Method for liquid-phase catalytic alkylation of aromatic amines

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a method for liquid-phase catalytic alkylation of aromatic amines. Method involves alkylation reaction of aromatic amines in the presence of hydrogen and lower alcohols at temperature 50-70°C on a heterogeneous catalyst. The distinctive specificity of method represents alkylation of amine with formaldehyde solution in reactor with reaction zone filled with catalyst consisting of aluminum oxide-base block high-porous cellular carrier with porosity value 7-95%, not less, and palladium as an active component with the mass content = 1.3-2%. As a rule, in the alkylation process catalyst prepared by impregnation of block high-porous cellular carrier with palladium salts treated preliminary in the constant magnetic field is used. Usually, in the case of alkylation of aniline and for preferential synthesis of monomethylaniline the molar ratio aniline to formaldehyde solution = 1.6:(1.1-1.6) is used. Proposed method as compared with the nearest analog in the case of alkylation of aniline provides preparing monomethylaniline mainly, to decrease the content of palladium as an active component in catalyst and to decrease the reaction pressure and hydraulic resistance of catalytic layer also. Invention can be used in producing antiknock additives to motor fuels (gasolines).

EFFECT: improved alkylation method.

3 cl, 4 ex

 

The invention relates to chemical-technological processes, such as petrochemical synthesis, in particular to a method for the catalytic alkylation of aromatic amines in the presence of hydrogen, used as anti-knock additives to motor fuel (gasoline) to increase its octane number.

It is known that the implementation of such processes are widespread processes of alkylation carried out in the gas phase by heterogeneous granular catalysts, for example, type NTC (low-temperature conversion of carbon monoxide), used in the production of hydrogen and ammonia (see, for example, a Method of obtaining N-methylaniline, RF patent No. 2066679, C 07 C 211/48, 01 J 23/86, Joint production of aniline and N-methylaniline, RF patent No. 2135460, 6 C 07 C 209/36, 211/46, 211/48, the Catalyst to obtain N-methylaniline, the patent of the Russian Federation No. 2066563, 6 01 J 23/84, C 07 C 211/48).

Alkylation of aniline in the presence of hydrogen on the catalyst type NTC (low-temperature conversion of carbon monoxide) or oxide composition: oxides of copper, manganese and aluminum occurs at elevated temperatures equal to 180...270°that increases the energy consumption for the process increases the amount of impurities in the target product and increases the risk of the process and is a disadvantage of known methods.

The most the closest to the technical essence and the achieved result to the present invention is a method of liquid-phase alkylation of aromatic amines, including aniline, an aqueous solution of formaldehyde in the presence of hydrogen in a heterogeneous palladium-based catalyst carrier of aluminum oxide in the presence of aliphatic C1-C5alcohols in the temperature range from 20 to 250°C and pressures up to 30 MPa (see patent US 4952734, "Process for preparing methylamines, published 28.08.1990).

The disadvantages of this method are in the process of alkylation of aromatic amines have a preferred output dimethylamino (for example, N,N-dimethylaniline, N,N-dimethyl-n-octylamine, N,N1-dimethylethylamine), high concentrations of the active catalyst component is palladium (5 wt%), high pressure reactions (up to 30.0 MPa), increased hydraulic resistance of the catalyst layer, which is in the process of alkylation (bulk catalyst layer consists of tablets).

The technical result, which directed the inventive method is a preferred process for the alkylation of aromatic amines getting monomethylaniline, reduction in catalyst content of the active component is palladium, reducing the pressure of the reaction and decrease the hydraulic resistance of the catalyst layer.

