A method of obtaining a polyfluorinated atanov

 

(57) Abstract:

Usage: polyfluorinated atany as refrigerants, foaming agents. The synthesis conditions: reagent 1-ethylene, reagent 2-cobalt TRIFLUORIDE. The synthesis conditions first TRIFLUORIDE With take into serpents with TRIFLUORIDE Mn in the ratio of 1 0,6 4 at 120 to 220°C, contact time 600 1500, then the resulting reaction mass is subjected to interaction with TRIFLUORIDE From 50 to 270°C. for 3 h.p. f-crystals, 1 table.

The invention relates to the technology of polyfluorinated Atanov: 1,1,1 - and 1,1,2-triptoreline, 1,1,2,2 - and 1,1,1,2-tetrafluorethane and Pentafluoroethane by fluorination of ethylene higher fluorides of metals of variable valence.

These polyfluorinated atany belonging to the group of halocarbons, have zero potential decomposition of the ozone layer compared to chloroformmethanol (freon 11 and 12) and are promising substitutes OzonAction halocarbons, 1,1,2-trifluoroethane (CR-143) is used as the refrigerant; 1,1,1,2-Tetrafluoroethane (CHL-134a) is used as the refrigerant in the installations of air conditioning and as a blowing agent for some types of plastics; 1,1,2,2-Tetrafluoroethane (CHL-C) can serve as a refrigerant and as a raw material in organic synthesis;asianam by fluorination of chlorine - or harversters of Atanov or etileno hydrogen fluoride [1-6] and CR-125 can be obtained by catalytic hydrogenation of CHLOROPENTAFLUOROETHANE [7] and fluoridation diftoretilena elemental fluorine [8] there are also Known methods of obtaining holdem-134 and CHL-125 by fluorination with cobalt TRIFLUORIDE-holdem-143 and CHL-134 respectively [9] In these methods is used, as a rule, expensive raw materials, and the target products often have a large number of side connections, sometimes very toxic.

Known also adopted for the prototype method of obtaining polyfluorinated Atanov by fluorination of ethylene F3[10] consists in the following:

In a horizontal reactor with a stirrer, filled F3and heated to 115aboutWith serves ethylene with a speed of 7 l/h At the end of the process the reactor is rinsed with nitrogen, gases from synthesis remove HF, passing them over heated to 80aboutWith sodium fluoride and fractionary the mixture of floridanew.

The authors of this paper studied the mechanism of fluorination of ethane and ethylene F4and F3and came to the conclusion that the method is of no practical value for industrial use because of the low selectivity with respect to any formed toratenu. At the same time on the basis of the reaction of fluorination of ethylene F3in which in addition to floridanew is formed only HF, it is theoretically possible to develop a zero waste industrial technology if possible to achieve the maximum possible yield of the target product at a relatively low temperature process that is acceptable is possible these requirements it is necessary to solve the main technical problem, limiting the entire process to develop an effective method of heat of reaction.

This task is solved as follows: as in the method prototype as the original product ethylene take, but fluoridation it is carried out in two stages: in the first mixture F3and nF3taken in the ratio of 1:0.6 to 4 at a temperature of 120-220aboutWith time and contact 600-1500 from the obtained reaction mixture, consisting mainly of CR-143 (70%) is subjected to further fluoridation, but only F3when 50-270aboutC. Varying the temperature of the second stage within the specified limits, can be obtained with a yield not less than 65% of any of the following refrigerants: 143, 125 mixture s and 134a.

When 50-80aboutWith a predominant product is CR-143, at 150-180aboutWith CR-134, 190-270aboutWITH CR-125.

Using the same mixture of higher fluorides of metals of variable valence with different oxidation potentials provides the starting period of the soft conditions, as with the use of a diluent. When the content F3above is allocated a significant amount of heat and the process is out of control, higher contents nF3requires a high temperature that the economic is the composition of the mixture at stage I and the lower output of the target product. This result leads and shorter than 6000 with contact time. More prolonged exposure leads to unnecessary energy expenses.

