SU642285A1 - Method of obtaining 1,1,1-trifluorine-2-chloropropane and 1,1,1-trifluorine-3-chloropropane - Google Patents

Description

Carrying out the process under the specified conditions allows 30Q-40 times.) The increase in the radioactive chemical yield of the target products in comparison with the known method. In addition to a sharp increase in the absolute yields of the target products, the selectivity of the process increases significantly: with an optimal molar ratio of DFT / HC1 of 1: 3, the ratio of yields L, b, i.e., is 3 times higher than the known method (| G / 1 1.5 ). Example 1, in a metal reactor made of nickel (

The dependence of the radiation-chemical yields of the target products and their ratio on the irradiation conditions in DFT-HC1 mixtures of different composition {irradiation temperature 30 ° C. dose rate, 33., 6 rad / s) 5 135 cm2, wall thickness b mm), equipped with a valve and a removable thermostatic jacket to remove heat generated during the reaction, are injected under pressure of 15-45 atm Hse and DFT with the known relation (see tab.) The mixture is irradiated at the gamma irradiation source (33.6 rad / s dose rate, irradiation time 2 hours, temperature. During the irradiation process, periodic sampling of the reaction products is carried out, which are analyzed chromatographically. The data obtained are in table 1. Table

As can be seen from the table below, 1, the radiation-chemical yield of the products is of an extreme nature, reaching a maximum at a ratio of DFT / HC: 3. The ratio of products II / 1 also varies depending on the composition from 5.1 to 2.7 by increasing the DFT / HC1 ratio from 1: 5 to 1: 0.33, respectively, Example 2,. In metal

 Dependence of target product yields on irradiation time and reactor material in gamma irradiation of a mixture of DFT / HC1 1; 3 (temperature, dose rate 33.6 rad / sf pressure 42 atm)

As can be seen from Table 2, the yield of target products depends on the material of the reactor and falls into a row of nickel, not stressful steel, titanium, Art.

The mixture of the desired products is separated (FROM the reaction mass by distillation at

The separation of 1 and II is carried out by distillation on a distillation column. The boiling points .1 and 11 are 30 + 0.5 ° C and 45 + b, 5 ° C, respectively.

Claims (1)

Data of elementary analysis of products I and II (the content is given in%): 5.1 92 5.3 90 4.6 91 4.982.7 4.169.5. A 2.733.4 reactor, as in Example 1, made of nickel, stainless steel, titanium, or St. 3, is introduced under a pressure of 42 atm HC1 and DFT with a ratio of TFP / HC1 of 1: 3. Irradiation and analysis of the reaction products is carried out as in Example 1. The results obtained, depending on the yields of the target products on the irradiation time and the material and the reactor, are listed in Table. 2, Table. 2 C26,22 H2.90 F43.95 C128.10 Gross formula C H F, C Formula of the invention. Method of obtaining 1,1,1-tr -2-chloropropane and 1,1,1-triflu propane by hydrochlorination 3.3 , 3-trifluoropropylene with hydrogen chloride at elevated pressure in the presence of gamma radiation as an initiator, characterized in that, in order to increase the radiation-chemical yield of the target products and to predominantly produce 1,1,1-trifluoro-chloropropane, the process is carried out under pressure 15 -45 atm and molar ratio of 3, 3,3-trif, torpropylene and hydrogen chloride 1: 3-5.