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Heat curing silicone rubber crosslinked with polyamine compound and preparation method thereof

A heat-vulcanized silicone rubber and polyamine compound technology, applied in the field of heat-vulcanized silicone rubber and its preparation, new vulcanization reaction system to prepare high-strength heat-vulcanized silicone rubber, can solve the problem of damage to the vulcanized rubber cross-linking system, loss of catalytic activity, catalyst "Poisoning and other problems, to achieve excellent mechanical properties, improve tear strength, improve the effect of comprehensive performance

Active Publication Date: 2010-07-14
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The hydrosilylation crosslinking system has become another commonly used vulcanization system in the industrial production of thermally vulcanized silicone rubber. However, the addition and crosslinking process requires the use of precious metals as addition catalysts, which cannot be recovered after the reaction and remain in the vulcanizate. Under certain conditions The cross-linking system of vulcanized rubber will be damaged; the trace amount of platinum catalyst used for cross-linking is very sensitive to impurities, such as sulfur, phosphorus, nitrogen and other compounds that can form ligands with platinum, which can easily "poison" the catalyst and lose Catalytic activity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 70ml of toluene, 36ml of distilled water and 34ml of concentrated hydrochloric acid into a 250ml four-neck flask equipped with a stirrer, dropping funnel, reflux condenser and thermometer, and then slowly add 10.6g of γ-chloropropyl in an ice-water bath with stirring. For the mixture of methyldiethoxysilane and 22.2g dimethyldiethoxysilane, keep the temperature of the reaction system below 20°C. After the dropwise addition, continue stirring at this temperature for 1.5 hours, then heat and reflux for 3 hours. The acid layer was removed from the product, washed with water until neutral, CaCl 2 After drying overnight, a colorless and transparent solution was obtained. After evaporating toluene, distill under reduced pressure at 2.66KPa, collect fractions at 110°C-140°C to obtain chloropropylheptamethylcyclotetrasiloxane (D 3 D. C3H6Cl ).

Embodiment 2

[0026] with N 2 Add 241.20g octamethylcyclotetrasiloxane (D 4 ), 2g chloropropylheptamethylcyclotetrasiloxane (D 3 D. C3H6Cl ) and appropriate amount of alkali gel (tetramethylammonium hydroxide silicon alkoxide), pass N 2 Bubbling, heating slowly, after the alkali glue is completely dissolved, raise the temperature to 70°C, keep it for 0.5 hours, continue to raise the temperature, and balance at 90°C-110°C for 6-7 hours. After the reaction was completed, the temperature was raised to about 150° C. and maintained for 0.5 hours. Finally, the temperature is raised to about 180° C. under vacuum conditions, and low boilers are removed to obtain chloropropylpolysiloxane (chloropropyl content: 0.17% mol).

Embodiment 3

[0028] with N 2 Add 206.00g of D 4 , 0.5g D 3 D. C3H6Cl And appropriate amount of alkali gum (tetramethylammonium hydroxide silicon alkoxide), pass N 2 Bubbling, heating slowly, after the alkali glue is completely dissolved, raise the temperature to 70°C, keep it for 0.5 hours, continue to raise the temperature, and balance at 90°C-110°C for 6-7 hours. After the reaction was completed, the temperature was raised to about 150° C. and maintained for 0.5 hours. Finally, the temperature is raised to about 180° C. under vacuum conditions, and low boilers are removed to obtain chloropropyl polysiloxane (chloropropyl content: 0.05% mol).

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PUM

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Abstract

The invention discloses heat curing silicone rubber crosslinked with a polyamine compound and a preparation method thereof. The preparation method comprises the following steps of: cohydrolyzing dimethyldiethoxysilane and chloropropyl-methyl-2-silane to obtain chloropropyl-7-central-4-methyl siloxane; cohydrolyzing the chloropropyl-7-central-4-methyl siloxane and 8-central-4-methyl siloxane to obtain chloropropyl methyl polysiloxane; using the chloropropyl methyl polysiloxane as a based adhesive, polyamines as a coupler, a gas-phase-method white carbon black as a reinforcing material and zinc oxide as an acid absorbent; and preparing by heat curing. The heat curing silicone rubber of the invention not only has excellent mechanical properties, but also overcomes some defects of a traditional curing system and has favorable economic benefits and popularization application values.

Description

technical field [0001] The present invention relates to a kind of thermally vulcanized silicone rubber and its preparation method, especially to the synthesis of chloropropylmethyl polysiloxane and the preparation of thermally vulcanized silicone rubber cross-linked with polyamine compounds, especially to the use of new vulcanized The invention relates to preparing high-strength thermally vulcanized silicone rubber through a reaction system, which belongs to the technical field of rubber production. Background technique [0002] Silicone polymer is the first elemental polymer to be applied in industry, it has good dielectric and high temperature resistance, surface activity, biocompatibility, high gas permeability and hydrophobicity. It has received widespread attention since its commercialization in the 1940s. [0003] Silicone rubber is one of the most important silicone products. It is made of polysiloxane with Si-O-Si as the main chain and side groups such as methyl, vi...

Claims

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Application Information

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IPC IPC(8): C08L83/08C08K3/36C08K5/17C08K3/22C08G77/24C08J3/24
Inventor 冯圣玉刁屾卢海峰张长桥
Owner SHANDONG UNIV
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