To achieve the technical result in the proposed method, liquid-phase alkylated the e aromatic amines exercise formalin in the reactor with a reaction zone, filled with a heterogeneous catalyst consisting of a block of high porosity porous media on the basis of aluminum oxide with a porosity of not lower than 70-95% and the active component is palladium with a mass content of equal to 1.3-2.0%, in the presence of hydrogen in the temperature range of 50-70°and initial hydrogen pressure equal to 0.4 MPa. As the source of the reaction mass using aniline and formaldehyde in a molar ratio equal to 1.6:(1,1-1,6), the lower alcohols (ethyl or methyl). The specified molar ratio selected on the basis of stoichiometry with a small surplus. Block highly porous cellular material (oxide of aluminum) with a porosity of not lower than 70-95%, is used as the catalyst carrier has a high Aero - and hydroponically, has a higher ratio of external mass transfer and low hydraulic resistance as compared with carriers of cellular structure and a bulk catalyst layer of the tablets. The process of liquid-phase alkylation (methylation) is conducted in the presence of an organic solvent, satisfactory solvent as the starting amine, and forming N-methylamine. The most convenient solvent are lower alcohols, in particular ethyl and methyl, in some cases, there may be used a source amines (aniline) and other solvents.

<> The catalytically active component of the catalyst is palladium is applied to block a highly porous cellular carrier by impregnation of soluble salts of palladium (palladium nitrate), pre-treated in a constant magnetic field. Heat treatment of the applied layer of palladium nitrate is carried out at a temperature of 450°C. the Recovery of palladium oxide to the metal, carried out the molecular hydrogen at a temperature of 50...55°C for one hour.

Examples.

In the reactor, which is a cylindrical vessel with an inner diameter of 50 mm, made of stainless steel, load 90 ml of ethyl or methyl alcohol, then pour aniline and formaldehyde in the ratio of 1.6:1,1. Block a highly porous honeycomb catalyst weight 30 g, with a porosity of 70-95%, containing 1,3-2,0% palladium, placed in the middle part of the reactor, providing its immobility due to mounting crosspieces and washers. The reactor lid, which provides a pocket for thermocouple fitting for input of hydrogen. The reactor using a special clamp fixed on the rocking chair, capable of producing the number of oscillations is equal to 120-160 min-1while the conditions under which the reaction is not limited by diffusion of the components to the outer surface of heterogeneous block highly porous honeycomb catalyst. Under eribaum the desired temperature in the reactor by the flow of the coolant in the jacket of the reactor from thermostat. The reactor isolate the asbestos to prevent heat loss into the environment.

1. When carrying out the synthesis of monomethylaniline (MMA) on heterogeneous block highly porous honeycomb catalyst with a mass content of 1.8% palladium free volume of the reactor is filled with hydrogen to the initial pressure of 0.4 MPa. The reaction rate estimate pressure drop in the reactor at a given temperature, 50...56°C. the Duration of the reaction is 600, the hydrogen pressure is changed at the same time from 0.4 MPa to 0.3 MPa. The products after the reaction of alkylation of aromatic amines in the reactor was analyzed by gas chromatography.

The reaction products were detected: 34.6% of monomethylaniline (MMA), 6,8% of dimethylaniline (DMA), 58.6% of unreacted aniline. The ratio of MMA:DMA is 1.0:0,2. For comparison in the experiments with the use of a catalyst prepared according to the traditional technology (soluble palladium salt is not processed in a constant magnetic field), the ratio of MMA:DMA is 1.0:4,0.

2. When carrying out the synthesis of MMA block on a highly porous honeycomb catalyst with a mass content of 1.3% palladium free volume of the reactor is filled with hydrogen to the initial pressure of 0.4 MPa. The reaction rate estimate pressure drop in the reactor at a given temperature, 50...52°C. duration the reaction is 730, the hydrogen pressure is changed at the same time from 0.4 MPa to 0.27 MPa. The composition of the reaction mixture after the alkylation reaction in the reactor: 52% MMA, 11.8 percent DMA, 36.2% of unreacted aniline. The ratio of MMA:DMA is 1.0:0,23.

