Method for producing 1,2-dipertahankan
(57) Abstract:Method for producing 1,2-dipertahankan relates to chemical technology of production of halocarbons (freons) and can be used to obtain 1,2-dipertahankan (halon 122) relating to perchloromethane low ozone depleting potentials. The method consists in the processing of dispersed trichloroethylene evaporated by uranium hexafluoride, which is diluted with an inert gas, when the reagent ratio close to stoichiometric. What's new is that in the response zone simultaneously with the source reagents injected condensed 1,2-dipertahankan or treatment products in the amount of 0.3 to 2.5 mol of 1,2-dipertahankan on 1 mol of uranium hexafluoride. The method allows to increase the yield of the target product on organic raw materials to 96.3% and significantly improve its quality by reducing the impurity content of trichloroethylene and other impurities. table 1. The present invention relates to methods of producing halocarbons and can be used to obtain 1,2-dipertahankan (halon 122) relating to perchloromethane with low ozone-depleting ability.The replacement of freon to keep the ASS="ptx2">One of these halocarbons that are of practical interest, is 1,2-dipertahankan.A known method of producing uranium tetrafluoride and 1,2-dipertahankan by fluorination of trichloroethylene by uranium hexafluoride (U.S. patent N 3382049, CL 23 353, 1968).The method was designed to obtain uranium tetrafluoride and did not aim to obtain organic product with high quality and output.The closest in technical essence and the achieved result to the present invention is a method of producing 1,2-dipertahankan by processing at elevated temperatures dispersed trichloroethane evaporated by uranium hexafluoride, diluted with an inert gas (nitrogen, argon, etc.,), when the reagent ratio close to the stoichiometric (see RF patent N 2030380 "a Method for obtaining fluorine-containing ethane series").The disadvantage of this method is the low quality and low yield of 1,2-dipertahankan: experimental-industrial tests of the method have shown that the product is contaminated with impurities organofluorine compounds, including admixture of tryptophanate. This mixture has a boiling temperature close to the temperature of the Sabbath./P> The reason for the low quality of the target product by a known method is unacceptably high temperatures in the response zone, causing the occurrence of several adverse reactions.The reaction of interaction of trichloroethylene with uranium hexafluoride is accompanied by the evolution of considerable heat.The known method does not provide the possibility of fast and efficient removal of heat of reaction, resulting in the points of contact of the reacting substances can develop high temperature (>400oC).The proposed method allows to eliminate the disadvantage of this method. It is based on the fact that in the known method for producing 1,2-deverticalization by processing the dispersed trichloroethylene evaporated by uranium hexafluoride, diluted with an inert gas, when the reagent ratio close to the stoichiometric in the response zone simultaneously with the source reagents injected condensed recycled 1,2-dipertahankan or treatment products in the amount of 0.3 to 2.5 gram-moles per gram mole of uranium hexafluoride.Example 1.In a laboratory reactor in the response zone served continuously evaporated exaptation. The molar ratio of the uranium hexafluoride:trichloroethylene:1,2-dipertahankan support equal to 1: 1:2.The resulting tetraploid uranium is poured into the lower part of the reactor and accumulates there, and organic reaction products continuously away from the reactor, condensed and analyzed.The results of the analyses, wt%
The halon 121 0,7
Ferrichloride (C2FCl3) 0.02
Other impurities 0,7
The mass yield of halon 122, calculated as the ratio of the percentage of halon 122 to the sum of the percentage contents of organic products (i.e. excluding unreacted trichloroethylene) is 96,3%
Example 2.Conduct a series of experiments similar to example 1, in which the change amount of HFC 122 supplied in the response zone. In one of the tests (op. N 6) in the response zone serves condensed organic products obtained in example 1.The results of all experiments are summarized in table.The data presented show that the proposed method allows to obtain 1,2-dipertahankan with a minimum content of n is from 0.3 to 2.5 mole of condensed 1,2-dipertahankan on one mol of uranium hexafluoride.At a flow rate of 1.2-dipertahankan on 1 mol of uranium hexafluoride less than 0.3 mol of the positive effect is markedly reduced, and the consumption of more than 2.5 mmol per 1 mol of uranium hexafluoride to further increase the quality and yield of 1,2-dipertahankan does not. Method for producing 1,2-dipertahankan by processing the dispersed trichloroethylene evaporated by uranium hexafluoride, diluted with an inert gas, when the reagent ratio close to the stoichiometric characterized in that the response zone simultaneously with the source reagents injected condensed 1,2-dipertahankan or treatment products in the amount of 0.3 to 2.5 mol of 1,2-dipertahankan on 1 mol of uranium hexafluoride.
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