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High-heat-resistance copolymerized silicon resin and preparation method thereof

A technology of silicone resin and high heat resistance, applied in the field of organic polymer materials, can solve the problems of great hidden dangers in the use of products in high temperature environments

Active Publication Date: 2021-09-14
NEW MATERIAL INST OF SHANDONG ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, such a result has a great hidden danger to the use of the product in a high-temperature environment.

Method used

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  • High-heat-resistance copolymerized silicon resin and preparation method thereof
  • High-heat-resistance copolymerized silicon resin and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0032] 200g hydroxyl-terminated polydimethylsiloxane (molecular weight 10×10 4 g / mol) and 6.5 g of triethylamine were dissolved in 600 g of toluene at room temperature, and were dropped into 125 g of phenyltrichlorosilane for 2 hours. After the feeding was completed, the reaction mixture was warmed up to reflux, reacted for 3h, then the mixture was cooled to room temperature, mixed with 18.5g tetramethyldivinyldisiloxane, added dropwise with 300g tetramethylammonium hydroxide (25% aqueous solution ) and 250g of water to make a strong alkali solution, and drop it in 3 hours. After the feeding was completed, the reaction was continued for 5 h at the reflux temperature of the solvent. After the reaction, the lower water layer was separated, the upper oil layer was washed with water until neutral, dried to remove water, and the solvent was evaporated under reduced pressure at 80°C, and the product was dried at 130°C for 3 hours to obtain 317g of copolymerized silicone resin with ...

Embodiment 2

[0034] 200g hydroxyl-terminated polydimethylsiloxane (molecular weight 5.8×10 5 g / mol) According to the reaction steps of Example 1, 310 g of copolymerized silicone resin was prepared, with a yield of 96%.

Embodiment 3

[0036] 200g hydroxyl-terminated polymethylphenylsiloxane (molecular weight 8.5×10 4 g / mol) and 6.5 g of triethylamine were dissolved in 800 g of xylene at room temperature, and were dropped into 125 g of phenyltrichlorosilane for 2 hours. After the feeding was completed, the temperature of the reaction mixture was raised to reflux for 3 hours of reaction, and then the mixture was cooled to room temperature and mixed with 20.6 g of dimethylvinylchlorosilane. Drop it into a strong alkali solution made of 85gKOH and 400g water, and finish dropping in 4h. After the feeding was completed, the reaction was continued for 5 h at the reflux temperature of the solvent. After the reaction, the lower water layer was separated, the upper oil layer was washed with water until neutral, dried to remove water, and the solvent was evaporated under reduced pressure at 80°C, and the product was dried at 130°C for 3 hours to obtain 314g of copolymerized silicone resin with a yield of 97% %.

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Abstract

The invention relates to a high-heat-resistance copolymerized silicon resin and a preparation method thereof. The preparation method comprises the following steps: catalyzing hydroxyl-terminated linear polysiloxane and organic trichlorosilane to be precondensed by using a weak base compound in an organic solvent medium, then carrying out cohydrolytic condensation under the action of a strong base to obtain a copolymer, and carrying out high-temperature curing on the copolymer to obtain a product with the structural formula of (R1R2ViSiO0.5)a(R1R2SiO)b(R3SiO1.5)c, wherein a+b+c=1, a:c=(3-20):1, b:c=(1-6):1, R1, R2 and R3 are the same or different and are selected from one or more of Me, Ph and Vi, and the number-average molecular weight is 5*10<4>-10<6>. The copolymerized silicon resin not only can keep good physical and mechanical properties, but also has high heat resistance, can be used for a long time at 300 DEG C, and still keeps high strength and high elasticity after being subjected to thermo-oxidative aging for 72 hours in an environment at 350 DEG C.

Description

technical field [0001] The invention relates to a silicone resin, in particular to a high heat-resistant copolymerized silicone resin and a preparation method thereof, belonging to the technical field of organic polymer materials. Background technique [0002] Silicone (containing T-links (RSiO 1.5 ) or Q link (SiO 2 )) polysiloxane with highly cross-linked network structure, linear polysiloxane system (D chain link (R 1 R 2 SiO)) has good compatibility and dispersion, and is one of the important reinforcing materials for silicone rubber materials. Huang Dejun et al. (Plastic Industry, 1988, 5, p20-24) prepared linear dimethylpolysiloxane and A block copolymer composed of bulk organopolysiloxane, the product has the characteristics of both silicone rubber and silicone resin. Hu Chunye et al. (Elastomer, 1996, 6(3), p14~19) prepared polydimethylsiloxane by direct cohydrolysis and condensation reaction of phenyltrimethoxysilane and hydroxyl-terminated polydimethylsiloxane...

Claims

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Application Information

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IPC IPC(8): C08G77/44
CPCC08G77/44
Inventor 牟秋红彭丹李金辉张硕王峰张方志
Owner NEW MATERIAL INST OF SHANDONG ACADEMY OF SCI
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