Method for producing 1,2-dichloroethane and the device for implementing the method

 

Use: receive dichlorethane. Essence: spend the interaction of ethylene with hydrogen chloride and oxygen-containing gas in the reactor oxidative chlorination with the formation of the reactive gas, in which the reactive gas after the filter is subjected to condensation without the prior stage damping. Technical result: cost reduction in the production of dichloroethane. 2 N. and 18 C.p. f-crystals, 3 ill.

The present invention relates to a method for producing 1,2-dichloroethane (EDC) by reacting ethylene with hydrogen chloride and oxygen-containing gas in the reactor oxidative chlorination, forming a reactive gas.

Under oxidative chlorination understand the interaction of alkene - in this case ethylene with hydrogen chloride and oxygen-containing gas such as air, with the formation of saturated chlorinated alkane - in this case, 1,2-dichloroethane, hereafter referred to as EDC. The reaction occurs according to the following equation:

With2H4+2hcl+1/2O2CL-CH2-CH2-CL+H2O.

However, a by-product of this reaction, the water may form Selecon expensive materials for the manufacture of the equipment.

In krupnoporistogo scale this process is often carried out in a fluidized bed or pseudocyesis layer in the presence of a catalyst mainly of copper chloride on a carrier of alumina.

Made up of German application DE 4132030 known method of removing catalyst dust, which is removed from the reaction zone together with the flow of the crude EDC-containing gas. When this catalyst dust in dry cleaning zone is separated from the crude gas containing dichloroethane. The advantage of this method is that the catalyst dust separated in the cyclone separator or an electrostatic precipitator. This cyclone separator shall be equipped with a bag filter, which is cleaned with compressed circulating gas. After separation of the catalyst dust gas stream is cooled and water is condensed, i.e. extinguished.

Further separated in the purification zone catalyst dust is freed from adsorbed reaction products in the desorption zone. Desorption zone can be used at a temperature of 50-350With, mainly at a temperature of 150-180With by saturating a gas or vacuum and pressurized gas using oxygen, nitrogen or circulating gas (the for 0.5-5 hours, mostly 1-2 hours at elevated temperature.

In this method of preventing contamination of heavy metals and inorganic sludge as produced and supplied water.

The application Germany DE 19546068 A1 relates to a method of reducing consumption of catalyst and contaminated waste catalyst when receiving EDC by way of oxidative chlorination. In this way the catalyst dust from the raw EDC-containing gas stream is separated in the separation zone, which runs dry. Catalyst dust fractions, and a certain fraction return again to the reaction zone. In this way the gas stream after separation of the catalyst dust is also cooled by the water and condense.

In DE-19753165 disclosed is a method of obtaining EDC by oxychlorination process in which the reaction gas in the reactor is freed from catalyst by fine filtration and returned to the reactor. Further purified from the catalyst, the reaction gas is sent to the quenching column, where it is condensed by known methods.

From practice it is known (Ullmann''s Encyclopedia of industrial Chemistry, so A6, 1986, S. 269) that the hot reactive gas containing along with EDC and water and unreacted gaseous Hcl is Otdelenia catalyst dust and unreacted Hcl from oxidative chlorination of ethylene. As wash water can be used as fresh water, and formed during the reaction, the so-called water jet. EDC together with water from the condenser zone of clearing Argonauts and condensed.

All practice technology fluidized bed have the disadvantage that formed by the reaction of polychlorinated dibenzo-p-dioxins/furans (PCDD/PCDF) are used during the mixing aqueous solutions. They should be removed and sent for additional processing, which is quite time-consuming and expensive due to contamination of condensate solutions PCDD/PCDF.

In addition, when the damping cannot be used in thermal energy of the hot working gases (reactive gases).

The objective of the invention is to develop a method and device for producing 1,2-dichloroethane, which formed during the reaction of polychlorinated dibenzo-p-dioxins/furans do not fall into the aqueous phase, and remain in the organic phase.

