A kind of high heat-resistant copolymerized silicone resin and preparation method thereof

A silicone resin and high heat-resistant technology, 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, and achieve high heat resistance, mild reaction conditions, and simple operation

Active Publication Date: 2022-07-12
NEW MATERIAL INST OF SHANDONG ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • A kind of high heat-resistant copolymerized silicone resin and preparation method thereof
  • A kind of high heat-resistant copolymerized silicone resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 200 g of 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 dropped into 125 g of phenyltrichlorosilane for 2 h. After the feeding was completed, the reaction mixture was heated to reflux for 3 hours, then the mixture was cooled to room temperature, mixed with 18.5 g of tetramethyldivinyldisiloxane, and added dropwise to 300 g of tetramethylammonium hydroxide (25% aqueous solution). ) and 250g of water into a strong alkaline solution, dripped for 3h. After the feeding was completed, the temperature was raised to the reflux temperature of the solvent and the reaction was continued for 5 h. After the reaction, the lower water layer was separated, the upper oil layer was washed with water until neutral, dried to remove water, the solvent was evaporated under reduced pressure at 80°C, and the product was continued to be dried at 130°C for 3 hours to obtain 317 g of...

Embodiment 2

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

Embodiment 3

[0036] 200 g of 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, dropped into 125 g of phenyltrichlorosilane, and dropped in 2 h. After the feeding was completed, the reaction mixture was heated to reflux for 3 h, then the mixture was cooled to room temperature and mixed with 20.6 g of dimethylvinylchlorosilane. Drop into the strong alkali solution made up of 85g KOH and 400g water, and finish dropping in 4h. After the feeding was completed, the temperature was raised to the reflux temperature of the solvent and the reaction was continued for 5 h. After the reaction, the lower water layer was separated, the upper oil layer was washed with water until neutral, dried to remove water, the solvent was evaporated under reduced pressure at 80°C, and the product was further dried at 130°C for 3 hours to obtain 314 g of copolymerized silicone resin with a yield of 97 %.

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Abstract

The invention relates to a high heat-resistant copolymerized silicone resin and a preparation method thereof. The pre-condensation of hydroxyl-terminated linear polysiloxane and organotrichlorosilane is catalyzed by a weak base compound in an organic solvent medium, and then under the action of a strong base Co-hydrolysis condensation obtains a copolymer, and the copolymer is cured at high temperature to obtain a product, and its structural formula is: (R 1 R 2 ViSiO 0.5 ) a (R 1 R 2 SiO) b (R 3 SiO 1.5 ) c ; where a+b+c=1, a:c=3~20:1; b:c=1~6:1; R 1 , R 2 , R 3 Same or different one or more selected from Me, Ph, Vi; its number-average molecular weight is 5×10 4 ~10 6 . The copolymerized silicone resin not only maintains good physical and mechanical properties, but also has high heat resistance, can be used for a long time at 300 ° C, and still maintains high strength and high elasticity under thermal oxygen aging at 350 ° C for 72 hours.

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 resin (including T-links (RSiO 1.5 ) or Q link (SiO 2 )) polysiloxanes with a highly cross-linked network structure, in-line polysiloxane systems (D segment (R 1 R 2 SiO)) has good compatibility and dispersibility, and is one of the important reinforcing materials for silicone rubber materials. Huang Dejun et al. (Plastics Industry, 1988, 5, p20~24) prepared linear dimethylpolysiloxane and polydimethylsiloxane by the pre-condensation of hydroxyl-terminated polydimethylsiloxane and chlorosilane, followed by co-hydrolysis and polycondensation. A block copolymer composed of bulk organopolysiloxane, the product has the characteristics of both silicone rubber and silicone resin. Hu Chunye et al. (Elastomers, 1...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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