DE729491C - Process for the production of hexachloroethane - Google Patents

Description

Process for the preparation of hexachloroethane It has already been proposed Ethyl chloride or ethylene chloride in the presence of animal charcoal at temperatures of To chlorinate Zoo up to 250 °, depending on the amount of chlorine used more highly chlorinated products. According to the proposal of the French patent specification 4-92175 -this process is said to be improved by working at temperatures works below 25o ° in the presence of activated charcoal, with an excess if necessary of chlorine can be used, but even here it only succeeds in a yield of 50% Hexachloroethane, for example from tetrachloroethane. To produce. It is also known to produce hexachloroethane from tetrachlorethylene by chlorination in the liquid phase, however, the work-up and purification of the hexachloroethane are considerable here Trouble.

It has now been found that hexachloroethane can be obtained in excellent yield and obtained free from by-products if one uses chlorine substitution products of Ethanes containing at least one free hydrogen atom, with a lot of chlorine, which exceeds the theoretically required for the formation of hexachloroethane, at temperatures between 25o and 300 ° above active charcoal, which is still with '- # 1_etallsalzen can be impregnated, conducts.

The main starting materials are i, i- and i, 2-dichloroethane, the various trichloro and tetrachloroethanes and also mixtures of these connections.

It is precisely these substances that can also contain unsaturated chlorine compounds with two Kolilenstoffatoinen; the amount of chlorine must then be measured in such a way that it is sufficient to saturate the double bond in these compounds. '# The resulting hexachloroethane si "e from the reaction gases can easily by A immediately bkühlen in solid and very pure form win. Low chlorinated ethanes, which are extremely difficult to separate from the hexachloroethane," ground is not formed. The applicable amount of chlorine is suitably between i , 2 and 2 mol per hydrogen atom of the starting materials. Larger amounts of chlorine can also be used, but this does not offer any special advantages.

Example i Through a quartz tube of 8oo mni length and d. mm clear width, which is charged with 1 l of activated charcoal, a mixture of 29 g of vaporous i, 2-dichloroethane with 124-chlorine is passed every hour at a contact temperature of -27o to 280 '. The vapors emerging from the tube are cooled to about 20 °, with pure hexachloroethane separating out in white crystals with a melting point of 184 to 185 °. The yield is practically qualitative. 87 "/, said hexachloroethane are obtained during cooling, while the remaining 137o are entrained by the fiberschüssigen chlorine gas. They can be @ -ewonnen by freezing as well.

If one conducts at the same temperature via "f'wn the same contact every hour A mixture of 30 g of gaseous i, 2-dichloroethylene finite 18 g of chlorine is so the yield also quai: ititative. By cooling @ .verden 82 ° 1o de Hexaclilorätlians deposited.

Example e At -2; o to -28o "hour 309 ines vaporous mixtures. from 9o parts of tetrachloroethane and io parts Pentacliloriitlian with -.og chlorine in a glass tube of 8no min length and do mm internal diameter than t 1 activated carbon passed is obtained in almost quantitative yield H. .exaclilorätlitin with a melting point of 18d '=.

Claims (1)

PATENT CLAIM: Process for the production of hexachloroethane by Chlorination of chlorine substitution products of ethane, the at least one free Hydrogen contained, in the gas phase in the presence of catalysts, thereby characterized in that at temperatures between 23o and 30o '= in the presence of more active hollow works with a quantity of chlorine, ie: that for the formation of 1dexaehlorätlian theoretically required.