The method of producing pentafluoroethane
(57) Abstract:The invention relates to organic chemistry, in particular to a method of obtaining Pentafluoroethane, which is used in the reactions telomerization and as raw material for the preparation of many organic compounds. The proposed method is the interaction of tetrafluoroethylene with a mixture of iodine, iodine PENTAFLUORIDE at a temperature of 40 - 80oWith the presence of metallic antimony as a catalyst and in the presence of additives mixture of deformity with triptorelin in number 710-4-2,610-2wt.%. The result is increased productivity of the process, exclude the use of inert diluent, reduced the price process becomes less dangerous, it is possible to obtain a finished product with a high content of basic substance, thereby eliminating stage further purification. This invention relates to the field of organic chemistry, in particular the production of godforsaken used in the reactions telomerization for the production of low molecular weight polymers and as raw material for the preparation of many organic compounds (including fluorinated surfactants).Describes a method for pentatomidae the catalyst - PENTAFLUORIDE antimony or a mixture of antimony TRIFLUORIDE and iodine [U.S. Pat. USA N 3283020 from 01.01.1996].Significant disadvantages of this method are the need to prior 1,2-deuteration, which leads to complication of the process; mandatory compliance with a specific ratio of reacting components, otherwise the reaction will proceed with the formation of longer carbon chain.Previously published method of producing Pentafluoroethane reaction of tetrafluoroethylene with monitoriza iodine in the presence of aluminum metal as a catalyst and in the presence of inhibitor (1,1,2-trichloro-2,2-diphtheriatetanus) [U.S. Pat. USA N 3006973 on October 31, 1961].The disadvantages of the method are low output Pentafluoroethane (59% in terms of amount of tetrafluoroethylene), the mandatory use of the inhibitor in the absence of which the main reaction products were terraformer and carbon.The closest in technical essence and essential features is the method of receiving odporucane reaction mixture farolatino with the inert gas with a solution of iodine and trioxide of antimony PENTAFLUORIDE in iodine at a temperature of 40 - 80Oska performance; the use of inert gas as a transporting agent in the synthesis of Pentafluoroethane that it is not possible to obtain the target product of high purity due to the presence of non-condensable impurities (inert gases). The raw contains no higher than 94% of Pentafluoroethane, as impurities contains tetrafluoroethylene 5.2%, freon-0.6%, pentaverate of 0.2%. Raw should be subjected to rectification, therefore, the process is complicated by the stage of purification.Use as inert nitrogen gas requires additional purification from oxygen to ensure the safe conduct of the process. Additional purification of nitrogen from oxygen, and an inert gas is expensive helium increase the cost of the process.As the catalyst used toxic antimony trioxide. The presence of acidic components (iodine, iodine PENTAFLUORIDE) capable of causing polymerization of tetrafluoroethylene, which can lead to uncontrolled reactions, ending with a Bang.The task of the invention is to develop a method of producing Pentafluoroethane without the above disadvantages.The problem is solved by the method of Metallichesky antimony as a catalyst and in the presence of additives mixture of deformity with triptorelin of 7 to 10-4- 2,6 10-2wt.% as inhibitors of spontaneous polymerization of tetrafluoroethylene. With the introduction of the mixture of deformity with triptorelin fewer than 7 of 10-4wt. % is observed the formation of polytetrafluoroethylene, which complicates the process, makes it more dangerous and reduces the efficiency of the process. The use of these additives in excess of 2.6 10-2wt.%, leads to deterioration of the composition of the raw, the decrease in the content of the basic substance in the resulting product.The process is conducted at a temperature of 40 - 80oC.The advantages of the proposed method are improving the performance of the process; the process without the use of an inert diluent, which reduces the process and make it less dangerous.As the catalyst, the proposed method uses a metal antimony is less toxic than antimony trioxide. The presence of additives: deformity and triptorelin stabilizes the process, except for the spontaneous polymerization of tetrafluoroethylene.The invention is illustrated by the following examples.Example 1.In the reactor of stainless steel with a capacity of 1 l, snobunny the 30 g of metallic antimony. The molar ratio of the initial reagents 1:1,25:0,24. Heated reactor to 60oC and gave tetrafluoroethylene with addition of 1.6 10-2wt.% a mixture of deformity with triptorelin. The total amount of tetrafluoroethylene 1260 After condensation synthesis gas obtained 3096 g of product containing 99.9% of Pentafluoroethane, 0.1% tetrafluoroethylene. The performance of the process 200 g/LCH.Example 2.Under the conditions described in example 1, the process is conducted in the presence of 5 to 10-4wt.% a mixture of deformity with triptorelin. After 2 hours of process in the reaction mass discovered polymer in an amount of 10% of spent of tetrafluoroethylene. The process is terminated.Example 3.Under the conditions described in example 1, the process is conducted in the presence of 3 to 10-2wt.% a mixture of deformity with triptorelin. Consumption of triptorelin 18,8 l/H. the synthesis Time is 15 hours. The obtained product with a basic substance content of 93.5%. The performance of the process 170 g/LCH. The method of producing Pentafluoroethane interaction of tetrafluoroethylene with a mixture of iodine, iodine PENTAFLUORIDE at a temperature of 40 - 80oC, characterized in that the catalyst used metal surim
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
FIELD: chemical industry; designs of the bubble-type reactors for production of 1.2-dichloroethane.
