Method of catalytic oxidation of the feed raw material, a method of obtaining a chromium catalyst and a chromium catalyst

 

(57) Abstract:

Describes a method for the catalytic oxidation of the feed raw materials, including the implementation of the contact of this material in a heated reaction zone in the presence of oxygen with a chromium catalyst on a solid substrate obtained by includ - ing compounds of chromium in the solid substrate with subsequent drying and calcination of the specified substrate containing the specified chromium compound, characterized in that the annealing is performed at 800 to 1100°C for a time sufficient to achieve the temperature of the processed substrate material of at least 800oC. is also Described a method of obtaining a chromium catalyst and a chromium catalyst. The technical result - increase in the efficiency of the process and ensuring environmental safety. 3 c. and 27 C.p. f-crystals, 1 Il., table 1.

The invention relates to the field of catalytic oxidation burn solid, liquid and gaseous, especially halogenated materials.

In the oxidation of chlorinated hydrocarbons is widely used alumina Al2O3in the form of small particles. When using the gamma form of alumina there is a top rate containing one or more oxides of metals: platinum, the platinum oxide/metal etc. In some cases use: Cr2O3-CuO/Al2O3Pt/Al2O3, MnO2/Cr2O3/Al2O3and mixtures containing oxides of cobalt, Nickel, vanadium and molybdenum.

Industrial processes for the catalytic oxidation are designed to destroy effluent organic solvents, organic impurities in the surface waters, by-products of organic synthesis, the exhaust gases of industrial furnaces and vehicles. In large-scale processes for the catalytic oxidation of chlorinated hydrocarbons gas is usually recovered in the form of vapor, and chlorine to form hydrogen chloride and/or chlorine. In the patent and scientific literature describes various approaches to this problem.

In British Patent N 1,506,238 Jamal Iden described the use of the oxides of aluminum and silicon, or mixtures thereof impregnated Cr2O3as solid or liquid catalysts for processing waste stream by-products formed during the oxychloination ethylene. The flow of by-products after oxidation, free of chlorinated hydrocarbons and containing HCl, can be reused in the process of oxychlorination process. The catalyst is up to 450oC. the Author got the catalyst as follows: aluminum oxide is impregnated with solutions of Cr(NO3)39H2O or CrCl36H2Oh, dried in a stream of hot air and made red-hot for about 16 hours at a temperature of 540oC. Method of preparation of the catalyst described by the author, in accordance with generally accepted view, that the temperature of calcination of the catalyst should be slightly above the temperature used during the oxidation, and usually 50-100oC above this value.

Ernest Johnston in U.S. Patent N 3,989,807 described the use of liquid Cr2O3/Al2O3for the regeneration of chlorine mixtures of chlorinated organic compounds from air by direct introduction of such mixtures in the reaction zone. According to this method, chlorine is regenerated to a greater extent in the form of chlorine gas, and not in the form of hydrogen chloride. The catalyst was prepared as follows: a substrate impregnated with a salt or oxide of chromium, dried and calcined at a temperature of 350-500oC. the Catalyst comprises 0.1-20% (wt.) metallic chromium, preferably 0.5-10%, deposited on a substrate with a surface area of at least 50 m2/g, preferably 200 m2oF, then dried at 250oF and calcined at 1300oF (704oC).

In the literature described as decontamination of industrial catalysts Al2O3-Cr2O3after long-term use in the oxidation process streams containing 500 ppm of chlorinated hydrocarbons (C1-C2) and their mixtures (see S. K. Agarwall, J. J. Spivey and J. C. Butt Catalyst Deactivation During Deep Oxidation of Chlorohydrocarbons. Applied Catalysis A: General, 82, (1992), pp. 259-275). The authors found that during long-term use of catalysts in the stream to maintain a high degree of conversion should increase the temperature of the reaction zone. It was shown that there is a continuous deactivation of the catalyst in the oxidation of flow of chlorinated and non-chlorinated hydrocarbons. is due to evaporation and abrasion of the most significant in the oxidation of threads chlorinated hydrocarbons. The authors suggest that the evaporation of chromium oxychloride may be beneficial for the oxidation process, because this opens up new layers of the active surfaces of the catalyst.