Another objective of this invention is to develop a method and device that uses thermal energy of the hot working gases.

These tasks are solved by developing a method and device of the above type, in which about who I am. Thus, there is no first required in the prior art, the operation of clearing the way with pseudocyesis layer.

Method and device thanks to this simple and cheaper.

This method does not require the so-called towers of damping that allows you to save space and reduce investment costs.

Further, due to the fact that with this method and the device in the aqueous phase are not PCDD/PCDF, eliminating time-consuming and expensive operation processing. Moreover, polychlorinated dibenzo-p-dioxins/furans (PCDD/PCDF) are separated from the other components and then, for example, together with other high-boiling components of the process are sent for incineration.

Due to the fact that the method and device according to the invention is not damping, it is possible to use thermal energy of the hot working gases. It is mainly used to produce steam or for pre-heating of the circulating gas or ethylene flow is directed into the reactor, for example, in the heat exchanger. The rest of the heat (enthalpy of vaporization EDC and water) may be supplied to other heat exchangers as a cooling medium. Pairs can be used in the future, for example, EDC/I (Winnie the saving energy and reducing costs.

For oxidative chlorination can use conventional reactor. Especially reliable for this purpose, the fluidized bed reactor. The reaction forms reactive gases that contain primarily 1,2-dichloroethane, but also water, hydrogen chloride, PCDD/PCDF and catalyst dust. In addition, they may contain unreacted ethylene and chlorine.

At the stage of oxidative chlorination is used as a rule, the catalysts which are most suitable CuCl2or Fl3.

Especially reliable as a catalyst CuCl2on the media. As the carrier used is silicon dioxide, kieselguhr, fallerovo earth, clay, aluminum oxide, with the most suitable-aluminum oxide.

Process, especially stage oxidative chlorination may be carried out under the conditions described in the German publication 1518931 and German patent 1468489, the disclosure of which is incorporated by reference in this description.

Due to the fact that reactive gases after oxidative chlorination is subjected to fine filtration, the aqueous phase does not get contaminated PCDD/PCDF catalyst, and remains on the filter. Under a thin filtering understand the process, when delayed small activitiesa so, as described for example in PCT/ER/07444. The disclosure of this publication is included by reference in this description.

The filtering process can be carried out of the reactor for the oxychlorination process. This design is particularly advantageous when some part of the system is installed in addition to existing.

However, for new installations it is preferable that the filtering was happening inside the reactor oxychlorination process.

According to the invention the filtering can be performed using filter cartridges, bag and/or cartridge filters. Such filters are described, for example, in the application Germany DE 19753165 A1 and produced, in particular, firms Pall, Micropul, Fluiddynamics, etc.

After filtering the reactive gas perform its cooling (without damping), while, for example, pre-heat supplied to the reactor circulating ethylene mixture and/or receive steam that powers a steam network installation and can be used to heat the columns and pre-heating. In the second heat exchanger reactive gas is partially condensed and the heat (again without damping) is supplied to the cooling fluid, for example, in the heat exchanger. In the separator liquid phase is separated from the circulating gas and napra pressure water-dichlorethane mixture, i.e., the organic and aqueous phase, while it evaporates a large part of the CO2.

In conclusion, water is supplied to the processing of wastewater, and EDC is directed to additional apparatus, in which by treatment with aqueous alkaline solution collapses contained in chloral and/or chloralhydrate. In the decanter EDC is separated from the aqueous phase. The aqueous-alkaline phase from the decanter is also available on the treatment of wastewater.

EDC from the decanter is fed to the distillation, for example in so-called drying column and the columns of light and high boiling. Such columns are known in EDC/I-units. Easy - and high-boiling components is a liquid with a lower and a higher boiling point than EDC. In the described way in the columns of high boiling extract of polychlorinated dibenzo-p-dioxins/furans, along with other high-boiling fractions and then go on burning.

