Production process of high viscosity phenylmethylvinyl silicone rubber

A technology of phenylmethyl ethylene and production process, applied in the field of preparation technology of polymer compounds, can solve problems such as narrowing the molecular weight distribution of products, and achieve the effects of small radial temperature difference, improved product quality, and uniform molecular weight distribution

Active Publication Date: 2010-12-22
SHANGHAI RESIN FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The invention uses a high-power high-shear vacuum stirring device to manufacture high-viscosity phenylmethyl vinyl silicone rubber, which can not only polymerize under stirring and shearing, but also solve the problem of heat and mass transfer in the reaction process, so that the molecular weight distribution of the product Narrowing, and high-power stirring can generate strong shear to high-viscosity silicone rubber to deactivate the catalyst and remove low boiling. Completed in the same device, forming a one-step process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Put phenylmethylcyclosiloxane, methylcyclosiloxane, vinylcyclosiloxane, and catalyst tetramethylammonium hydroxide silicon alkoxide into a high-load vacuum mixer, start stirring, and control the stirring speed at 20 rev / min, heat up to 60°C, and dehydrate for 1 hour under a vacuum of -0.095Pa. At a stirring speed of 20 rpm, a temperature of 98°C, and a vacuum of -0.09Pa, polymerize for 2.5 hours, then control the stirring rate to 6 rpm, raise the temperature to 150°C to deactivate the catalyst for 30 minutes, and then raise the temperature to Keep the above stirring rate at 180°C, remove the low boiling for 4 hours under the vacuum degree of -0.1Pa, and finally press the product out of the equipment.

[0011] The product prepared in Example 1 was tested according to the HG / T3313-2000 standard, and its volatile content was 2.56%, and its molar mass was 750,000. The polydispersity index is 2.7 and the refractive index is 1.4609.

Embodiment 2

[0013] Put phenylmethylcyclosiloxane, methylcyclosiloxane, vinylcyclosiloxane, and catalyst tetramethylammonium hydroxide silicon alkoxide into the planetary strong mixer, start stirring, and control the stirring speed at 30 rpm / min, heat up to 50°C, dehydrate for 1.5 hours under -0.09Pa vacuum degree, polymerize for 2 hours at a stirring speed of 24 rpm, 100°C, -0.085Pa vacuum degree, and then control the stirring rate to 8 RPM, raise the temperature to 150°C to deactivate the catalyst for 40 minutes, then raise the temperature to 180°C to maintain the above stirring rate, remove the low boiling for 5 hours under a vacuum of -0.097Pa, and finally press the product out of the equipment.

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PUM

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Abstract

The invention discloses a manufacturing process for preparing a high-viscosity phenyl methyl vinyl silicone rubber. The manufacturing technique comprises three steps: polymerization, catalyst deactivation and low boiling, and all the steps are finished in a high-power high shear vacuum stirring device. Compared with the prior art, the process has the advantages of remarkably improved heat transfer effect, small reaction kettle radial temperature difference, and greatly improved product quality, and can be used for large-scale production. For the high-viscosity phenyl methyl vinyl silicone rubber prepared by the process, the volatile compositions are less than 3 percent, the molar mass is larger than 700,000, the polydispersity index representing the molecular weight distribution is less than 3, and the production capacity of a single set of equipment is large. The indexes are better than that of the similar products manufactured by a static method on the market.

Description

[technical field] [0001] The invention belongs to the field of preparation technology of polymer compounds, in particular to a production technology of high-viscosity phenylmethyl vinyl silicone rubber. [Background technique] [0002] Due to the presence of phenyl groups in high-viscosity phenylmethyl vinyl silicone rubber, the viscosity of silicone rubber is significantly greater than that of methyl silicone rubber with the same molar mass. So far, high-viscosity phenylmethyl vinyl silicone rubber is manufactured by the traditional static bubbling method, that is, the silicone is polymerized in the reactor first, and then the polymer is taken out to deactivate the catalyst in a vacuum device. And the batch operation of removing low volatile matter, the whole process is carried out step by step. This production process has the following disadvantages: ①Static polymerization leads to poor heat transfer effect, large temperature difference in the radial direction of the react...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/20C08G77/06
Inventor 陈少彪吴蓁王立伟陈友张涛孙揭阳朱爱琴宋琼
Owner SHANGHAI RESIN FACTORY
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