There is a method of catalytic oxidation of the feed raw materials, including the implementation of the contact of this material in a heated reaction zone in the presence of oxygen with a chromium catalyst on a solid substrate, which is obtained by incorporating compounds of chromium in the solid substrate with subsequent drying and calcination of the specified catalyst at a temperature of from 400oC to 800oC (EP 0465243 A1, B 01 J 23/26,1994).

When the catalytic oxidation of chlorinated materials in industrial scale the maximum process temperature is limited to the optimum temperature range for the catalyst and corrosion resistance of metal surfaces of the equipment. For example, alloy steel and Nickel is subjected to severe corrosion in the presence of hydrogen chloride and/or at temperatures above 530oC. increase in the temperature of the reaction zone to 530oC can lead to increased corrosion rate. From an economic point of view it is necessary that the degree of conversion of raw material SOS is eat, conventional chromium catalysts lose activity with long-term use for oxidation of chlorinated hydrocarbons to reduce losses of chromium is necessary or decrease decontamination, or reduce the rate of oxidation which reduces the level of activity of the chromium catalyst.

Loss of catalytic activity in the oxidation of using catalysts on the substrate caused by physical abrasion that leads to a change in the substrate material, and reduction of surface area. Loss of activity of metal oxides are associated not only with physical abrasion during contact of the catalyst with a stream of the raw materials, but also by evaporation in the form of chromium oxychloride, which increases in the presence of chlorinated compounds in the feedstock. It is assumed that in some cases, leaching of the catalytic surface is advantageous to maintain activity. The loss of active metal substrate catalyst can be advantageous from a technical point of view, but from the point of view of environmental protection loss of metals can cause some problems, because the composition of the effluent of the catalytic oxidation must comply with local the reed chrome CrO2Cl2included in the list of carcinogens, trivalent chrome in the list of toxic compounds, and there are strict limitations on their concentration in the wastewater. Thus, there is a need to reduce the loss of chromium in the process of catalytic oxidation.

The authors claimed invention was investigated changes in catalysts - metal oxides in the process of their use for the catalytic oxidation of flow of chlorinated hydrocarbons and developed a method of producing catalyst impregnated with chromium, which is characterized by high stability during long-term use. Thus, the use of the catalyst not only improves efficiency, but also ensures the safety of the environment.

According to the invention, a method of producing the catalyst is in the fixation of chromium on the substrate. The resulting chemical conversion catalyst, providing a significant reduction of losses of chromium for long-term use of the catalyst in the process. The activity of this catalyst does not decrease after several thousand hours of use in the stream with a catalytic aciclostad chrome compounds and calcining the impregnated substrate at 725-1100oC.

According to the invention further proposes a method of using chromium catalyst for the oxidation of the combusted solids, liquids and/or gases. The process of catalytic oxidation of the feed material is in contact with the feed material in the reaction zone at the reaction temperature of 400-800oC in the presence of air or oxygen, and in the reaction zone should be a catalyst consisting of chromium, deposited on a substrate during annealing at temperatures 725-1100oC. Most preferred are processes, including regeneration heat of reaction and chlorine to form hydrogen chloride and/or chlorine.

The way chromium deposition on a substrate at higher temperatures leads to a decrease of the surface area of the substrate in comparison with the known methods. However, it was shown that the catalyst obtained according to the invention, provides a significant reduction of losses of chromium and a very high degree of conversion for a long period without increasing the process temperature. The optimal process temperature may be significantly higher than when using conventional chromium catalysts. If this save is lately substances, as polychlorinated biphenyls, dibenzofurans and dibenzodioxins.

