Optically transparent organosilicon material and preparation method thereof

An optically transparent and organosilicon technology, applied in the field of UV-curable optically transparent organosilicon materials and their preparation, can solve the problems of complex polymer material composition, high cost, poor mechanical and mechanical properties, and inconvenience for industrialization, so as to improve mechanical and mechanical properties. and thermal stability, good mechanical properties and thermal stability

Active Publication Date: 2020-05-05
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the problems of poor mechanical properties of unmodified optically transparent silicone materials, long curing time during preparation, or high energy consumption, as well as the complex composition and high cost of existing UV-curable polymer materials, it is not convenient for industrialization For these problems, the present invention proposes an optically transparent organic silicon material and a preparation method thereof, by adopting hyperbranched vinyl polycarbosilane and mercapto silicone resin through thiol-ene click reaction, and obtaining material mechanical properties and thermal stability through UV curing Good optically transparent silicone material, without the use of photoinitiators, diluents and various additives, the material composition is simple, cost saving, and easy for industrialization

Method used

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  • Optically transparent organosilicon material and preparation method thereof
  • Optically transparent organosilicon material and preparation method thereof
  • Optically transparent organosilicon material and preparation method thereof

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preparation example Construction

[0036] Preparation of GS-1Vi: Under anhydrous and anaerobic conditions, place Mg chips (60g, 2.500mol) and two grains of iodine in a clean three-necked flask, then add ether (1000ml), and cool the mixed system to After 0~5C, a mixed solution of diethyl ether (200ml) and allyl bromide (252.0g, 2.100mol) was slowly added dropwise. After the dropwise addition, react at 0-5°C for 2 hours to obtain an ether solution of allylmagnesium bromide Grignard reagent. Mercaptopropyltrimethoxysilane (82.450g, 0.420mol, 0.5 times excess) and diethyl ether (3000mL) were mixed with a dropping funnel, slowly added dropwise to the allylmagnesium bromide solution within 30 minutes, and the mixture was After stirring overnight at room temperature, the reaction was quenched with methanol and filtered. The organic phase was dried with anhydrous magnesium sulfate, and the solvent was removed under reduced pressure to obtain 53.78 g of colorless liquid mercaptopropyltriallylsilane (yield 85%, the prep...

Embodiment 1

[0055] (1) Under anhydrous and oxygen-free conditions, 45.2 g of a colorless, transparent, viscous oily product GS-1Vi was prepared according to the aforementioned method.

[0056] (2) Under mechanical stirring at 50°C, add 78.54g 3-mercaptopropyltrimethoxysilane, 48.75g dimethyldiethoxysilane, 47.98g methyltrimethoxysilane, 1.62g hexamethyldisiloxane Add dropwise the mixture of 56.2g of deionized water and 3.5g of 36.5% concentrated hydrochloric acid in the mixture of alkane (according to the mercapto group content of 0.4mol / g, the organic group / silicon atom is 1.3 ratio) and 175g of toluene, 0.5h dropwise Then continue to react at 50°C for 18h, then wash with water until neutral, and remove the solvent, residual raw materials and low-molecular products under reduced pressure at 130mmHg / 170°C to obtain 70.5g of colorless and transparent mercapto-containing polysiloxane.

[0057] (3) Take 8 g of mercapto-containing polysiloxane and 2.4 g of GS-1Vi, mix evenly, degas under vacu...

Embodiment 2

[0060] (1) Under anhydrous and oxygen-free conditions, 135.6 g of a colorless, transparent, viscous oily product GS-6Vi was prepared according to the aforementioned method.

[0061] (2) Under mechanical stirring at 40°C, add 78.54g 3-mercaptopropyltrimethoxysilane, 64.34g dimethyldiethoxysilane, 32.83g methyltrimethoxysilane, 1.62g hexamethyldisiloxane Add a mixture of 127.2 g of deionized water and 8.785 g of p-toluenesulfonic acid dropwise to a mixture of alkane (according to the mercapto group content of 0.4 mol / g, organic group / silicon atom ratio of 1.4) and 351.4 g of xylene, dropwise for 0.5 h After completion, continue to react at 40°C for 24h, then wash with water until neutral, and remove the solvent, residual raw materials and low-molecular products under reduced pressure at 130mmHg / 170°C to obtain 75.8g of colorless and transparent mercapto-containing polysiloxane.

[0062] (3) Take mercaptopolysiloxane and GS-6Vi according to the proportions in Table 1 below, mix t...

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Abstract

The invention relates to the field of organic polymer materials. In order to solve the problems that an existing unmodified optically transparent organosilicon material is poor in mechanical property,the curing time is long or the energy consumption is high in the preparation process and an existing UV curing high polymer material is relatively complex in composition and relatively high in cost and these problems are inconvenient for industrialization, the invention puts forward an optically transparent organosilicon material and a preparation method thereof. Hyperbranched vinyl polycarbosilane and sulfydryl silicon resin are subjected to a thiol-ene click reaction, and after UV curing, the optically transparent organosilicon material with good mechanical properties and thermal stabilityis obtained. The light transmittance in the light wave range of 400-800 nm is larger than 95%, the tensile strength is 0.4-2.1 MPa, the hardness is controllable in the range of B-9H, the thermal decomposition temperature is 285-385 DEG C, the water contact angle is 96.5-106.5 degrees, and the material can be bent. In the preparation method, a photoinitiator, a diluent and various assistants are not needed, the material composition is simple, the cost is saved, and industrialization is facilitated.

Description

technical field [0001] The invention relates to the field of organic polymer materials, in particular to a UV-curable optically transparent organic silicon material based on hyperbranched polycarbosilane and a preparation method thereof. Background technique [0002] Flexible and transparent electronic devices have a wide range of applications in flexible display, wearable devices, wireless communication, human-computer interaction, biomedical and other fields, and high-performance transparent and flexible materials are one of the key raw materials for the preparation of such electronic devices. At present, traditional optically transparent polymer materials such as polymethyl methacrylate and polycarbonate have disadvantages such as high and low temperature resistance, poor aging resistance, large linear expansion coefficient, easy moisture absorption, and poor chemical stability. The development needs of electronic components, etc. Silicone flexible optically transparent ...

Claims

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Application Information

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IPC IPC(8): C08G77/42
CPCC08G77/42
Inventor 杨雄发吴于飞刘江玲焦晓皎程飞来国桥
Owner HANGZHOU NORMAL UNIVERSITY
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