SU127256A1 - The method of separation of the fraction of direct synthesis of ethylchlorosilanes - Google Patents

Description

It is known that the production of EF-1, EF-3 and EF-5 electrically insulating varnishes is based on scarce ethyltrichlorosilance.

The proposed method for separating diethylchlorosilane and ethyltrichlorosilane contained in the direct synthesis fraction at a boiling point of 99-100 °, based on different component activities in the esterification reaction with butanol, allows to isolate the valuable product ethyltrichlorosilane and feedstock for the synthesis of organosilicon liquids - diethylchlorosilar.

Ethyltrichlorosilane reacts with the butanol Io scheme:

C2H:, SiCl3 + XC4H9OH C2H5Si (OC4H9) .vCl3, - XHCl. h) yes Kik diethylchlorosylai and this reaction almost takes part and can be distilled from the reaction mixture.

Example. Fraction, 59 :) chlorine (calculated: (C9H5) 251С1з-, (CvMrjlaSiCl-ly-lu) in an amount of 150 g is loaded into a flask with a stirrer and at a temperature of 20 78 g of isobutyl alcohol (1.5 mol lia 1 mole of ethyl trichloroyl chloride) are charged mixture). When the mixture is completed, it is gradually heated to the temperature of the Kпr perennial, after which it is cooled and discharged.

The resulting product (195 g) is loaded into the cube of a distillation head | columns with a height of 1.3 m with a winding of 3 mm porcelain rings (e: effective 20 theoretical plates). During the distillation in 1, 2 g of the cue fraction is taken up at a temperature of 99-100.

 and a l and s: Raechitano dl Received

Chlorine content in "29.0030.10

Hydrogen content

and flint in .S20,81

SiO content; . -19.0049.50.

(CoKOoSiHCl

By.: First Scenic Scalpus лll, Llsl Sufficiently Clean; Play, 1.l () RS11l} 1st.

In the experiments carried out with other ratios of epi x butgd oloma ethyltrnhlorsidan, according to the following results are obtained:

Output fr. 99-100

II, iO g INITIAL

mixtures

18, and

13.0

15.7

12.6

9.0

12.0

47

85

Thus, during the esterification of the fraction 99 ° with butanol i; the amount, 3-1,5 mol of mole of ethyl trichloroxylan, the main amount of chloroethyl chloride comes in and is returned 1; Once) onke mixture, while ethylchlorosilane is almost complete, about the reaction comes; esterification. The residue obtained from the mixture of diethylchlorosilane gives high-quality electrically insulating varnishes such as EF-3 and EF-5 when used instead of ethyltrichlorosine, dl hydrolysis the nerve stage of obtaining a varnish for the certificate of a mixture of wood / wood).

PRED. 1 ET and B about t t e n and

The method of separation of the ir fraction of the synthesis of ethylchlorosilanes with a boiling point hemi-temperature of 99-100 ° C, and so on; and with the fact that the fraction is treated with butanolol m, in an amount of 1.2-1.5 mol per 1 mol of ethyltrichlorosilane, then the mixture is dispersed with the release of diethylchlorosilane and products of partial esterification of 9thyltrichlorosilane.

chlorine in f

H ii to days 99-1100