In Fig. 1 shows a plot of the chromium in the catalyst (weight percent) on time use in the stream (hours) 3-chrome catalysts obtained by annealing to the substrate at 704, 750 and 900oC.

The method of producing catalysts and catalytic oxidation are designed for use in processes with fixed or liquid reaction layer depending on certain physical properties of a solid substrate. In the process using a catalyst containing 0.1-30%, preferably 0.5-20%, more preferably 2-10%, and most preferably 4-6% by weight of metallic chromium to the total weight of the catalyst. When the chromium compound is applied onto the substrate at a temperature 725-1100oC. as compounds of chromium using CrO3or CrCl3. To obtain the catalyst is most preferable to use a substrate with a surface area of 100-250 m2/g or 130-220 m2/, for Example, upon receipt of the catalyst is aluminum oxide for use in processes with liquid layer annealing at 725-1100oC can lead to a significant reduction of the area overheating may be 50-150 m2/, Preferably calcined catalyst at 750-1100oC, more preferably 800-1100oC, most preferably at 850-1100oC, and better at 900-1100oC.

The method of applying a chromium on a substrate designed for use of the catalyst in the reactor with a fixed layer. The method of obtaining a fixed catalyst layer includes drying and extrusion or granulation of aluminum oxide, followed by treatment with a chromium compound and roasting. Dry aluminum oxide (Al2O3) can be obtained using well-known industrial methods. For example, the interaction of sodium aluminate with an appropriate reagent is formed hydrogel of alumina. In another case, when the interaction of ammonium hydroxide to a salt of aluminum, for example, sulphate or aluminium chloride are added in sufficient amount to form aluminum hydroxide. In the drying and calcination of aluminum hydroxide is formed of aluminum oxide. Aluminum oxide fray with slow addition of water up until the moisture content reaches 50%, and to the consistency of aluminum oxide, suitable for carrying out the extrusion. Then the aluminum oxide to extruder using a belt drier or dryer with tray and calcined 1-4 hours at a temperature of 480-750oC. the Calcined extrudate is characterized by a large surface area and porosity. Extruded particles impregnated with an aqueous solution (50%) chromic acid at a temperature of 50oC. the resulting mixture was dried at 120oC and annealed at 725oC and above. Almost the time of annealing can reach from 1 to 24 hours, however, satisfactory results can be obtained when the temporary drying in continuous drying for 3 hours. The aluminum oxide can be enjoyed on a number of commercial firms, including Alkoa Industrial Chemicals Division, Bauxite, Ar., USA or Alkoa International, Lausanne, Switzerland.

For brevity in the description of the proposed invention includes examples of receiving only the catalyst for use in the reactor with the liquid layer. For such catalysts, it is preferable to use particles with an average diameter in the range of 40-140 μm. It is recommended to avoid the formation of too small or "fine" particles with diameter less than 20 microns. "Fine" particles of the catalyst can be regenerated in the process of catalytic oxidation using cyclone separators.

On a substrate applied the following salts and chromium oxides: chloride chromium 3 and chromium 2, the chromium oxide 4, phosphate, HRO the Oia and sodium bichromate. Preferred is the use of chloride chromium 3 and chromium acid, the latter being most preferred. Differences in the efficiency of catalysts containing chromium oxide or chromium chloride 3 was not observed. Compounds of chromium can be enjoyed on the number of firms (see catalog Chemicalweek Buyers Guide, Oct. 1991, Chemicalweek International, Inc).

It is preferable that the content of metallic chromium in the substrate was 0.1-30% or 2-10% (wt.) metallic chromium. Most preferably 4-6% (wt.). Chrome compounds are usually dissolved in water for impregnation of the substrate. 0.3% of chromium oxide correspond to 0.1% metallic chromium, 2% metallic chromium corresponds to 6% Cr2O3; 10% metallic chromium corresponds to 29% Cr2O3.

