Addition type liquid silicone rubber with high transparency and resistance to thermo-oxidative aging, and preparation method thereof

A liquid silicone rubber, addition-type technology, applied in the field of heat-resistant oxygen aging modification of silicone polymer materials, can solve the problem of deterioration of silicone rubber transparency, processing performance and mechanical properties, and poor compatibility between metal oxides and polymer matrix and other problems, to achieve excellent thermal stability, improve thermal stability and thermal oxygen aging resistance, and high heat resistance efficiency

Active Publication Date: 2018-04-20
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In summary, due to the poor compatibility between metal oxides and polymer matrix, the transparency, processing performance and mechanical properties of silicone rubber will be deteriorated, which greatly limits the use of silicone rubber in thermal insulation coatings, aerospace glass potting materials, etc. Applications in fields with high requirements for transparency and mechanical properties

Method used

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  • Addition type liquid silicone rubber with high transparency and resistance to thermo-oxidative aging, and preparation method thereof
  • Addition type liquid silicone rubber with high transparency and resistance to thermo-oxidative aging, and preparation method thereof
  • Addition type liquid silicone rubber with high transparency and resistance to thermo-oxidative aging, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 11.54g octaphenylbicyclooctasiloxane tetrasilanol sodium salt (Na 4 o 14 Si 8 (C 6 h 5 ) 8 ) was dispersed in 200g of methanol, and then 2.56g of zirconium tetrachloride (ZrCl 4 ), stirred at 60°C for 12h, filtered with suction, washed 3 times with 100mL of methanol, and dried in vacuum at 50°C for 24h to obtain zirconium metal hybrid cage silsesquioxane (Zr-POSS), whose structural formula is as follows:

[0038]

[0039] The Zr-POSS that embodiment 1 obtains is carried out infrared spectrum and nuclear magnetic resonance silicon spectrum analysis, and result is as follows figure 1 and 2 shown. It can be seen from the infrared spectrum that Zr-POSS mainly has the following characteristic peaks: 3073 and 3051cm -1 (υ Ar-H ), 1594cm -1 (υ C＝C ), 1200~1000cm -1 (υ Si-O-Si ) and 954cm -1 (υ Si-O-Zr ). Such as figure 2 Shown, in the nuclear magnetic resonance silicon spectrum of Zr-POSS: (1) δ=-68.86ppm belongs to Si atom on Si-O-Zr; (2) δ=-78.84ppm belo...

Embodiment 2

[0046] 11.54g octaphenylbicyclooctasiloxane tetrasilanol sodium salt (Na 4 o 14 Si 8 (C 6 h 5 ) 8 ) was dispersed in 200g of ethanol, and then 1.90g of titanium tetrachloride (TiCl 4 ), stirred at 60°C for 12h, filtered with suction, washed 3 times with 100mL of methanol, and dried in vacuum at 50°C for 24h to obtain the titanium metal hybrid cage silsesquioxane (Ti-POSS). IR and NMR results indicated that Ti-POSS was successfully synthesized.

[0047]

[0048] In terms of parts by mass, 98 parts of vinyl-terminated polydimethylsiloxane (viscosity at 25°C is 24200mPa·s, vinyl content is 0.25mol%), 2 parts of vinyl-terminated polymethylvinyl Siloxane (viscosity at 25°C is 2095mPa·s, vinyl content is 8.7mol%), 40 parts fumed silica (specific surface area 200m 3 / g, particle size 50nm) and 6 parts of hexamethyldisilazane were added to a vacuum kneader, mixed at room temperature for 3 hours, heated to a material temperature of 160°C for 2 hours, vacuumed and mixed for 1 ...

Embodiment 3

[0052] 11.54g octaphenylbicyclooctasiloxane tetrasilanol sodium salt (Na 4 o 14 Si 8 (C 6 h 5 ) 8 ) was dispersed in 200g of ethanol, and then 2.47g of cerium trichloride (CeCl 3 ), stirred at 60°C for 12h, filtered with suction, washed 3 times with 100mL of methanol, and dried in vacuum at 50°C for 24h to obtain the cerium metal hybrid cage silsesquioxane (Ce-POSS). IR and NMR results showed that Ce-POSS was successfully synthesized.

[0053]

[0054] In terms of parts by mass, 98 parts of vinyl-terminated polydimethylsiloxane (viscosity at 25°C is 24200mPa·s, vinyl content is 0.25mol%), 2 parts of vinyl-terminated polymethylvinyl Siloxane (viscosity at 25°C is 2095mPa·s, vinyl content is 8.7mol%), 40 parts fumed silica (specific surface area 200m 3 / g, particle size 50nm) and 6 parts of hexamethyldisilazane were added to a vacuum kneader, mixed at room temperature for 3 hours, heated to a material temperature of 160°C for 2 hours, vacuumed and mixed for 1 hour, and...

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Abstract

The invention discloses an addition type liquid silicone rubber with high transparency and resistance to thermo-oxidative aging, and a preparation method thereof. The addition type liquid silicone rubber comprises the following raw materials by mass: 100 parts of vinyl silicone oil, 30 to 50 parts of white carbon black, 5 to 7 parts of hexamethyldisilazane, 1 to 5 parts of hydrogen-containing silicone oil, 1 to 5 parts of metal hybrid cage silsesquioxane, 5 to 20 ppm of a platinum catalyst and 0.03 to 0.07 part of 1-ethynyl-1-cyclohexanol. The preparation method comprises the following steps:subjecting vinyl silicone oil, white carbon black and hexamethyldisilazane to high-temperature mixing with a vacuum kneader, and then carrying out cooling and grinding with a three-roll grinder so asto obtain masterbatch; and then adding metal hybrid cage silsesquioxane, hydrogen-containing silicone oil, 1-ethynyl-1-cyclohexanol, the platinum catalyst and the like into the masterbatch, and then carrying out mechanical mixing and vulcanization so as to obtain the addition type liquid silicone rubber. The prepared silicon rubber of the invention has excellent resistance to thermo-oxidative aging, high transparency and good mechanical properties, and can be applied to fields such as aerospace and aviation, the nuclear power industry, electronic appliances and medical equipment.

Description

technical field [0001] The invention relates to the field of heat and oxygen aging modification of organosilicon polymer materials, in particular to a highly transparent heat and oxygen aging addition type liquid silicone rubber and a preparation method thereof. Background technique [0002] Because of its excellent high and low temperature resistance, ozone aging resistance and electrical insulation, silicone rubber is widely used in aerospace, nuclear power industry and electronic appliances as potting glue, sealing ring and heat insulation coating. areas with high performance requirements. When used in a high temperature environment for a long time, silicone rubber will be attacked by high heat and atomic oxygen, and the side chain groups will be oxidized and degraded to generate a large number of free radicals, which will trigger further crosslinking, making it hard and brittle, and eventually lose its mechanical properties and use value. With the increasingly harsh us...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L83/07C08L83/05C08L83/08C08K3/36C08K5/5445
Inventor 赖学军邱杰东曾幸荣李红强
Owner SOUTH CHINA UNIV OF TECH
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