SUBSTANCE: the invention is pertaining to the design of the bubble-type reactors for production of 1.2-dichloroethane by the method of the liquid-phase chlorination of ethylene with the reaction heat removal at boiling of the working medium. As the contact device the reactor uses two layers of the metallic nozzle. The liquid 1.2-dichloroethane is fed from above to the nozzle, into the space between the layers of the nozzle feed the gaseous chlorine with nitrogen, and under the lower layer of the nozzle feed the gaseous ethylene with nitrogen, that allows to reduce the diameter of the reactor in 1.5-2 times due to the increased effectiveness of stirring and formation of the developed contact surface of the phases. At that the heat of the reaction is removed by evaporation of 1.2-dichloroethane in nitrogen. At that the temperature of the liquid is maintained below the boiling temperature. The technical result of the invention is the increased selectivity of the process, reduction of the outlet of the by-products (the highest ethane chlorides) and the decreased overall dimensions of the reactor.
EFFECT: the invention ensures the increased selectivity of the process, reduction of the outlet of the by-products (the highest ethane chlorides) and the decreased overall dimensions of the reactor.
1 ex, 4 dwg
FIELD: organic chemistry, chemical technology.
SUBSTANCE: invention relates to a method for synthesis of 1,2-dichloroethane by method of liquid-phase chlorination of ethylene. The process is carried out by direct feeding gaseous reagents chlorine and ethylene in liquid reaction medium of reactor. Before feeding into reactor chlorine and ethylene are heated preliminary in heat-exchangers to temperature equal to that of liquid in reactor. Method provides enhancing selectivity of process and reducing formation of by-side substances representing higher chlorine-derivatives of ethane.
EFFECT: improved method of synthesis.
4 dwg, 1 ex
FIELD: chemical technology.
SUBSTANCE: invention relates to a method for synthesis of 1,2-dichloroethane by method of liquid-phase chlorination of ethylene. Method involves maintaining the optimal ratio of heat eliminated based on evaporation and heat eliminated based on cooling a liquid medium in a heat exchanger in the process. One-sixth part of heat formed in reactor is eliminated based on evaporation of synthesized compound in boiling and 5/6 part of formed heat is eliminated based on circulation of liquid working medium in external heat exchanger. The temperature gradient in the reaction zone is maintained equal 52°C. Invention provides enhancing selectivity of process and reducing amount of by-side products of reaction (higher chlorine-derivate of ethane).
EFFECT: improved method of synthesis.
3 dwg, 1 ex
FIELD: industrial organic synthesis.
SUBSTANCE: invention relates to a process of liquid-phase chlorination of ethylene wherein reaction heat is removed by means of vaporization of reaction medium. Process is conducted at vacuum-mediated reduction of reaction medium boiling temperature below 60°C, vacuum being developed because of condensation of vapors formed in external condenser accompanied by removal of non-condensed gases by vacuum pump.
EFFECT: enhanced selectivity of process and decreased yield of by-products (higher chlorine derivatives of ethane).
FIELD: chemical industry.
SUBSTANCE: vacuum reactor comprises tower (1), distributors of chlorine (2) and ethylene (3), circulation pipe (5), perforated plates (6), condenser (7), pump (8), vacuum-pump (9), and hydraulic valve (10).
EFFECT: improved quality of the product.
FIELD: chemical industry; apparatuses for production of the chlorinated allyl.
SUBSTANCE: the invention presents the reactor for production of the chlorinated allyl intended for realization of the method of production of the chlorinated allyl by the direct gaseous phase chlorination of the propylene. The reactor includes the closed circuit of circulation of the reaction gases, the devices of injection of the source propylene and chlorine, the device of the forced circulation of the part of the reaction gases and the device of withdrawal of the other part of the reaction gases. At that the closed circuit of the reaction gases circulation forms the jet pump, which includes in series connected the reception chamber, the mixing chamber and the diffuser, and the pipe of the circulation circuit connecting the outlet of the diffuser with the appropriate inlet of the reception chamber of the injector and acting as the main reaction zone of the ideal displacement with the presence time of 0.7-0.9 s, in which the scatter of the temperatures does not exceed ±10°С. The reception chamber contains the nozzles used as the devices for injection of the source propylene and chlorine. The jet pump ensures fulfillment of the concerted functions: introduction of the streams of the source propylene and chlorine, which are the working injecting streams; the forced circulation pump with the repetition factor of 5-10 of the reaction gases stream, which is the injected stream; the high-velocity mixer and the preheater of the source reactants in the mixing chamber due to the strong turbulence during (0.01-0.04)s, which is formed by the combination of the nozzles of the injected gases at the arrangement of the nozzle/ nozzles of the chlorine coaxially to the main nozzle of the propylene arranged on the shaft of the mixing chamber. The technical result of the invention is, that the presented design of the reactor allows to increase the selectivity of the process of production of the chlorinated allyl.
EFFECT: the invention provides, that the presented design of the reactor allows to increase the selectivity of the process of production of the chlorinated allyl.
1 ex, 1 dwg
SUBSTANCE: invention relates to method of producing high purity 1,2-dichloroethane from dissolved chlorine and dissolved ethylene which are brought into contact with each other while using a liquid reaction medium excited for circulation, where the said medium essentially consists of 1,2-dichloroethane and a catalyst and at least passes through a vertical reaction zone which forms a loop, where both knees of the loop are joined by a gas separator lying above, from which the reaction product is tapped in gaseous and/or liquid form, characterised by that: at least 3 supply sections are located in the knee of the loop along which the liquid flows upwards; and each of these supply sections consists of a unit for supplying dissolved or gaseous ethylene located at the inlet of the section, and a unit for supplying dissolved chlorine located at the output of the section, and can also have static mixing devices. The invention also relates to a device for implementing the said method.
EFFECT: method is more cost-effective, enables increase of power without increasing outside dimensions of the reactor and simultaneous production of high purity dichloroethane.
3 cl, 1 dwg