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Symmetrical tetraphenyl phenyl vinyl silicone oil and preparation method thereof

A technology of phenylvinyl silicon and polyvinyl silicone oil, which is applied in the field of synthesizing symmetrical tetraphenyl phenyl vinyl and its preparation, can solve the problems of increasing system viscosity, unevenness, affecting process performance, etc., and achieve improvement The effect of bond strength and strong thermal deformation resistance

Pending Publication Date: 2021-11-26
沈阳先进涂层材料产业技术研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, these commonly used silicone oils cannot be used under special conditions, such as aerospace, nuclear industry and other extreme conditions, which require silicone oils with tetraphenyl or condensed ring groups, and substances containing polyphenyl rings are more likely to absorb high-energy rays radiant energy, the energy is dispersed in the large conjugated system, and then the energy is emitted to the surrounding environment in the form of light and heat, but the existing silicone oil with non-uniform distribution of tetraphenyl groups, in Adding to the system will increase the viscosity of the system and affect the process performance, and the non-uniform distribution of tetraphenyl groups will easily cause local inhomogeneity when dispersing energy

Method used

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  • Symmetrical tetraphenyl phenyl vinyl silicone oil and preparation method thereof
  • Symmetrical tetraphenyl phenyl vinyl silicone oil and preparation method thereof
  • Symmetrical tetraphenyl phenyl vinyl silicone oil and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Put 5 parts of tetraphenylcyclopentadienone powder and 50 parts of xylene into a 200ml three-necked flask with a condensation reflux device, magnetic stirring and ventilation device, and keep the temperature at 50°C until the tetraphenylcyclopentadienone is completely After dissolving, heat up to 75°C, slowly add 20 parts of polyvinyl silicone oil (containing 0.04 mol / L of vinyl group) into the system, stir for 5min after the dropwise addition, and slowly drop 1 part of α-chloronaphthalene in 20min Add it to the three-necked flask, introduce nitrogen (speed 1m / s), heat up to 155°C to continue the reaction, when the color of the reaction system turns dark green into an orange transparent solution, heat up to 220°C and continue the reaction for 15 hours, stop the reaction, slowly Cool the product to 20°C, place the product in a separatory funnel and stand for layers, collect the upper layer product, wash the collected upper layer product with methanol until transparent, an...

Embodiment 2

[0031] Put 5 parts of tetraphenylcyclopentadienone powder and 60 parts of xylene into a 200ml three-necked flask with a condensation reflux device, magnetic stirring and ventilation device, and keep it at a constant temperature of 50 ° C until the tetraphenylcyclopentadienone is completely After dissolving, the temperature was raised to 85°C, and 25 parts of polyvinyl silicone oil (containing 0.04 mol / L of vinyl group) was slowly added to the system. Add it to the three-necked flask, introduce nitrogen (speed 1.5m / s), heat up to 165°C to continue the reaction, when the color of the reaction system turns dark green into an orange transparent solution, heat it up to 220°C and continue the reaction for 15 hours, stop the reaction, The product was slowly cooled to 20°C, the product was placed in a separatory funnel and then left to stand for stratification, the upper layer product was collected, the collected upper layer product was washed with methanol until transparent, and metha...

Embodiment 3

[0033] Put 10 parts of tetraphenylcyclopentadienone powder and 80 parts of xylene into a 200ml three-necked flask with a condensation reflux device, magnetic stirring and ventilation device, and keep it at a constant temperature of 50 ° C until the tetraphenylcyclopentadienone is completely After dissolving, heat up to 75°C, slowly add 20 parts of polyvinyl silicone oil (containing 0.054 mol / L of vinyl group) into the system, stir for 5min after the dropwise addition, and slowly drop 2 parts of α-chloronaphthalene in 30min Add it to the three-necked flask, introduce nitrogen (speed 1.5m / s), heat up to 155°C to continue the reaction, when the color of the reaction system turns dark green into an orange transparent solution, heat up to 230°C and continue the reaction for 10 hours, stop the reaction, The product was slowly cooled to room temperature, the product was placed in a separatory funnel and then left to stand for stratification, the upper layer product was collected, the ...

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Abstract

The invention belongs to the field of high polymer materials, and particularly relates to symmetric tetraphenyl phenyl vinyl silicone oil and a preparation method thereof. The symmetric tetraphenyl phenyl vinyl silicone oil is synthesized from tetraphenyl cyclopentadienone and polyvinyl silicone oil in a normal-pressure open system of chloronaphthalene. The synthesized symmetric tetraphenyl phenyl vinyl silicone oil is mainly used for high-temperature-resistant auxiliaries and radiation-resistant auxiliaries of silicone rubber and silicon resin adhesives. When the silicone rubber is vulcanized, the symmetric tetraphenyl phenyl vinyl silicone oil can participate in a cross-linking reaction of the silicone rubber and is bonded to a macromolecular chain of the silicone rubber. The function of phenyl groups of symmetrically distributed tetraphenyl groups is equivalent to that of a nanoscale reinforced phase, so that the heat deformation resistance, the heat aging resistance, the high temperature resistance, the irradiation resistance and the solvent resistance are relatively high. The symmetric tetraphenyl phenyl vinyl silicone oil is used for improving the bonding strength, shear strength and high temperature resistance of the silicon resin adhesive.

Description

technical field [0001] The invention belongs to the field of macromolecular materials, in particular to a symmetrical tetraphenyl phenyl vinyl silicone oil and a preparation method thereof, in particular to the use of tetraphenyl cyclopentadienone and polyvinyl silicone oil in the normal pressure opening of chloronaphthalene In the formula system, a symmetrical tetraphenyl phenyl vinyl group and a preparation method thereof are synthesized. Background technique [0002] Silicone oil is a linear structure oil formed by hydrolysis and polycondensation of bifunctional or monofunctional organosilicon monomers. It is a chain polysilicon oil with different degrees of polymerization. Its structural formula: [0003] [0004] In the formula, n is the degree of polymerization, R is a hydrocarbon group such as methyl, ethyl, and phenyl, and X is a hydroxyl group or hydrogen. Another type of silicone oil is modified silicone oil. The main chain of the molecule is not entirely comp...

Claims

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Application Information

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IPC IPC(8): C08G77/20
CPCC08G77/20
Inventor 郭书利李娜孙洪涛史胜南高博陈栋何晓峰
Owner 沈阳先进涂层材料产业技术研究院有限公司
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