As solid substrates for the preparation of catalysts used: Al2O3, SiO2-Al2O3Mo-Al2O3active Al2O3, silica gel, diatomaceous earth, fuller's earth, kieselguhr, pumice, asbestos, colic, bentonite, zeolites (zeolite A, X and Y), silica-magnesium oxide-Al2O3, Cr2O3-Al2O3. Most preferred is a substrate of aluminum oxide and aluminum oxide enriched gamma form. Promice may be agglomerated or processed by granulation or extrusion, as described above for reactors with a fixed layer, or by using spray drying and calcination powder for use in reactors with liquid layer.

As raw materials can use a number of combusted materials in any form that you can enter into the reaction zone of combustion. For example, chlorinated hydrocarbons are usually mixtures or compounds containing only carbon, chlorine and hydrogen or carbon, chlorine, hydrogen and oxygen. Such mixtures of chlorinated hydrocarbons may contain compounds with a low molecular weight, i.e., contain from 1 to 30 carbon atoms, and, more typically, from 2 to 8 carbon atoms, or compounds with large molecular weight, i.e., chlorine-containing polymers or plastic with a molecular weight of about 1 million or more. As raw materials can use waste gas streams furnaces burning or intermediate products of chemical synthesis, such as the synthesis of vinyl chloride or chloroprene, synthetic food, the processes of production of different coatings or processes using other solvents. As specific examples of the combusted material contained in the effluent can lead uglevodoroy to vinyl chloride, dichloropropane, dichloroethylene, trichloroethylene, pentachloroethane, hexachlorodibenzodioxin, hexachlorodibenzofuran, tetrachlorobiphenyl, intermediate products of ethylene oxychlorination process, polyvinylchloride, polyvinylidenechloride, polychloroprene, polytetrafluoroethylene, and chlorinated polyethylene. To use active chromium catalyst is most preferred is zero or minimal (< 100 ppm) content in raw materials of metal impurities such as copper, calcium or sodium. These impurities should be removed before processing.

