SU658122A1 - Method of obtaining carbon tetrachloride - Google Patents

Description

(54) METHOD FOR OBTAINING FOUR-CHLORINE CARBON

chlorine. In this case, an occluded chlorine anion remains in the catalyst cell.

I

. PRI me R. 50 g of zeolite CaX are treated with a solution of 4 g of CaCig in 80 ml of distilled water. After drying, the catalyst is loaded into the furnace and calcined for 12 hours at a current of air. The cooled catalyst is washed with boiling distilled water until chlorine ions are absent.

The process is carried out as follows. Chlorine gas from a cylinder through a drying tank with a concentrated monostat, a flutometer enters the reactor. Air through a monostat, a flutometer, a drying column enters the liquid feed evaporator and then goes to the reactor. Liquid feed - chlorine-containing propane compounds using a mechanical syringe dispenser at a rate of 2.8 g / hour enters the evaporator and then vapor-gas mixture of chlorine-containing propane compounds and air enters reactor. Mixing the steam-gas mixture with chlorine occurs directly in

fluidized bed

layer

catalyst. The reaction products from the reactor enter refrigerators, cooled with dry ice to a temperature. Noncondensed gases through the vial with a short circuit enter the gas meter and further into the atmosphere. The reaction products for the content of chlorohydrocarbons are analyzed by chromatography.

The chlorine content in the reaction products is determined by iodometry. The content of hydrogen chloride in the reaction products is determined by acidometry. Carbon tetrachloride was isolated from the reaction products by a clear distillation method. Studies are conducted in the temperature range of 250-450s and the ratio of chlorine-containing propane: chlorine 1: 1g5, contact time from 2 to 8 seconds.

The optimal process conditions are: temperature 375 ° C, molar ratio chlorine-containing propane compounds: chlorine 1: 1.2, chlorine-containing propane compounds: oxygen 1: 2.3, contact time 4.1 sec.

The material balances of the process of oxidative chlorination of chlorine-containing propane compounds on the developed catalytic system are presented in Table. 1-4.

Table.

2.8 24.4 - --1, 8 15.6 0.2 1.80.76.1

1.6 14.0 0.5 4.40.97.9

5.3 46.0 5.3 46.05 3546.0

- - - -0,32,6

82.6 56.8

3.8 33,02,521,7

0.3 2.60.32.6

0.2 1.70.10.9

0.43.5

0.5 4,40,32,6

Carbon monoxide Carbon dioxide Compaction products Notes

1,2,3-trichloropro note.

Continued tabl,

0.1 0.9 O, 1 0.9 0.3 2.6 0.3 2.6

0.3 2.6 0.3 2.6

11.5

100

100

11.5 11.5 100 11.5 100 11.5 100 e. Process parameters: temperature 37500, molar ratio of chlorine derivatives of propane: chlorine 1: 1.2, chlorine derivatives of propane; oxygen 1: 2.3, contact time 4.1 seconds, the duration of the experiment 1 hour. Process parameters: temperature, molar ratio of the chlorine derivatives of the propane compounds: chlorine 1: 1.2, the chlorine derivatives of the compounds: oxygen 1: 2.3, contact time 4.1 seconds, duration of the experiment 1 hour. Table 2.

Chlorine derivatives of propane

Chlorine

Air oxygen

Nitrogen

Four Chloride Carbon Notes

T a b e c ia 3.

24.4 15.6 14.0

46.0 46.0 5.3

3.2 27.9

71.2

100 11.5

100

11.5

T of the bar. 4. e: Process parameters: temperature 450 ° C, molar composition of chlorine derivatives Propane compounds: chlorine 1: 1.2, chlorine derivatives of propane compounds: oxygen): 2.3, contact time 4.1 seconds duration 1 hour, Note.

Claims (2)

1. Author's certificate of the USSR 303658, cl. C 07 S 19/06, 1967. 2. USSR author's certificate as per application 1724387/23-04, C 07 C 19/06, 09.12.71. Process parameters: temperature 375 ° C, molar ratio chlorine-made compounds of propane: chlorine 1: 1, chlorine derivatives of compounds of propane: oxygen 1: 2.3, contact time 4.1 seconds, experiment duration 1 hour.