SU166025A1 - METHOD OF OBTAINING ALKYL- AND ARYLSILANE CHLORIDES - Google Patents

Description

A known method for producing alkyl and arylsilane chlorides by reacting a silica – contact mass with chloride alkyls or aryls with stirring.

According to the proposed method, in order to increase the productivity and yield of the target product, the mass is stirred by passing a jet of alkyl chloride or aryl at a speed of 1-20 cm / sec. The process is conducted in a fluidized bed. In this case, the contact mass is crushed to a particle size of 0.02-0.25 mm.

Example 1. In a reaction apparatus, which is a glass tube with a diameter of 20 mm and a height of 200 mm, equipped with electrical heating, 40 g of a silicon-copper alloy 100-250 microns in size (70% silicon) are loaded. After drying the alloy (at 280 ° C in a stream of nitrogen) at a temperature of 320 ° C, chloroethyl begins to be supplied at a rate of 65 l / h. The reaction product collected during 4 hours, after the distillation of chloroethyl, is loaded into a distillation column with a height of 450 mm and a diameter of 12 mm, equipped with 2-3-turn nichrome spirals with a diameter of 2 mm.

From 106.8 g of the loaded product receive:

Fractions 95-102

9.8

8.1 (50% chlorine) 102-125 23.9 (45.2% chlorine) 125-132

VAT residue 14.6

Loss of 25

Based on the above data, the following indicators can be calculated (taking losses during rectification as chloroethyl): Contact mass capacity (ethyl silane chloride mixture - weight), g / kg h

510

Capacity, g / l of reaction volume per hour 320 Yield of ethyl silane chloride mixture,% by weight of silicon in contact mass 293

The content of diethylsilane

in a mixture of ethylsilane chloride,% 36.8

Example 2. The process of producing ethylsilane chlorides was reproduced in a steel apparatus with a diameter of 50 mm and a height of 400 mm with electrical heating. 612 g of a silica-silica powder (see Example 1) are loaded into the apparatus. After drying (in a stream of nitrogen at 280 ° C) at a temperature of 300 ° C, chloroethyl begins to be supplied at a rate of 180 l / h.

Over the next 2 hours and 30 minutes, 1,830 g of chloroethyl are passed through and 973 g of chloroethyl and 405 g of a mixture of ethylsilane chlorides are obtained.

When rectification of the first half of the condensate (ethylsilane chlorides plus residual chloroethyl), from 436 g of the product you get:

Weight, g

Fractions, ° C

up to 20 (chloroethyl) 160

20-7551

75-9545

95-10226

102-12580 (49.9% chlorine)

125-13246 (45,204 chloro)

VAT residue22

Loss6

When rectification of the second half of the condensate from 791 g of the product is obtained:

Fractions, ° CW, g

up to 20 (chloroethyl) 380

105

20-75 68 34

75-95

95-102

100 (50% chlorine)

102-125 70 (45.3% chlorine)

29 5

kill the wounded

The calculation shows that in the experiment the following

1 half (3 hours)

The performance of the contact mass in g of a mixture of ethylsilane chlorides with 1 kg of mass in

 an hour ... 147

Performance mass in g of the mixture with 1 liter of reaction volume. . . 18

The content of diethyldichlorosilane in a mixture of ethylsilane chloride,% ... 39,4

36

The table presents the results obtained when conducting experiments on this device.

 Low output due to partial loading of the device.

Subject invention

Claims (2)

1. A method for producing alkyl- and arylsilane chlorides by reacting silica-silica contact mass with chloride alkyls or aryls with stirring, characterized in that, in order to increase productivity and yield of the target product, the mass is mixed by directing the jet of alkyl chloride or aryl at a rate of 1- 20 cm / sec and the process is carried out in a fluidized bed. 2. A method according to claim I, characterized in that the contact mass is ground to a particle size of 0.02-0.25 mm.