Loss of chromium catalysts obtained by known methods, is directly proportional to the total number of raw material passing through the reaction zone. Thus, loss of chromium increases with increasing concentration of the feed components in raw materials. The method of obtaining chromium catalyst described in the present invention, and its use for the catalytic oxidation of the feed material can significantly reduce the loss of chromium by burning more concentrated raw materials. Moreover, this method allows to obtain a high degree of conversion of polychlorinated samples, which are usually not oxidized completely Klenow zone. For example, chlorinated organic compounds can be mixed in the reaction zone in the vapor phase with oxygen or gas containing oxygen, or mix them up to feed to the reaction zone. Non-volatile organic compounds can be fed into the reaction zone in liquid form, for example in the form of drops, spray, or via an air nozzle in the form of a jet. If necessary, chlorinated organic compounds, which in the normal state are solid at the reaction temperature or they are sublimated, can be dissolved in a liquid solvent, for example, low-boiling(s) chlorine(their) hydrocarbon(Ah) before introduction into the reaction zone, or enter them in the form of suspensions or solids. Solid particles of the polymer, such as soil or crushed particles, can be dosed into the reaction zone with the tape blade. Description of suitable reactors with liquid and fixed layer are given in a review article, "Vinyl Chloride" (J. A. Cowfer and A. J.'s magistro, Kirk Othmer Encyclopedia of Chemical Technology, volume 23, 3rd ed., (1983), JohnWiley, pp. 865-885. Reactors with liquid layer are cylindrical vessels made of highly corrosion-resistant alloys of Nickel and steel, and has an internal coil, dig catalyst particles. Reactors with a fixed layer are typically Novotrubny heat exchangers filled with a vertical catalyst tube fixed to the tubular bars at the top and bottom parts of the reactor. Heat away usually by generating steam in the reactor vessel or by using any other heat transfer fluid. You can use a mixture of the catalyst with an inert diluent, which is placed in a certain proportion, therefore, to provide a low catalytic activity at the inlet of the reactor and the gradient activity towards the outlet. The reactor may be made of Nickel alloy, its design may be a liquid layer or the fixed layer. The main factors influencing the process of catalytic oxidation, is the process temperature, the ratio of carbon and oxygen in the raw material, the ratio of hydrogen and chlorine and contact time of the mixture components in the burning zone. The calculation of relevant ratios can only be done with appropriate composition and properties of raw materials. For example, the chlorine content of the organic liquid raw material can be calculated density of sample (indirect method definitions). In baltinstrument or an excess of molecular oxygen relative to carbon (O2:C2). Preferably, the ratio of oxygen to carbon was 1.1:1. To determine and control the velocity of the incoming air or oxygen to the flow rate of the feed material can be carried out quantitative measurement of excess oxygen in the flowing stream. Under optimal conditions, the regenerated chlorine in the combustion process is included in the resulting stream is preferably in the form of HCl, and the number of Cl2can be up to 20% of the total chlorine content of the resulting thread. For the preferred formation of HCl in the combustion process it is necessary to maintain the molar ratio of hydrogen to chlorine in the reaction mixture, equal to more than 1.4, i.e. in the range from 1.4 to 5.5. The combustion temperature at which the conversion rate is more than 90% of the feed material should be more than 300oC. the Optimum temperature depends on the chemical composition of the raw material. In most cases, the combustion of chlorinated aromatic hydrocarbons is not full, therefore, it is preferable to raise the temperature of the process up to 455 - 525oC. At temperatures above 455oC is a conversion of more than 99% of the raw materials. The contact time in the burning zone may be from the 5 to 100 seconds, better from 5 to 50 seconds. In the reaction zone can be used atmospheric, reduced or elevated pressure. Basically, the pressure in the reaction zone may be from 0.5 to 15 MPa, preferably from 0.5 to 10 ATM, better from 1 to 7 ATM. Basically, the process of catalytic oxidation begins with the filing of hot air through the catalyst bed until then, until a temperature of approximately 300oC. Then add a lower, saturated, tonirovany hydrocarbon, and released heat of reaction provides the desired temperature in the reaction zone. Designed for burning raw material is introduced into the reaction zone and modulate the process in such a way as to provide a stationary conditions and 99% conversion of raw materials in chlorine, oxides of carbon and water. The most simple way of analysing the relationship of carbon to oxygen is in the measurement of excess oxygen in the gas mixture in the hole to reset. If you know the composition of the feedstock and the equation for the combustion reaction, it is easy to calculate the molar ratio of carbon to oxygen using the normal stoichiometry. After a certain period of time in the reactor add a further quantity of catalyst as it is galling to ensure optimal conditions for the process of the Oia oxidation process using the catalyst. The experiments were carried out to map the extent of the loss of chromium by contact of the catalyst with a stream of the reaction mixture, depending on the method of manufacture of the catalyst. As previously stated, lamivudine particles of chromium catalyst layer into the stream flowing from the reactor, and in accordance with limitations on the protection of the environment the presence of chromium in the wastewater must be considered.

Examples 1 - 3

The catalyst was impregnated with chromium, obtained as follows: 256 g CrCl36H2O are dissolved in 300 ml of distilled water to obtain a clear solution. 845 g of gamma-alumina is placed in a mixer with postoloprty stirrer and with slow stirring, gradually add the aqueous solution of chromium chloride in several minutes. The catalyst was dried and divided into several portions, which are calcined at different temperatures, as indicated below. The calcination is carried out in the presence of steam during the night. To obtain industrial designs catalyst you can use an ordinary rotary kiln. The time of firing the impregnated chromium compound of the solid catalyst should be from a few seconds to neskolko, to the solid material of the catalyst was heated to 725oC, preferably at least 800oC, it is better, at least up to 850oC and most preferably up to 900oC. Use redundant time of annealing is unprofitable, as this may lead to undesirable reduction of the area of the catalyst due to the phase transition, in particular it relates to a substrate of gamma-aluminum oxide. In examples 1 to 3, the annealing was performed under the following conditions:

