A method for preparing phenyldisilane from organosilicon high boilers

A technology of phenyldisilane and high boilers, applied in the field of organosilicon monomer preparation, can solve the problems of increasing reaction and operation difficulty, unfavorable industrial production, increasing production cost, etc., and achieves increasing high-value utilization, increasing Market application, the effect that is beneficial to industrial production

Active Publication Date: 2017-01-25
INST OF PROCESS ENG CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the activity of Grignard reagent is very high, and it is easy to react violently when encountering water and oxygen, resulting in explosion.
Therefore, the preparation process of this method must ensure an absolutely anhydrous and oxygen-free reaction environment, which

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Rectify the organosilicon high-boiler, take the fraction at 150°C, and obtain Me 4 Cl 2 Si 2 . Under the protection of nitrogen, add 23g Na to 115g toluene, add 1.15g liquid paraffin at the same time, stir and heat to 100°C to prepare sodium sand, add 56.3g chlorobenzene to the prepared sodium sand, and react for 2 hours to obtain Sodium phenyl, add sodium phenyl to 93.5g Me 4 Cl2 Si 2 , while adding 1.87g H(OCH 2 CH 2 ) 3 OH, under the condition of 10°C, after reacting for 3 hours, stop the reaction, cool to room temperature, filter the reaction solution, sample the filtrate, analyze it by gas chromatography, and calculate Me 4 PhSi 2 The yield of Cl is 85.7%, Me 4 Ph 2 Si 2 The yield is 3.8%, and the total yield of target product phenyldisilane with active groups is 89.4%.

Embodiment 2

[0039] Rectify the organosilicon high-boiler, take the fraction at 150°C, and obtain Me 3 Cl 3 Si 2 with Me 4 Cl 2 Si 2 of the mixture. Under the protection of neon gas, add 15g Na and Li alloy to 150g toluene, add 1.5g stearic acid at the same time, stir and heat to 105°C to prepare alkali metal sand, add 78.5g bromobenzene to the prepared alkali metal sand In the sand, reaction equilibrium 2h, obtains phenyl alkali metal salt; The phenyl alkali metal salt is added to 46.8g Me 4 Cl 2 Si 2 , while adding 0.936g H(OCH 2 CH 2 ) 5 OH and 15-C-5 mixed cocatalyst, under the condition of 40 ℃, after reacting for 3 hours, stop the reaction, cool to room temperature, filter the reaction solution, sample the filtrate, analyze it by gas chromatography, and calculate Me 4 PhSi 2 Cl yield is 81.1%, Me 4 Ph 2 Si 2 The yield was 4%, and the total yield of the target product phenyldisilane with active groups was 85.2%.

Embodiment 3

[0041] Rectify the organosilicon high boiler, and take the fraction at 165°C to obtain Me 4 Cl 2 Si 2 with Me 3 Cl 3 Si 2 of mixed components. Under the protection of helium, add 39g K to 390g toluene, add 2.6g oleic acid at the same time, stir and heat to 102°C to prepare potassium sand, add potassium sand to 82.5g Me 4 Cl 2 Si 2 with Me 3 Cl 3 Si 2 Add 0.83g of cyclodextrin and tetraphenylphosphine chloride as a mixing aid to the mixed solution and 56.3g of chlorobenzene mixed solution. After reacting for 4 hours at 30°C, stop the reaction and cool to room temperature. Filter, sample the filtrate, analyze it with gas chromatography, and calculate Me 4 PhSi 2 The yield of Cl is 27.9%, Me 4 Ph 2 Si 2 The yield is 6%, Me 3 PhSi 2 Cl 2 Yield is 39.1%, Me 3 Ph 2 Si 2 The Cl yield is 19%, and the total yield of the target product phenyldisilane with active groups is 86%.

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Abstract

The invention belongs to the field of preparation of organic silicon monomers, and discloses a method for preparing phenyldisilane from an organic silicon high-boiling material. The method comprises the steps of 1) rectifying the organic silicon high-boiling material, and selecting a fraction of 150-180 DEG C to obtain disilane; 2) adding an alkali metal or an alkali metal alloy into methylbenzene under the protection of an inert gas, and simultaneously adding a dispersant to prepare alkali metal sand; and 3) adding the alkali metal sand in the step 2) into a mixed solution of halogenobenzene and the disilane obtained in the step 1), and simultaneously adding a reaction aid to obtain a phenyldisilane product; or adding the halogenobenzene into the alkali metal sand prepared in the step 2), and performing reaction balance for 1-5h to obtain a phenyl alkali metal salt; adding the phenyl alkali metal salt into the disilane obtained in the step 1), and simultaneously adding the reaction aid to obtain the phenyldisilane product. The method disclosed by the invention is mild and controllable in process and simple in operation, the yield of the target product with active groups, namely the phenyldisilane is high, and the method is very favorable for industrial production.

Description

technical field [0001] The invention belongs to the field of organosilicon monomer preparation and relates to a method for preparing phenyldisilane from organosilicon high boilers. Background technique [0002] Organosilicon high boilers are a mixed liquid with pungent odor and strong corrosiveness produced in the process of industrial production of organosilicon monomer methylchlorosilane by direct method, accounting for about 7%-8% of the output, the boiling range is 80-215 ° C, mainly some silane mixtures containing silicon-silicon bonds. The composition of high boilers is very complex, the market application is limited, and the industrial added value is very low. How to improve the industrial added value and market application of high boilers is an urgent problem to be solved in the silicone industry. At present, the treatment methods of high boiling substances are used as raw materials for the preparation of waterproofing agents, defoamers, acidic silicone resins, sili...

Claims

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Application Information

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IPC IPC(8): C07F7/12
Inventor 高俊杰胡庆超宋超徐晓光张懿
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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