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Method for chlorinating methyl phenyl dichloro-silane

A technology of methylphenyldichlorosilane and catalyst is applied in the fields of high resistance, grease, chlorination of organosilicon monomers, and low temperature lubricating oil, and achieves the effects of high yield, no environmental pollution and good lubricity.

Inactive Publication Date: 2012-09-12
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no related technology reported in the literature at home and abroad for the chlorination of methylphenyldichlorosilane.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] With stirring, reflux condensation, thermometer, Cl 2 Add 64 mL of methylphenyldichlorosilane to the 100 mL four-necked flask of the introduction tube device, add anhydrous ferric chloride catalyst, the dosage is 0.1% of the total mass of methylphenyldichlorosilane, stir to disperse uniform. The reaction temperature was 80 °C, and nitrogen was introduced into the system to replace the air, and then Cl 2 (dried over concentrated sulfuric acid) for the reaction, Cl 2 The flow rate is 10 mL / min. Exhaust gas through CCl 4 , After the lye is absorbed, it is ventilated to the atmosphere. After 10 h of reaction, samples were taken to analyze the product composition by gas chromatography.

[0024] Repeat the above steps but change the anhydrous FeCl 3 The amount used is 0.1%, 0.05%, 0.01%, and 0.005% of the total mass of methylphenyldichlorosilane. See Table 1 for product analysis.

[0025] Table 1: Effect of Catalyst Amount

[0026] Anhydrous FeCl 3 Dosage ...

Embodiment 2

[0030] With stirring, reflux condensation, thermometer, Cl 2 Add 64 mL of methylphenyldichlorosilane to the 100 mL four-necked flask of the introduction tube device, add anhydrous ferric chloride catalyst, the dosage is 0.1% of the total mass of methylphenyldichlorosilane, stir to disperse uniform. The reaction temperature was 80 °C, and nitrogen was introduced into the system to replace the air, and then Cl 2 (dried over concentrated sulfuric acid) for the reaction, Cl 2 The flow rate is 10 mL / min. Exhaust gas through CCl 4 , After the lye is absorbed, it is ventilated to the atmosphere. After 10 h of reaction, samples were taken to analyze the product composition by gas chromatography.

[0031] Repeat the above steps, but change the reaction temperature to 20 °C, 50 °C, and 100 °C. The analysis of the product results is shown in Table 2.

[0032] Table 2: Effect of Reaction Temperature

[0033] temperature reflex MePhSiCl 2 Conversion rate Total yield o...

Embodiment 3

[0036] With stirring, reflux condensation, thermometer, Cl 2 Add 64 mL of methylphenyldichlorosilane to the 100 mL four-necked flask of the introduction tube device, add anhydrous ferric chloride catalyst, the dosage is 0.1% of the total mass of methylphenyldichlorosilane, stir to disperse uniform. The reaction temperature was 80 °C, and nitrogen was introduced into the system to replace the air, and then Cl 2 (dried over concentrated sulfuric acid) for the reaction, Cl 2 The flow rate is 10 mL / min. Exhaust gas through CCl 4 , After the lye is absorbed, it is ventilated to the atmosphere. After 10 h of reaction, samples were taken to analyze the product composition by gas chromatography.

[0037] Repeat the above steps, but change the reaction time to 6 h, 15 h, and 20 h. The product analysis results are shown in Table 3.

[0038] Table 3: Effect of Reaction Time

[0039] Reaction time MePhSiCl 2 Conversion rate Total yield of chlorobenzenes MeClPhSiCl ...

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Abstract

The invention relates to a method for chlorinating methyl phenyl dichloro-silane, belongs to the technical field of organosilicon monomer chlorinating and particularly relates to a method utilizing anhydrous FeCl3 serving as a catalyst and Cl2 serving as a chlorinating agent to catalyze and chloridize methyl phenyl dichloro-silane to prepare methyl polychlorinated phenyl dichloro-silane. According to the method, gas-liquid continuous reactions are adopted, reaction process flows are simple, reaction conditions are mild, the reactions are easy to control, conversion rate of a raw material is high, and the yield of a product is good. When the using quantity of the catalyst is 0.1% of the total mass of the raw material, the flow of Cl2 is 10mL / min, the reaction temperature is 80 DEG C and the reaction time is 10h, the conversion rate of methyl phenyl dichloro-silane is 99.82%, and the yield of methyl polychlorinated phenyl dichloro-silane is 87.28%. Methyl polychlorinated phenyl dichloro-silane prepared by the method has no obvious breakage of Si-C bond, and the main products are a methyl monochloro product.

Description

technical field [0001] The invention relates to a method for chlorination of methylphenyldichlorosilane, which belongs to the technical field of organosilicon monomer chlorination, and also belongs to the technical field of high- and low-temperature-resistant lubricating oil and grease. [0002] Background technique [0003] At present, aviation lubricants are mainly synthetic ester oils, supplemented by petroleum base oils. Petroleum base oils are only used in old models, while ester aviation lubricants have been widely used in civil aviation and military aircraft at home and abroad. . [0004] With the continuous development of modern science and technology and the continuous improvement of the thrust-to-weight ratio of aero-engines, the requirements for high-temperature use of aviation lubricating oils are getting higher and higher. The key to the level of development of aviation lubricants lies in the level of high-temperature service temperature. In the early 1980s, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/12C10M105/76
Inventor 姜逸倩殷恒波柳艳君付玉军颜晓波
Owner JIANGSU UNIV
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