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Phenylsilane purification method

A purification method, phenylsilane technology, applied in the direction of silicon organic compounds, can solve the problems of high cost, difficult separation, and inability to meet the application requirements of high-purity diphenylsilane

Active Publication Date: 2022-04-01
ZHENGZHOU SIGMA CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002]Diphenyldisilane (Formula Ia) has good photoelectric and material properties, and is used in photoresist, olefin polymerization photoinitiator, thin film optical waveguide , organic photoconductors, ultraviolet optical materials and other fields that require higher product purity, but there is no report on the simple purification method for diphenylsilane, so it is of great significance to study the purification of diphenylsilane
[0006] The above-mentioned references all use phenylchlorosilane as raw material, but the reaction between phenylchlorosilane and water is very easy to produce the impurity diphenyl diphenyl disulfide expressed in (formula IIa) Siloxane, its reaction is as recorded in the document Journal of the Chemical SocietyPerkin transactions I, 1998,7,1209, can not meet the application requirements of high-purity diphenylsilane, and needs to be purified, but the boiling point of the impurity formula IIa compound is the same as that of the formula The boiling point of the Ia compound diphenylsilane is close, so it is very difficult to separate the two by methods such as rectification, the efficiency is low, and the cost is high, which needs to be improved.

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0038] Mix 100 g of crude diphenyltetramethyldisilane (compound Ia) with an impurity compound IIa content of 11.2%, 8.5 g of boron trifluoride etherate complex, and 800 mL of toluene, stir and heat up, and keep the reaction at 70 ° C for 4 h. After the reaction, the temperature was raised to 80° C. at -0.1 MPa to separate low-boiling point impurities from diphenyltetramethyldisilane by distillation to obtain 83.6 g of refined diphenyltetramethyldisilane.

[0039] The gas chromatogram before the purification of diphenyltetramethyldisilane is as follows figure 2 As shown, the purity before purification was 83.5%, and the content of impurity compound IIa was 11.2%. The gas chromatogram after diphenyltetramethyldisilane purification is as follows image 3 As shown, its purified purity is 99.9%.

[0040]

[0041] The proton nuclear magnetic resonance spectrum figure of the diphenyltetramethyldisilane of the present embodiment is as follows figure 1 shown by figure 1 It can ...

Embodiment 2

[0043] Mix 1Kg of diphenyltetramethyldisilane (Compound Ia) crude liquid with impurity compound IIa content of 9.4%, 120g of boron trifluoride etherate complex and 2L of toluene, stir and heat up, and keep the reaction at 80°C for 8h. After the reaction, the temperature was raised to 85° C. at -0.1 MPa to separate low-boiling point impurities from diphenyltetramethyldisilane by distillation to obtain 897.9 g of refined diphenyltetramethyldisilane.

[0044] The gas chromatogram before the purification of diphenyltetramethyldisilane is as follows Figure 4 As shown, the purity before purification was 89.7%, and the content of impurity compound IIa was 9.4%. The gas chromatogram after diphenyltetramethyldisilane purification is as follows Figure 5 As shown, its purified purity is 99.9%.

Embodiment 3

[0046] 150g impurity compound IIb content is 7.6% bis (4-methoxyphenyl) -1,1,2,2-tetramethyldisilane (compound Ib) crude product solution, 14.0g boron trifluoride diethyl ether complex Mix the mixture with 600mL toluene and stir to raise the temperature, and keep it warm at 80°C for 5h. After the reaction, heat up to 120°C at -0.09MPa to distill the low-boiling impurities and bis(4-methoxyphenyl)-1,1 , 2,2-Tetramethyldisilane was separated to obtain 138.1 g of refined bis(4-methoxyphenyl)-1,1,2,2-tetramethyldisilane.

[0047] The gas chromatogram of bis(4-methoxyphenyl)-1,1,2,2-tetramethyldisilane before purification is as follows Image 6As shown, wherein, its purity before purification is 92.0%, and the content of impurity compound IIb is 7.6%. The gas chromatogram after purification of bis(4-methoxyphenyl)-1,1,2,2-tetramethyldisilane is as follows Figure 7 As shown, its purified purity is 99.9%.

[0048]

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Abstract

The invention discloses a purification method of phenylsilane, diphenyl siloxane in a phenylsilane crude product reacts with a boron trifluoride complex in an organic solvent, high-boiling-point impurities are decomposed into low-boiling-point impurities, then the low-boiling-point impurities are conveniently separated out in a distillation mode, and the purification method is high in yield, high in reaction efficiency, low in cost and safe to operate. And the method accords with the current clean production concept and has good industrial application value.

Description

technical field [0001] The invention relates to the technical field of purification, in particular to a method for purifying phenylsilane. Background technique [0002] Diphenyldisilane (Formula Ia) has good photoelectric and material properties, and is used in photoresists, olefin polymerization photoinitiators, thin film optical waveguides, organic photoconductors, ultraviolet optical materials, etc. for product purity requirements Higher fields, but now there is no report on the simple purification method for diphenylsilane, so it is of great significance to study the purification of diphenylsilane. [0003] [0004] Documents J.Organomet Chem., 2007, 692, 3559; Organometallics, 2019, 38, 2902 and Dalton T, 2020, 49, 1731 all report a method for preparing diphenyldisilane from phenylchlorosilane , the reaction equation is as follows: [0005] [0006] The above-mentioned references all use phenylchlorosilane as a raw material, but the reaction of phenylchlorosilan...

Claims

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Application Information

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IPC IPC(8): C07F7/08C07F7/20
Inventor 汪游清余明慧杨勇金金
Owner ZHENGZHOU SIGMA CHEM
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