Example - Temperature calcination,oC

Control 1 - 704

2 - 750

3 - 900

Each sample of the catalyst was tested individually in a laboratory quartz reactor (inner diameter 30 mm) with a liquid layer, equipped with heating elements for temperature control. The height of the liquid layer was approximately 18 inches. The upper part of the quartz tube was expanded to an internal diameter of approximately 60 mm and got the cone, which is used as a cyclone to hold the catalyst particles. Each sample of the catalyst was filled in a column volume of 180 cm3Raw materials containing 31% (weight. ) perchlorethylene and 69% (wt.) dichlorobenzene, was injected through the inlet of the reactor in such a way that is at 450oC. the flow Rate of the raw material after the start of the process was 0.14 g/min air Flow was divided into two equal flow. One part of the stream was mixed with the flow of raw materials directly before entry into the reaction layer, another part of the thread was filed in the lower part of the quartz reactor. The total air flow rate was approximately 27 mmol/min Gas flow flowing out of the reactor, barbirolli through the layer of water and the resulting samples were dried in a desiccator for subsequent analysis by gas chromatography. The chromium content in the original catalyst and through certain periods of time after its use was determined by the method of fluorescent emission x-ray (XRF) x-ray fluorescence spectrometer (Fisons model ARL 8410). Used for the analysis of the K-alpha 1,2-line chromium (69,36 degrees, crystal LIF 200) and FPC detector. Parameters x - ray tube 50 Kv and 50 Ma. The results are shown in Fig.1 and table 1.

The table shows that with continuous use of the catalyst (obtained according to example 1) within 450 hours loss of chromium be 31.7%, when using the catalyst according to example 2) for 491 hours loss decreased to 12.8%, and in the use of the main parameter, affecting the stability of the catalyst is the temperature at the stage of calcination and the data obtained indicate that there is a significant, unexpected transition temperature degree of fixation of chromium in the catalyst is in the range between 704 and 750oC. When annealed at 725oC there is a significant decrease losses of chromium compared with the catalyst calcined at 704oC. Reduce emissions of chromium in the waste gas stream, depending on the treatment of the catalyst according to examples 1, 2 and 3 is of great commercial importance. For example, taking into account the capacity of the reactor is equal to 100,000 pounds (45 400 kg), and 0.15% loss of chromium per day associated with the physical abrasion of chromium catalyst, loss of chromium in the year connected with his entering into the waste gas flow values are given in the end of the description.

Obtained according to the invention (including stage of annealing at 900oC) the catalyst is characterized by high stability in long-term use in the reactor; however, there are start-up losses of chromium, approximately 10%, after use in the stream during the first few hundred hours during the combustion of materials containing 31% per udaetsya, moreover, there is no change in its activity after use for more than 3000 hours at a constant temperature. Due to the fact that the essence of the invention is reduced to the preferred embodiment of the process parameters, it is possible that an experienced, qualified professionals can reproduce the methodology with the help of various modifications based on the above description. To exclude the possible modification of the proposed method, the authors state the implementation of the method described in the claims.

1. Method of catalytic oxidation of the feed raw materials, including the implementation of the contact of this material in a heated reaction zone in the presence of oxygen with a chromium catalyst on a solid substrate obtained by incorporating compounds of chromium in the solid substrate with subsequent drying and calcination of the specified substrate containing the specified chromium compound, characterized in that the annealing is performed at 800 - 1100oC for a time sufficient to achieve the temperature of the processed substrate material of at least 800oC.

2. The method according to p. 1, characterized in that it includes a stage of regeneration of eye-catching components, belonging to the group of hydrocarbons, chlorinated hydrocarbons, chlorinated polymers and mixtures.