In another form of execution of the invention the supply of at least one educting gas stream containing hydrogen chloride and oxygen, through pipelines, having a porous, gas-permeable elements. According to the invention the oxygen-containing gas can be, for example, air, oxygen Torah oxidative chlorination. Such porous, hispanically elements produce, for example, firms Pall, Fluiddynamics,and other

According to the following preferred form of execution of the supply of ethylene and/or circulating gas in the reactor oxidative chlorination carried out through the bottom, made of a porous gas-permeable material. Such a porous gas-permeable materials are, for example, alloyed steels, vysokokorrozivnuyu alloys INCONEL, MONEL, HASTELLOYand ceramic materials.

Oxygen-containing gas, on the one hand, and ethylene in micronized form, preferably served in pseudocyesis layer of catalyst, as, for example, described in DE 19903335 A1.

Carts can be performed, for example, by the method described in DE 19903335 A1, which is described in the specification.

The method according to the invention is preferably carried out in a special device for producing 1,2-dichloroethane by reacting ethylene with hydrogen chloride and oxygen gas. Such a preferred device comprises a reactor for oxidative chlorination, filter, condenser and distillation device for 1,2-dichloroethane is tion.

The filter is a fine filter, may be formed of filter cartridges, bag and/or cartridge filters.

If you use the filter candles, they must be made from appropriate materials, suitable for EDC. This is, for example, metals, alloys, glass and/or ceramics. Preferably the filter cartridges contain sintered metals and/or ceramics.

In addition, can also be applied to fabric filters are of a sufficiently heat-resistant materials, especially fluoric synthetic materials, such as polytetrafluoroethylene, in the form of a sleeve or cartridge type.

Later it was discovered that distilling the installation should be performed preferably in such a way that it contained the drying column and the column of light and high boiling.

In order to get as clean as possible products, generator, water vapor/eductively heater shall be manufactured from steel, and the capacitors from the working party should be made of Ni-containing materials, such as Ni-alloys, such as HASTELLOYcompany Haynes International, Inc., or tantalum.

Along with this may also work the walls of the water vapor generator and condenser both, in particular, it is important to provide a device podwodami for supplying hydrogen chloride and oxygen-containing gas, leading directly to pseudocyesis layer reactor oxychlorination process.

These pipelines may contain a porous, gas-permeable elements.

Also it is particularly important that the ethylene and the circulation of the gas stream was fed into the bottom of the reactor for the oxychlorination process, made of a porous gas-permeable material or contain such material.

Other advantages and features of the invention are given C the claims, the drawings and description in which, with reference to the drawings described examples of the invention.

Fig.1 shows the claimed device for implementing the inventive method according to the first preferred form of execution of the present invention.

Fig.2 shows the claimed device for implementing the inventive method according to the second preferred form of execution of the present invention.

Fig.3 shows the claimed device for implementing the inventive method according to the third preferred form of execution of the present invention.

In Fig.1 shows a device for implementing statereason gas in the reactor oxidative chlorination with the formation of the reactive gas. Here is a direct condensation with eductional preheat. The filter 5 in this case is located outside of the reactor 4 pseudocapsule layer (in pixels).

In Fig.1 shows the reactor 4, preferably made as a reactor to the PCB. Connected to it two pipelines 1 and 3, of which are working gases. Hydrogen chloride and oxygen are fed into the reactor 4 through line 1, and the ethylene and circulating the gas through the pipeline 3. The pipe 3 has a heat exchanger 6, which uses the waste heat coming out of the reactor reactive gases for preheating ethylene (also called Atena) and/or circulating gas. Ethylene installation is supplied through the pipe 2. The reactor 4 is connected to the filter 5, which is formed in the reactor hot gases are released from the solid particles. The reaction gases are cooled in heat exchanger 6 before they will be directed to the condenser 7, the waste heat from which again is used in the heat exchanger.

