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Dendritic organosilicon compounds with multiterminal functional groups and preparing method of dendritic organosilicon compounds

A technology of organosilicon compounds and functional groups, applied in the field of dendritic organosilicon compounds and their preparation, can solve problems such as poor repeatability, and achieve the effects of good modifiability, good solubility and clear structure

Inactive Publication Date: 2019-10-29
HUBEI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN102863623A publicly reported a two-step circulation method for the preparation of dendritic organic silicon products through a hydrosilylation reaction and then a reduction reaction. Two-step cycle method to prepare branched silicone products, but there are uncertainties in the above synthesis process, and the reproducibility of the reaction is poor

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  • Dendritic organosilicon compounds with multiterminal functional groups and preparing method of dendritic organosilicon compounds
  • Dendritic organosilicon compounds with multiterminal functional groups and preparing method of dendritic organosilicon compounds
  • Dendritic organosilicon compounds with multiterminal functional groups and preparing method of dendritic organosilicon compounds

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preparation example Construction

[0018] Embodiments of the present invention provide a method for preparing a dendritic organosilicon compound with multi-terminal functional groups, comprising the following steps:

[0019] Step S1, polymethoxysilane (R (4-n) Si(OCH 3 ) n ; R is any one of alkyl and phenyl; n=2,3) and tetramethyldihydrodisiloxane (HSi(CH 3 ) 2 OSi(CH 3 ) 2 H) Mix according to a certain ratio, adjust the pH value to 1 with acid, add a catalyst with a total mass of 2000ppm, react at 50±2°C for 1h to 1.5h, reduce the pressure to 6kPa after the reaction, and distill at 120°C for 2h to obtain terminal silicon hydrogen bonded silicone products (R (4-n) Si(OSi(CH 3 ) 2 h) n ); the acid used to adjust the pH is selected from any of hydrochloric acid, sulfuric acid, glacial acetic acid, etc.; the catalyst is selected from any of p-toluenesulfonic acid, dodecylbenzenesulfonic acid, acetic anhydride or trifluoromethanesulfonic acid.

[0020] Step S2, in a nitrogen atmosphere, combine the silico...

Embodiment 1

[0025] (1) Mix 41.27 g of phenyltrimethoxysilane with 44.80 g of tetramethyldihydrodisiloxane, adjust the pH value to 1 with hydrochloric acid, then add 1.56 g of trifluoromethanesulfonic acid and react at 50°C for 1 hour. After the reaction Reduced pressure to 6kPa and distilled at 120°C for 2h to obtain 59.49g of organosilicon product A with silicon-hydrogen bond;

[0026] (2) In a nitrogen environment, take 33.06g of the silicon-hydrogen bond-terminated organosilicon product A obtained in step (1) and mix it with 88.94g of vinyltrimethoxysilane, and then add 0.1220g of a platinum catalyst to undergo a hydrosilylation reaction, React at 80°C for 5h, after the reaction is over, reduce the pressure to 6kPa and distill at 120°C for 2h to obtain 71.45g 3 ) 3 ) organosilicon product A;

[0027] (3) Mix 31.00 g of the organosilicon product A with multiple methoxy groups at the end obtained in step (2) with 31.44 g of tetramethyldihydrodisiloxane, adjust the pH value to 1 with hy...

Embodiment 2

[0034] (1) Mix 27.20g of methyltrimethoxysilane with 52.49g of tetramethyldihydrodisiloxane, adjust the pH value to 1 with hydrochloric acid, then add 0.24g of trifluoromethanesulfonic acid and react at 50°C for 1h. After the end, reduce the pressure to 6kPa and distill at 120°C for 2h to obtain 40.58g of organosilicon product C with silicon-hydrogen bond;

[0035] (2) In a nitrogen environment, take 24.15g of the silicon-hydrogen bond-terminated organosilicon product C obtained in step (1) and mix it with 60.06g of vinyltrimethoxysilane, then add 0.0675g of a platinum catalyst to undergo a hydrosilylation reaction, React at 90°C for 5h, after the reaction is over, reduce the pressure to 6kPa and distill at 120°C for 2h to obtain 55.86g of 3 ) 3 ) organosilicon product C;

[0036] (3) Take 14.26g of the end obtained in step (2) with multiple methoxy groups (-Si(OCH 3 ) 3 ) organosilicon product C and 15.72g tetramethyldihydrodisiloxane press, adjust the pH value to 1 with ...

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Abstract

The invention provides a preparation method of dendritic organosilicon compounds with multiterminal functional groups through a two-step circulating method. The preparation method comprises the following steps that S1, polymethoxylsilane and tetramethyldihydrodisiloxane are mixed, acid is used for adjusting the pH value to be one, a catalyst is added for a reaction, and thus an organosilicon product with a terminal silicon-hydrogen bond is obtained; S2, in a nitrogen atmosphere, the organosilicon product, obtained in the step S1, with the terminal silicon-hydrogen bond is mixed with vinyl trimethoxysilane, hydrosilylation is conducted under the effect of a platinum catalyst, and thus an organosilicon product with a plurality of methoxy groups at the terminal is obtained; and S3, the organosilicon product, obtained in the step S2, with the multiple methoxy groups at the terminal serves as a reactant, reactions in the step S1 and the step S2 are sequentially repeated according to the sequence, and thus the dendritic organosilicon compounds with different structures and the multiterminal functional groups (-Si(OCH3)3 or -SiH) are obtained.

Description

technical field [0001] The invention relates to the field of preparation of organic functional materials, in particular to a class of dendritic organosilicon compounds with multi-terminal functional groups and a preparation method thereof. Background technique [0002] Dendrimer has the advantages of good solubility, low viscosity, no crystallization, and no entanglement between molecular chains, and it has been widely used in the fields of fluorescent materials, photoelectric materials, and modified materials. The preparation of dendrimers is mainly a cyclic two-step method. Patent CN102863623A publicly reported a two-step circulation method for the preparation of dendritic organic silicon products through a hydrosilylation reaction and then a reduction reaction. A two-step cycle method is used to prepare branched organosilicon products, but there are uncertainties in the above-mentioned synthesis process, and the repeatability of the reaction is poor. Contents of the in...

Claims

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Application Information

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IPC IPC(8): C08G83/00
CPCC08G83/003
Inventor 孙争光付道松吴军张文镐詹园黄世强
Owner HUBEI UNIV