4. The method according to p. 1, characterized in that the catalyst contains 0.5 to 30.0 wt.% metallic chromium.

5. The method according to p. 1, characterized in that the time in this stage of calcination is 1 to 24 hours

6. The method according to p. 1, characterized in that the chromium compound selected from the group of compounds, including chromium chloride, chromium phosphate, chromium nitrate, chromium acetate, chromium formate, chromium bromide, chromium carbonate, chromium hydroxide, barium chromate and bichromate of barium.

7. The method according to p. 1, characterized in that the use of the combusted material containing a by-product of wastewater received at the oxychloination ethylene.

8. The method according to p. 1, characterized in that in the reaction zone support temperature of 400 - 800oC.

9. The method according to p. 1, characterized in that in the reaction zone, introducing a molar excess of oxygen relative to carbon.

10. The method according to p. 1, characterized in that the use of the combusted material containing chlorinated compounds and fed into the reaction zone to provide the relationship of hydrogen to chlorine 1,4 - 5,5.

11. The method according to p. no fixed layer.

12. The method according to p. 1, characterized in that the shape and size of the catalyst perform suitable for use in the reaction zone with a liquid layer.

13. The method according to p. 1, characterized in that the material of the solid substrate is selected from compounds of the group comprising alumina, alumina - silica, oxides of molybdenum and aluminum, activated alumina, silica gel, diatomaceous earth, fuller's earth, kieselguhr, pumice, asbestos, kaolin, bentonite, zeolite, silica-magnesium oxide-aluminum oxide.

14. The method according to p. 13, characterized in that the material of the substrate is an aluminum oxide.

15. A method of obtaining a chromium catalyst, including the implementation of the contact material of the solid substrate with a chromium compound with the formation of the processed substrate material, with subsequent drying and calcination of the specified processed substrate material, characterized in that the annealing is performed at 800 - 1100oC for a time sufficient to achieve a temperature of the substrate material of at least 800oC.

16. The method according to p. 15, characterized in that the material of the solid substrate is selected from compounds of the group consisting of aluminum oxide, the howl of the earth, the fuller's earth, diatomaceous earth, pumice, asbestos, kaolin, bentonite, zeolite, silica-magnesium oxide-aluminum oxide.

17. The method according to p. 16, characterized in that the material of the substrate is an aluminum oxide.

18. The method according to p. 15, characterized in that the temperature of calcination is 900 - 1000oC.

19. The method according to p. 15, characterized in that the shape and size of the catalyst perform suitable for use in the reaction zone with a fixed layer.

20. The method according to p. 15, characterized in that the shape and size of the catalyst perform suitable for use in the reaction zone with a liquid layer.

21. The method according to p. 15, characterized in that the content of metallic chromium in the catalyst is 0.1 - 30.0 wt.%.

22. The method according to p. 15, characterized in that the content of metallic chromium in the catalyst is from 2 to 10 wt.%.

23. The method according to p. 15, characterized in that the content of metallic chromium in the catalyst is from 4 to 6 wt.%.

24. Chromium catalyst containing a chromium compound and the material of the substrate, characterized in that the catalyst is obtained by calcination at 800 - 1100oC after suggesting Arial solid substrate selected from compounds of the group, including alumina, alumina-silica, oxides of molybdenum and aluminum, activated alumina, silica gel, diatomaceous earth, fuller's earth, kieselguhr, pumice, asbestos, kaolin, bentonite, zeolite, silica-magnesium oxide-aluminum oxide.

26. The catalyst p. 25, characterized in that the material of the substrate is an aluminum oxide.

27. The catalyst according to p. 24, characterized in that the annealing is performed at 900 - 1000oC.

28. The catalyst according to p. 24, characterized in that the shape and size of the catalyst perform suitable for use in the reaction zone with a fixed layer.

29. The catalyst according to p. 24, characterized in that the shape and size of the catalyst perform suitable for use in the reaction zone with a liquid layer.

30. The catalyst according to p. 24, characterized in that it has a surface area of at least 50 m2/,

 

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