solvent for 3 times, and then dried to obtain a vinyl functionalized white carbon black product.

[0020] attached figure 1 It is the infrared spectrogram of the vinyl-functionalized silica prepared in this example; in the figure, -CH2 and -CH2 and - The characteristic peak of CH3, the characteristic peak of ethylene end group = CH2 appeared at the wave number of 1410cm-1; the infrared results confirmed that the vinyl group of undecylenol was successfully grafted...

Embodiment 2

[0022] Adopt torque rheometer to prepare mixed rubber, the preparation process is as follows: add methyl vinyl silicone rubber, the vinyl functionalized white carbon black that embodiment 1 makes and hydroxyl silicone oil and mix by the mass ratio of 100:40:8 Mixed uniformly in a container to prepare the mixed rubber I, the mixing temperature was 105°C, the rotational speed was 90 r / min, and the time was 30 min; Mix uniformly in the mill to prepare mixed rubber II, and test the vulcanized storage modulus; use a flat vulcanizer to prepare vulcanized rubber. The preparation process is as follows: the mixed rubber II is vulcanized on a plate at 120°C to obtain a vulcanized rubber sheet, which is then cut. sample test.

[0023] attached figure 2 It is the vulcanization temperature scanning storage modulus test chart of the mixed rubber II of Example 2; in the figure, compared with the unmodified silica and the undecyl alcohol modified silica, the vinyl functionalized silica It ...

Embodiment 3

[0028] A preparation method of vinyl functionalized white carbon black for methyl vinyl silicone rubber reinforcement, the preparation steps are: tetraethyl orthosilicate: catalyst ammonia water: solvent absolute ethanol: modifier undecenyl alcohol is 6 : 3:1:1 volume ratio, mix ethyl orthosilicate, catalyst ammonia water, solvent absolute ethanol and modifier undecylenol evenly, react at 50°C for 2h, and then filter, the solid obtained after filtration The product was washed twice with absolute ethanol as a solvent, and then dried to obtain a vinyl-functionalized white carbon black product.

[0029] Others are the same as embodiment 1 and embodiment 2, omitted.

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Abstract

The invention discloses a method for preparing vinyl-functionalized white carbon black for reinforcing methyl vinyl silicone rubber. The method is characterized by comprising the steps of: uniformly mixing tetraethoxysilane, ammonia water as a catalyst, absolute ethyl alcohol as a solvent and undecylenyl alcohol as a modifier according to the volume ratio of 6:3:1:1, reacting for 1-2 hours at 50-80 DEG C, then filtering to obtain solid matters, washing the solid matters for two to five times with the absolute ethyl alcohol as the solvent, and drying to obtain the vinyl-functionalized white carbon black. The vinyl-functionalized white carbon black prepared by using the method has a CH2=CH-functional group participating in a crosslinking reaction with methyl vinyl silicone rubber, and is added in the methyl vinyl silicone rubber as stuffing; vinyl on the surface of the white carbon black has a chemical bonding reaction with a molecule chain of the silicone rubber, so that a reinforcement effect of the white carbon black on the silicone rubber can be improved; and the method is applicable to the silicone rubber reinforcement industry.

Description

technical field [0001] The invention belongs to the preparation of silicon compounds with carbon-carbon unsaturated bonds, and relates to a preparation method of vinyl functionalized white carbon black for methyl vinyl silicone rubber reinforcement. The vinyl-functionalized white carbon black prepared by the present invention can participate in the cross-linking reaction of methyl vinyl silicone rubber, and can be used for the reinforcement of silicone rubber, and is especially suitable for the high-strength and low-relaxation of silicone rubber materials under ultra-high pressure conditions. Special needs. Background technique [0002] Silica has small particle size, high specific surface area, and low density. It is widely used in the rubber industry. It is an excellent rubber reinforcing agent that can improve the tensile strength, tear strength and wear resistance of rubber. For example, applying silica to tires can reduce fuel consumption and increase its service life;...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09C1/28C09C3/08C08L83/07C08K9/04C08K3/36
Inventor 宋丽贤卢忠远宋英泽芦艾康明宋开平丁涌
Owner SOUTHWEAT UNIV OF SCI & TECH
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