At the outlet of the condenser 7 of the reactive gas is still a temperature of about 60C. With the temperature of the mixture containing 1,2-dichloroethane organic and aqueous phase is sent to a separating set the cut pipe 12 is separated from the gaseous phase, which again is used as the circulating gas in the heat exchanger 9 and the thickener 10 circulating gases. Before thickener 10 circulating gases includes a pipe 11 for the exhaust gases.

According to a preferred form of execution shown in Fig.1, the reactive gas after exiting the PCB-reactor is filtered and without damping is condensed.

In Fig.2 shows another preferred form of execution of the proposed invention. Here we have used the same notation of structural elements, as in Fig.1.

In Fig.2 illustrates a block diagram of the installation, in which instead of or in addition to the preheating process gases in the heat exchanger 6 uses the waste heat reactive gases by obtaining the water vapor in the heat exchanger 6A.

Finally, in Fig.3 shows the reactor 4 which is located inside the filter 5, so that the filtration of hot reactive gases occurs in the reactor 4, and by filtering reduces the loss of heat before feeding a reactive gas into the heat exchanger 6, is used to preheat the reaction gas and/or steam generating, in particular water vapor. The rest of us is retana use the reactor for oxidative chlorination with the PCB, and as catalyst CuCl2. The oxychloination is as follows.

5910 N3per hour Hcl with temperature 150C and 1600 N3/h O2heated to 110With serves directly at pseudocyesis layer (40 t catalyst; Al dioxide content C 4 wt.%) reactor 4 via pipelines 1 and 3, containing a porous gas-permeable elements, for example, of Cr-Ni-steel company Pall. Submission of ethylene (3000 N3/h) and flow of the reaction gas occurs through the bottom of reactor 4 oxidative chlorination, and the bottom is made of a porous gas-permeable material. After oxychlorination process hot reaction gas (200-250C) consisting of EDC, N2O CO2WITH nitrogen, With2H4, HCl and O2after passing through the PCB sent to the Department of trapped particles of catalyst (here CuCl2in the upper part of the reactor 4 oxidative chlorination on the fine purification filter 5, where the catalyst and separated.

Hot reactive gas with a temperature of about 200-250From the upper part of the reactor is cooled to 140With in shell and tube heat exchanger made of C-steel. Education is ATEM use for EDC distillation in columns of light and high boiling.

Thus obtained pairs with a temperature of 135C and a pressure of 3 bar is used in a distillation column EDC/I-installation (light columns and high boiling).

On further cooling stage of the reactive gas passes through the tube and shell heat exchanger of the acid-resistant material, for example graphite NS1 company SIGRI where it is cooled to approximately 60C, and the resulting EDC and water from the circulating flow is directed to condensation. The received power is supplied to heat cold water.

Generator 6A water vapor is a horizontal shell-and-tube heat exchanger, in which the OS-containing working gas is fed through the pipes, and the water vapor is collected in a special casing and through pressure valve serves to steam network installation.

The capacitor 7 from the working party is made of graphite, WS2 company SIGRI in order to avoid further contamination of the reactive gases. The condensed product is fed to the EDC distillation, where by distillation separated PCDD/PCDF together with so-called high-boiling fraction and then burn.

Contained in the crude EDC-gas PCDD/PCDF fraction through the lower part of the column of light boil sent to the high column is those with other high-boiling residues are burned in the heat treatment device at 1200C.

Claims

1. Method for producing 1,2-dichloroethane by reacting ethylene with hydrogen chloride and oxygen or oxygen-containing gas in the reactor oxidative chlorination with the formation of reactive gas, wherein the reactive gas is filtered and then without damping condense.

2. The method according to p. 1, characterized in that thermal energy of the reactive gases are used, in particular, to produce steam and/or for cross heat exchange (heating) different production streams, preferably the circulating gas.

3. The method according to p. 1 or 2, characterized in that the reactor oxidative chlorination consists of a reactor with pseudocyesis layer.

4. The method according to PP.1-3, characterized in that the filtering is carried out inside the reactor oxidative chlorination.