P R I m e R s: the Experiments were carried out in a Nickel reactor with a diameter of 76 mm and a length of 1000 mm, filled with a mixture F3and nF3the total mass of 5 kg In the reactor was submitted to 39.6 g of ethylene, and the resulting synthesis gases were sent to the second stage in the same reactor, containing 5 kg F3. Upon completion of the reaction products were collected in a cold trap and analyzed by GLC. The target products were isolated by distillation. The process parameters and the results of the experiments presented in the table.

From the presented experimental data suggests that, while compliance with a specified set of features is achieved technical result consists in creating in the first reaction zone conditions, allowing to obtain the desired product with a yield not less than 60% in Addition this method yields up to 40% can be obtained 1,1,2,2-Tetrafluoroethane, practical methods of obtaining of which is unknown. Toratani not contain toxic impurities, and resulting from the reaction of hydrogen fluoride can also be used as a ready probortona, including fluorination of ethylene with cobalt TRIFLUORIDE at elevated temperature, characterized in that the first cobalt TRIFLUORIDE take in a mixture with manganese TRIFLUORIDE in the ratio 1:(0,6-4,0) and the process is conducted at 120-220oWith time and contact 600-1500, then the resulting reaction mass is subjected to interaction with cobalt TRIFLUORIDE at 50-270oC.

2. The method according to p. 1, characterized in that in the case of triptorelin interaction of the reaction mixture with cobalt TRIFLUORIDE is carried out at 50-80oC.

3. The method according to p. 1, characterized in that in the case of Tetrafluoroethane interaction of the reaction mixture with cobalt TRIFLUORIDE is carried out at 150-180oC.

4. The method according to p. 1, characterized in that in the case of Pentafluoroethane interaction of the reaction mixture with cobalt TRIFLUORIDE is carried out at 190-270oC.

 

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FIELD: industrial organic synthesis.

SUBSTANCE: invention is dealing with production of chlorohydrocarbons exhibiting plasticizing properties in polymer compositions in production of synthetic building materials, varnishes and paints, artificial films and leathers, in rubber industry, and as fire-retardant additives in polymers. Process comprises chlorination of waste obtained in production of C14-C32 fraction by ethylene-α-olefin oligomerization. Chlorination is accomplished in two steps: addition chlorination at 35-55°C followed by substitution chlorination at 40-105°C. Chlorohydrocarbons thus obtained can, in particular, be used as secondary plasticizer in polyvinylchloride compositions.

EFFECT: reduced expenses due to using production waste.

4 tbl, 30 ex

FIELD: petrochemical and industrial organic synthesis.

SUBSTANCE: process comprises separating gaseous pyrolysis products to recover ethylene-containing fraction with 54-65% ethylene content and C3-C5-hydrocarbon fraction. Ethylene-containing fraction is subjected to liquid-phase catalytic chlorination. Gas phase of chlorination product is purified via adsorption and fed into furnace as fuel. C3-C5-Hydrocarbon fraction is subjected to exhaustive hydrogenation, hydrogenation product is combined with fresh raw material at weight ratio (0.05ч1):1 and sent to pyrolysis plant.

EFFECT: achieved integration of process, increased reliability thereof, and reduced expenses.

1 dwg, 1 tbl, 15 ex

FIELD: organic chemistry.

SUBSTANCE: 1,2-dichloroethane is obtained by liquid phase ethylene chlorination with discharging of reaction heat due to operation medium boiling. In claimed process nitrogen is added to chlorine and ethylene reagents. Ratio of chlorine volume consumption to nitrogen volume consumption is maintained as 1:1. Reaction is carried out at temperature lower than 1,2-dichloroethane boiling point, and discharging of reaction heat is carried out by evaporative cooling of operation medium in nitrogen.

EFFECT: process of increased selectivity; decreased yield of by-products.

1 tbl, 5 dwg

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