SU1599360A1 - Method of producing 1,2,3-trichloropropylene - Google Patents

Abstract

The invention relates to chlorohydrocarbons, in particular to the preparation of 1,2,3-trichloropropene intermediate in the preparation of triallate herbicide. The goal is to increase the yield of the target product. The preparation is carried out by chlorination of 2,3-dichloropropene with chlorine in the liquid phase in the presence of phenol or ortho-chlorophenol, or 2,6-dichlorophenol, taken in an amount of 2-3 wt.% From the starting 2,3-dichloropropene, at 20-50 ° WITH. Preferably, phenol (1 wt.% Of the starting 2,3-dichloropropene) is added to the reaction mass every 10 minutes and chlorination is carried out until the conversion of 2,3-dichloropropene is reached 84-85%, after which the desired product is isolated by distillation. When the conversion of 2,3-dichloropropene is reached, 22.4-28.6% also isolates the target product by distillation, and the unreacted 2,3-dichloropropene is returned to the chlorination stage. The yield is 72.4%, i.e. 14.5 - 26.6% higher than in the known method. 2 hp ff, 2 tab.

Description

The invention relates to chloro-glucose. hydrogen, in particular, to methods for producing 1,2,3-trichloropropene (THP) - intermediate in the preparation of triallate herbicide.

The purpose of the invention is to increase the distribution of the target product.

Example 1. The process is carried out in a glass-type tempered temperature controlled reactor at 20fc. 42 g of 2,3-dichloropropene (DHP) and 0.84 g (2 May. 7) of phenol are placed in the reactor. 21.3 g of chlorine are supplied over 1 hour. 60.41 g of chloroformal mass are obtained with a content of 54% (conversion of 22.4%), a TCP of 30.9%, the rest is chlorophenols and tetrachlorhydropane. Chlormass is subjected to rectification and 17.7 g of TCP and 31.4 g of DHP are isolated. Unreacted DHP is returned to the reactor and used again to obtain PTS.

Similarly lead the process in examples 2-7. The conditions and results of the experiments are presented in table 1,

Example 8. The process will proceed as in Example 1, but the initial loading of DHP is 60 g, phenol - 1.8 g (3 wt.%). The process is carried out for 3 h, adding every 10 min, 1 wt.% (0.6 g) of phenol. Chlorine consumption 99.4 g. The process is conducted on the conversion of DHP 64%. Received 80 g of TCL.

SP

WITH

with

3159

output per reacted

DHP 72.4%,.

I Similarly lead the process in example 9-13.

Conditions and results of experiments are presented in table. 2

From tab. 1 and 2, it can be seen that the yield of TCP in the proposed method is 14.5- 26 6% higher, than in the well-known. Comparative examples 2-7 and 11-13 show

expediency of the process

 outside the selected intervals

i conditions.

Claims (3)

1. A method of producing 1,2,3-trichloropropene by chlorinating 2,3-dichloropropene with chlorine in the liquid phase with subsequent introduction of the target product, which is different because, in order to increase the yield, it is targeted: product, the process is carried out in the presence of phenol or ortho-chlorophenol, or 2,6-dichlorofanol, taken in an amount of 2-3 wt.% from the starting 2,3-dichloropropene, at 20-50 C. 2. The method according to claim 1, wherein the process is carried out until the conversion of 2,3-dichloropropena reaches 22.4-28.6%, after which the desired product is isolated by distillation and unreacted 2,3-dichloropropene is returned to the chlorination stage. 3. The method according to p, 1, o tl and h and y and with the fact that phenol is additionally added to the reaction mass every 10 min in an amount of 1 wt.% from the starting 2,3-dichloropropene and chlorination is carried out until reaching a conversion of 2,3-dichloropropene 84-85%, after which the target product is recovered with rectificadium. Table Ta bl and c a