SU742421A1 - Method of preparing 1,1,2-trichloroethane - Google Patents

Description

This invention relates to a process for the production of 1,1,2-trichloroethane and raw material in the production of vinylidene chloride. A known method of producing 1,1,2-trichloroethane (TCE) by hydrochlorinating a mixture of C1U- and trans-1,2-dichloroethylenes (DCE) in two successive stages in the presence of a catalyst - aluminum chloride, at a pressure of 15 atm and a temperature of 110 ° C LlJ The "drawback" of the process is the need to carry out the process in two stages, as well as the complexity of the technology due to the use of increased pressure. The purpose of the invention is to simplify the technology of this process. This is achieved by the method of producing 1,1,2-trichloroethane, consisting in that 1,2-dichporethylenes are hydrochlorinated at a temperature of 25-5 ° C in the presence of a catalyst - ferric chloride in the amount of 1-2.2 weight,% calculated on the the sum of the initial reagents and the solvent, the process is carried out in a solvent medium — mixtures of 1,1-dichloroethane and trichlorethylene, the molar ratio between which is from 1: 1 to 2: 1. In the practical implementation of the process, vinylidene chloride can be introduced into the reaction zone. In this case, the reaction products contain two isomers of trichloroethane; 1,1,1- and 1,1,2-trichloroethane. This method can be carried out with recycling of initial reagents, which practically do not enter into side reactions. The method was tested under laboratory conditions. Example 1. In a flask equipped with a stirrer, load 225 g of a solution containing 9.2 mol.% Trans-1,2-dichloroethylene, 8.3 mol% cis-1,2-dichloro lene and 2.22% anhydrous chlorine iron in a solvent consisting of two molar parts of 1,1-dichloroethane and one mole of trichlorethylene. The contents of the flask are heated to 25 ° C and at this temperature, with stirring, the flask is fed

Dry hydrogen chloride is used in excess of 20% of the stoichiometry 15. reactions after 6 hours. After the completion of the reaction, a sample is taken for anapiz, which is carried out by the method of haao-liquid chromatography.

The yield of 1.1.2 trichloro tan from theoretical is 41.4 mol Wo.

Example 2. The procedure for carrying out the experimental experiment is similar to Example 1. A solution containing a mole is used. % trans-1,2 dichloroethylene, 7.9 mol,% cns--1,2-dichloroethylene, 11 mol,%, vinylidene chloride (VD) and 1 wt.% ferric chloride in a solvent consisting of 1 molar portion of 1 D -dichloroethane and 1 molar part of trichlorethylene. The reaction time is 8 hours, the reaction temperature. As a result of the reaction, 1,1,2 trichloroethane and 1 DDD-trichloroethane are formed.

Bbtxoa isomeric trichloroethanes. 37.4 mol%.

The composition of the resulting product;

1D, 2 trichloroethane - 8O mole,%

1.1 D. trichloroethane - 20 mol.%.

Example 3 Reaction conditions are the same as Example 2, except for the reaction temperature, which is 50 ° C and the concentration of ferric chloride is 2% by weight,

The yield of isomeric trichloroethanes 44.2 mol.,%;

The composition of the product being taught;

1,1,2-trichloroethane - 50 mol%

1D, 1 trichloroethane - 50 mol.%.

The proposed method does not require the promotion of high pressure, with the result that it is characterized by lower capital costs, it is simpler in terms of technology and hardware design. The method can be used for the processing of secondary fractions of vinylideichloride production, which, along with 1,2 g Dichloroethylene, contain 1,1-dichloroethyl NI trichlorate, which is the solvent that provides the process.

Claims (1)

1. The patent of Germany 939324, cl. 12О, 2 / О1, published. 1961,