A kind of high temperature resistant halogen-free flame retardant silicone rubber and preparation method thereof

A silicone rubber and high temperature resistant technology, which is applied in the field of high temperature resistant halogen-free flame retardant silicone rubber and its preparation, can solve the problems of preparation and application research that have not been reported, limit practical application, etc., and achieve the purpose of inhibiting the degradation of snapping and reducing the impact , high efficiency effect

Active Publication Date: 2020-06-19
SOUTH CHINA UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, fullerenes can inhibit the normal vulcanization of high temperature vulcanized silicone rubber (HTVSR) by capturing free radicals generated by peroxide vulcanizing agents, which greatly limits its practical application in silicone rubber.
Therefore, the preparation and application of high-temperature vulcanized silicone rubber / fullerene nanocomposites have not been reported yet.

Method used

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  • A kind of high temperature resistant halogen-free flame retardant silicone rubber and preparation method thereof
  • A kind of high temperature resistant halogen-free flame retardant silicone rubber and preparation method thereof
  • A kind of high temperature resistant halogen-free flame retardant silicone rubber and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] 6.00g fullerene C 60 Ultrasonic dispersion in 200mL benzene organic solvent, then add 6.00g aminopropyl polydiphenylsiloxane (viscosity at 25°C is 2000mPa·s, nitrogen content is 0.05wt%), stir at 100°C for 12h , after rotary evaporation, 100mL ethanol washing and centrifugation for 3 times, and vacuum drying at 50°C for 24h, the aminophenyl silicone oil modified fullerene 1 was obtained, its structural formula is as follows:

[0043] Where n is 40-50;

[0044] Aminophenyl silicone oil modified fullerene 1 obtained in embodiment 1 is carried out infrared spectrum analysis, and aminophenyl silicone oil modified fullerene 1 mainly has following characteristic peak: 3440cm -1 (υ N-H ), 2963cm -1 (υ C-H ), 1200~1000cm -1 (υ Si-O-Si ), 575 and 525cm -1 (υ C＝C ), indicating that the aminophenyl silicone oil modified fullerene 1 was successfully synthesized.

[0045] In parts by mass, 93 parts of vinyl-terminated polydimethylsiloxane (molecular weight 5.5*10 5 g / mol...

Embodiment 2

[0051] 6.00g fullerene C 60 Ultrasonic dispersion in 200mL benzene organic solvent, then add 6.00g aminopropyl polymethylphenylsiloxane (viscosity at 25°C is 500mPa·s, nitrogen content is 0.3wt%), stir at 100°C After 12 hours, rotary evaporation, 100mL ethanol washing and centrifugation for 3 times, and vacuum drying at 50°C for 24 hours, the aminophenyl silicone oil modified fullerene 2 was obtained, whose structural formula is as follows:

[0052]

[0053] Where n is 10-20, m is 5-10;

[0054] In parts by mass, 93 parts of vinyl-terminated polydimethylsiloxane (molecular weight 5.5*10 5 g / mol, vinyl content is 0.025mol%), 7 parts of polymethylvinylsiloxane (molecular weight is 5*10 5 g / mol, vinyl content is 2.03mol%), 40 parts of fumed silica (specific surface area 220m 3 / g, particle size 35nm), 0.6 parts of hydrogen-containing silicone oil (molecular weight is 3000g / mol, hydrogen content is 1.2wt%) and 6 parts of hydroxyl silicone oil (molecular weight is 450g / mol, h...

Embodiment 3

[0058] The difference between this example and Example 1 is that the amount of aminopropyl polydiphenylsiloxane is changed to 12.00 g, the benzene solvent is changed to toluene solvent, and the reaction is carried out at 110° C. for 20 hours. It can be seen from Table 1 that the vulcanization performance of silicone rubber does not change much, the highest service temperature reaches 350 °C, the tensile strength and elongation at break are maintained at 7.9MPa and 586%, respectively, and the LOI is 30.0%. The performance has passed the UL‐94V‐0 rating. After aging at 300℃ for 24h, the tensile strength and elongation at break of the silicone rubber remained at 5.9MPa and 483%, respectively. It shows that aminophenyl silicone oil modified fullerene can significantly improve the high temperature resistance and flame retardancy of silicone rubber without affecting the mechanical properties of silicone rubber.

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Abstract

The invention discloses high-temperature-resisting halogen-free and flame-retarding silicon rubber and a preparation method thereof. A formula comprises the following raw materials in parts by mass: 100 parts of methyl vinyl silicon rubber, 20 to 50 parts of white carbon black, 5 to 7 parts of a structured control agent, 0.5 to 2 parts of hydrogen-contained silicone oil, 1 to 5 parts of amino phenyl silicone oil modified fullerene and 1 to 5 parts of a peroxide vulcanizing agent. A preparation process comprises the following steps: firstly, uniformly mixing the methyl vinyl silicon rubber, thewhite carbon black, the structured control agent and the hydrogen-contained silicone oil through a vacuum kneading machine; then adding the amino phenyl silicone oil modified fullerene and the peroxide vulcanizing agent and uniformly mixing; finally, carrying out high-temperature vulcanization to obtain the high-temperature-resisting halogen-free and flame-retarding silicon rubber. The silicon rubber prepared by the invention has excellent high-temperature-resisting performance and flame-retarding performance, and can be used as a package material applied to fields including LED (Light Emitting Diode), electronics and electrical appliances, automobile industries, aerospace and the like.

Description

technical field [0001] The invention relates to the field of high temperature resistant and flame retardant modification of organosilicon polymer materials, in particular to a high temperature resistant halogen-free flame retardant silicone rubber and a preparation method thereof. Background technique [0002] Silicone rubber is a special rubber with Si‐O‐Si as the main chain, which has excellent high and low temperature resistance, oil resistance, chemical resistance, weather resistance and electrical insulation properties. However, with the popularization and application of silicone rubber in the fields of aerospace, automobile manufacturing and high-voltage power transmission and transformation, higher requirements are put forward for the service performance of silicone rubber. Silicone rubber is in high temperature or burning environment, the free radicals (peroxide radicals, methyl radicals) produced by the oxidation and degradation of side methyl groups will cause furt...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L83/07C08L83/05C08K9/06C08K3/04C08K5/14C08K3/36C08K13/06
CPCC08L83/04C08L2201/02C08L2201/08C08L2201/22C08L2205/025C08K9/06C08K3/045C08K5/14C08K3/36C08K13/06
Inventor 赖学军邱杰东曾幸荣李红强陈桂忠周游
Owner SOUTH CHINA UNIV OF TECH
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