5. The method according to PP.1-3, characterized in that the filtering is made outside of the reactor oxidative chlorination.

6. The method according to any of the preceding paragraphs, characterized in that the filtering is performed in the filter candles, filter bag and/or cartridge filters.

7. The method according to any of the preceding paragraphs, characterized in that after the condensation staradub under item 7, characterized in that the distillation of 1,2-dichloroethane first performed at the drying column and the column of light boil and then in the column high boiling point.

9. The method according to p. 8, characterized in that column high boiling/vacuum column is separated polychlorinated dibenzo-p-dioxins/furans.

10. The method according to any of the preceding paragraphs, characterized in that hydrogen chloride, ethylene, circulating gas and/or oxygen-containing gas fed into the reactor oxidative chlorination through a porous gas-permeable elements.

11. Device for producing 1,2-dichloroethane by reacting ethylene with hydrogen chloride and oxygen-containing gas, in particular, using the method according to any of the preceding paragraphs, containing the reactor oxidative chlorination, filter, condenser and distillation device for distillation, 1,2-dichloroethane, characterized in that it includes additional generator water vapor or eductively heater, and also works on cold water condenser and does not contain a quenching column.

12. The device according to p. 11, wherein the filter is a filter candles, filter bag and/or cartridge filter.

13. The device according to p. ubomo of PP.11-13, characterized in that the distillation device comprises dehydrating column, the column of light, and high boiling.

15. Device according to any one of paragraphs.11-14, characterized in that the capacitor from the working party contains a Ni-containing material, for example, an alloy based on Nickel.

16. Device according to any one of paragraphs.11-15, characterized in that the capacitor from the working party contains a graphite material.

17. Device according to any one of paragraphs.11-16, characterized in that the reactor oxidative chlorination is a reactor with pseudocyesis layer.

18. The device under item 17, characterized in that the pipelines to supply hydrogen chloride and kislorodsoderzhathikh gas directly in pseudocyesis layer of the reactor.

19. The device under item 18, characterized in that the piping is formed of a porous, gas-permeable elements.

20. Device according to any one of paragraphs.11-19, wherein the circulation gas and/or ethylene through the bottom, containing a porous, gas-permeable material, fed into the reactor oxidative chlorination.

 

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FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a method for preparing vinyl chloride monomer. Method involves generating outlet flow from reactor by catalytic interaction in common ethane, ethylene, oxygen and at least one source of chlorine taken among hydrogen chloride, chlorine or chlorohydrocarbon wherein the mole ratio of indicated ethane to indicated ethylene is in the range from 0.02 to 50. At this stage of catalytic interaction method involves using a catalyst comprising component of rare-earth material under condition that catalyst has no iron and copper practically and under additional condition that when component of rare-earth material represents cerium then catalyst comprises additionally at least one more component of rare-earth material being except for cerium. Indicated outlet flow from reactor is quenched to form flow of crude product that doesn't comprise hydrogen chloride practically. Flow of crude product is separated for vinyl chloride monomer flow and light fractions flow and the latter flow is recycled for catalytic interaction in common with indicated ethane, indicated ethylene, indicated oxygen and indicated chlorine source at the indicated generating stage. Also, invention proposes variants of a method in producing vinyl chloride. Invention provides the complete extraction of hydrogen chloride from the reactor outlet flow after conversion of ethane/ethylene to vinyl (chloride).

EFFECT: improved producing method.

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EFFECT: improved producing method.

40, 9 tbl, 3 dwg, 31 ex

FIELD: organic chemistry, chemical technology.

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EFFECT: improved conversion method.

61 cl, 8 tbl, 32 ex

FIELD: chemical technology.

