The method of producing hexachlorethane

 

(57) Abstract:

The invention relates to the production of hexachlorethane, which is used in the production of halon 113, tablets for degassing at low tide aluminum parts, upon receipt of deodorants, antibacterial drugs and smoke mixtures. The method is carried out by adding CCL4to the powdered aluminum in an argon atmosphere. Aluminum pre-activated with iodine. The molar ratio of aluminum: CCL4= 1: 8. The process is conducted at atmospheric pressure, at a temperature of 45oC for 30 minutes Technical result is an increase in the yield of the target product, waste is reduced.

The invention relates to the field of organic chemistry, in particular to a method of obtaining hexachlorethane

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which can find application in the production of halon 113, tablets for degassing at low tide aluminum parts, upon receipt of deodorants, antibacterial drugs, as well as for obtaining smoke mixtures.

In industry hexachlorethane produced by chlorination of 1,2-dichloroethane over activated carbon, which serves as a catalyst. (Industrial organochlorine products. Edited Osina L. A., Chemistry. 1978. 195[1]). with chlorine, then the mixture is directed into the tubular reactor, heated to has reached 270-290oWith and filled with activated charcoal AG-3. Chlorine is usually served in 30% excess relative to 1,2-dichloroethane. The reaction produces a complex mixture of chlorinated compounds: Hcl, trichloroethane, tetrachloroethylene, tetrachlorethane, Hexachlorobutadiene and hexachloroethane. The output of hexachlorethane is 17%.

CH2Cl-CH2Cl+CL2-->CCL3-CCl3+HCl+l= l2+CCl2= CCl2+CCl2= CCl CCL= CCL2< / BR>
The disadvantages of this method of synthesis of hexachlorethane are:

1. Low output hexachlorethane - 17%.

2. The use of gaseous chlorine, which requires the use of expensive corrosion-resistant equipment. In addition, it requires special technology unit (tanks, piping, instrumentation, pumps, protective area) for storing, dispensing, and disposal of chlorine and chlorine-containing waste.

3. High temperature reactions (has reached 270-290oC) and the associated high costs of energy.

4. Low selectivity of the reaction, the formation of side trudnoreshaemyh products.

Known IU Islandia organochlorine products. Edited Osina L. A., Chemistry. 1978, 196 [2]). With this method in optimal conditions (100-110oC, 4 h, the molar ratio ([C2CL4]:[Fl3]=100: 1) output hexachlorethane is 40-45%.

CCl2=CCl2+CL2-->CCL3CCl3< / BR>
The method has the following disadvantages.

1. Low output hexachlorethane (40-45%).

2. Use as reagent mycotoxins and environmentally hazardous chlorine.

3. The complexity of the hardware design process, because for the storage, dispensing and disposal of chlorine requires special manufacturing equipment from corrosion-resistant materials.

It should be noted that hexachloroethane was first obtained from chetyrehhloristy carbon, passing vapors through a glass tube heated to 500o(W. Kolbe // Lieb. Ann. Century 54, S. 14 [3]). Decomposition CCl4proceeds selectivity and results (along with hexachlorethane) chlorine, dichloroacetylene and unidentified products.

Regularities of thermal decomposition CCL4were investigated in later writings (A. E. Shilov, R. D. Sabirov, " DOKL. Ser. physical chem., 1957, T. 114, 5, S. 1058[4]; A. E. Shilov, R. D. Sabirov // Ser. physical chem., Hamartomas the collapse of the CCl4in the temperature range from 227 to C accompanied by the formation of chloride, tetrachloroethylene, and hexachlorethane, the output of which does not exceed 1.7%.

CCl4-->CCL3-CCl3+CCl2=CCl2+Cl2< / BR>
On the composition of thermal decomposition of CCl4significantly influenced by the material of the reactor. So, Korshak centuries with staff investigated the decomposition of CCl4in a porcelain tube heated to 400-700oAnd found that the main reaction product is tetrachlorethylene, and hexachlorethane is formed in the amount of ~10%, and the maximum conversion CCl4not exceed 52% (Century. Century. Korshak, Y. A. StepAhead, L. F. Bertoletova // AH, 1947, 17, c. 1626[7]).

Method of obtaining hexachlorethane by thermal decomposition has the following disadvantages.

1. Decomposition CCl4with a noticeable speed occurs at elevated temperatures (400-700oC) therefore, the necessary high energy costs.

2. The decomposition of CCl4passes selectivity and leads to the formation of a mixture trudnoreshaemyh products.

3. The low yield of the target product.

The closest in technical essence to this method is a method of gaining the glia 790896, 19.02.1958].

The essence of this method lies in the fact that in the corresponding reactor with a stirrer placed 27 parts of aluminum. Then add 150 parts of diethylaluminium, start stirring and heated to 150oC for 1 h then the reaction vessel was placed 1000 parts of heptane. The reactor is heated to boiling, approximately 95oC. In boiling the reaction mixture for 2 h add 460 parts of carbon tetrachloride. After completion of the reaction, the reactor is cooled, the reaction mixture was hydrolized with hydrochloric acid. Received GHA filtered.

This method has a serious drawback: the use elyuminirovanie, which significantly complicates the technological process.

We propose a method of obtaining hexachlorethane of carbon tetrachloride, free from the above disadvantages.

The essence of the method consists in obtaining hexachlorethane from CCL4under the action of aluminum powder activated with iodine, taken in a molar ratio Al: CCl4=1:8. Activation occurs as follows. The addition of aluminum, is placed in a reactor, add a few crystals of iodine and under argon negrohernan pressure, gradually add the CCl4. The reaction time is about 30 minutes

The reaction proceeds according to the scheme:

6Cl4+2l-->2ll3+3C2CL6< / BR>
Excess CCl4this reaction is necessary in order to reduce the amount of by-products that may result from engaging in the reaction hexachlorethane.

Output defined chromatographic method internal standard is 99%. As a side product observed Hexachlorobutadiene in the amount of 0.6%.

The proposed method has the following advantages/

1. High yield of the target product.

2. The availability of source reagents.

3. The formation of small quantities of waste. Unreacted excess CCl4it is easy to return a simple distillation and reused in the reaction. ll3formed in the reaction, can be used as catalysts in other processes.

4. Does not require high temperature and pressure increase.

5. The absence of such toxic and environmentally dangerous component as chlorine.

6. Reduce the cost and simplify technology for reducing energy and labor costs, Ekologicheskie CLASS="ptx2">

In a glass reactor with a volume of 50 ml is placed 0.32 g (to 11.8 mmol) of powdered Al and a few crystals of iodine. In an argon atmosphere rector heated with a spirit lamp until fully sublimation of iodine. The reactor set on a magnetic stirrer, add 10 ml (97,3 mmol) CCl4. Periodically including a stirrer, conduct stirring the reaction mixture for 30 min at a temperature of 45oC. Upon completion of the reaction, the reaction mixture becomes brown in color. The reaction mixture was hydrolized with water, then separate the organic layer and put it through Al2ABOUT3then it evaporated to dryness. Double recrystallization from ethanol obtain 2.9 g of white crystalline powder (hexachloroethane), representing 81.3% of theoretical yield.

IR spectrum (cm-1): 760

Elemental analysis (in parentheses are theoretical content):= To 10.62 (10,13)%:CL=88,9(89,87)%

An NMR spectrum13With (, m D.): 105,15.

The method of producing hexachlorethane of carbon tetrachloride, wherein the powdered aluminum, pre-activated with iodine, add CCL4in a molar ratio of 1:8 in argon atmosphere, at atmospheric pressure, at a temperature of 45C during the course

 

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