SUBSTANCE: invention relates to a method for preparing 1,2-dichloroethane. Method involves the oxychlorination reaction of ethylene with hydrogen chloride and oxygen-containing gas and alkaline treatment of dichloroethane also. Before alkaline treatment of 1,2-dichloroethane carbon dioxide is removed that is carried out by decrease of the reaction mixture pressure comprising 1,2-dichloroethane, or by addition of inert gas wherein nitrogen is used, or by heating. Before separation of carbon dioxide the product of the 1,2-dichloroethane-containing the oxychlorination reaction is quenched, cooled and/or condensed. After separation of carbon dioxide the 1,2-dichloethane-containing reaction mixture is treated with an aqueous alkaline solution followed by its separation. The prepared 1,2-dichloroethane-containing reaction mixture is characterized by the content of chloral and/or chloral hydrate less 0.02 wt.-% but preferable less 0.005 wt.-%, and especially preferably, less 0.002 wt.-%. Invention provides reducing consumption of an alkaline solution, prevention of formation of by-side products of chloral and chloral hydrate, and preparing the pure 1,2-dichloroethane with respect to such by-side products.

EFFECT: improved preparing method.

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FIELD: organic synthesis catalysts.

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EFFECT: increased activity of catalyst at high temperatures and avoided adhesion of catalyst particles and loss of active components.

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FIELD: industrial organic synthesis.

SUBSTANCE: 1,2-dichloroethane is obtained via reaction of ethylene with hydrogen chloride, and oxygen-containing gas. Process is implemented in oxyclorination reactor using fluidized bed to form reaction gas. The latter is filtered outside of oxyclorination reactor on filter having at least one filter candle.

EFFECT: achieved removal of catalytic dust al low cost, high degree of catalyst separation, and satisfactory separation of polychlorinated dibenzo-p-dioxin/furans from reaction gas.

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FIELD: chemistry.

SUBSTANCE: described is a catalyst composition for oxychlorination of hydrocarbons which contains a catalytically effective amount of an oxychlorination catalyst and a diluent which contains aluminosilicate particles, where average size of the particles of the catalyst and diluent ranges from 5 to approximately 300 micrometres. Described is a catalyst composition for oxychlorination of hydrocarbons which contains the following: (a) a catalytically effective amount of an oxychlorination catalyst, having surface area greater than 25 m2/g, in which the oxychlorination catalyst contains support material in which an active salt composition is distributed; and (b) a diluent having surface area from approximately 0.1 m2/g to approximately 25 m2/g, in which the support material and the diluent are chemically different, and average size of particles of the catalyst and diluent ranges from approximately 5 to approximately 300 micrometres. Also described is a method for oxychlorination of hydrocarbons, involving a step for bringing reagents containing hydrocarbons, a chlorine source and an oxygen source into contact with the oxychlorination catalyst composition in conditions for the method to obtain chlorinated hydrocarbons. Also described is a method for oxychlorination of hydrocarbons, involving a step for bringing reagents containing hydrocarbons, a chlorine source and an oxygen source into contact with one of the catalyst compositions described above, containing a catalytically effective amount of an oxychlorination catalyst and an inert diluent under conditions of the method to obtain chlorinated hydrocarbons, in which the method is realised at Topt(2) - optimum working temperature of the method, which is at least approximately 1C higher than Topt(1) - the optimum working temperature of the method which uses the same reactor, the same reagents, amount of loading the reactor, productivity standards and oxychlorination catalyst, but without an inert diluent.

EFFECT: attaining higher reaction temperatures without detriment to other vital parametres of the oxychlorination process.

31 cl, 11 tbl, 9 ex, 8 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to a method of using reaction heat from producing 1,2-dichoroethane from ethylene via an exchange reaction with oxygen and hydrogen chloride (oxychlorination) in a fluidised-bed reactor, while removing said reaction heat through a bundle of cooling pipes which lie in the fluidised bed in the reactor. The method is characterised by that a portion of the reaction heat is removed by heating boiler feed water, wherein the heated boiler feed water is used to heat heat-sinks during production.

EFFECT: use of the present invention improves use of heat while reducing the corresponding installation components.

5 cl, 3 dwg

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