3. When carrying out the synthesis of MMA block on a highly porous honeycomb catalyst with a mass content of 1.6% palladium free volume of the reactor is filled with hydrogen to the initial pressure of 0.4 MPa. The reaction rate estimate pressure drop in the reactor at a given temperature, 50...53°C. the Duration of the reaction is 630, the hydrogen pressure during the reaction is changed from 0.4 MPa to 0.3 MPa. The composition of the reaction mixture after the alkylation reaction in the reactor: 47,6% MMA, 10% DMA, 42,4% unreacted aniline. The ratio of MMA:DMA is 1.0:0,23,

4. Methylation of aniline is performed on a block of highly porous honeycomb catalyst with a content of 2.0% palladium, the free volume of the reactor is filled with hydrogen to the initial pressure of 0.4 MPa. The reaction rate estimate pressure drop in the reactor at a given temperature equal to 80°C. the duration of the synthesis reaction is 470, the hydrogen pressure during the reaction is changed from 0.4 MPa to 0.26 MPa. The composition of the reaction mixture after the alkylation reaction in the reactor: 53% MMA, 14% DMA, 33% of unreacted aniline. The ratio of MMA: DMA is 1.0:0,26.

In all the above examples after the performed tests (implementation of the alkylation reaction in the reactor) was absent erosion heterogeneous block highly porous honeycomb catalyst. This was judged by the transparency of the reaction mass and, as a consequence, prior to performing analyses on the content of the components of the reaction mass after the alkylation reaction in the reactor does not require additional filtering.

To obtain the target N-methylaniline in the commodity as it can be distinguished from catalyzate any conventional manner, for example by distillation.

1. The method of liquid-phase catalytic alkylation of aromatic amines on a heterogeneous catalyst in the presence of hydrogen and a lower alcohol at a temperature of 50-70°C, characterized in that the alkylation is carried out with formaldehyde in the reactor with a reaction zone filled with a catalyst consisting of a block of high porosity porous media on the basis of aluminum oxide with a porosity of not lower than 70-95% and the active component is palladium with a mass content of equal to 1.3 to 2.0%.

2. The method according to claim 1, characterized in that the use of a catalyst obtained by impregnation of a block of high porosity porous media soluble salts of palladium, pre-treated in a constant magnetic field.

3. The method according to claim 1, characterized in that in the case of alkylation of aniline to receive preferential monomethylaniline use a molar ratio of aniline to formaldehyde 1,6:(1,1-1,6).



 

Same patents:

FIELD: organic chemistry.

SUBSTANCE: claimed method includes reduction alkylation of nitrobenzene or mixture thereof with aniline using methanol in gaseous phase on oxide copper-chromium catalyst. Said reduction alkylation is carried out in mixture of hydrogen and carbon dioxide in molar ratio approximately of 3:1, obtained by gaseous phase methanol condensation with water. Preferably hydrogen and carbon dioxide mixture is obtained in separate contact apparatus from 20-90 % aqueous methanol on oxide copper-iron-chromium catalysts followed by or without separation of methanole and water vapors. Amount of hydrogen and carbon dioxide mixture feeding to alkylation must be sufficient to provide hydrogen/nitrobenzene ratio in limits of 4-6 mol to 1 mol of nitrobenzene. Nitrobenzene/aniline mol ratio is from 0.1-1.0 to 2:1.0; and amount of methanol feeding to alkylation is 0.5-1.5 mol to 1 mol of nitrobenzene or mixture thereof with aniline. Off-gases may be recycled.

EFFECT: method for production of N-methylaniline with improved efficiency.

6 cl, 2 tbl, 7 ex

FIELD: organic synthesis catalysts.

SUBSTANCE: invention provides improved method for preparing catalyst for synthesis of N-methylaniline from aniline and methanol. Method comprises impregnation of alumina carrier with copper nitrate solution, to which were added nitrates of modifying metals selected from group consisting of manganese, chromium, iron, cobalt, and zinc, after which impregnated carrier is dried at temperature ensuring effective conversion of deposited nitrates into oxides of corresponding metals. When calcined, catalyst is subjected to additional impregnation with copper ammine solution, wherein Cu content (on conversion to oxide) lies within 0.6 to 7.0% based on the weight of catalyst, then dried at 100-120°C, and re-calcined at 230-250°C. After first calcination Cu content is 10.1-13% and after the second it rises by 0.6-5.0%. Lifetime of catalyst increases by a factor of 1.3 to 2.

EFFECT: increased lifetime of catalyst.

1 tbl, 12 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a liquid-phase catalytic method for preparing alkylated aniline used as additive to gasoline for elevating its octane number. Method involves alkylation of aniline with formalin in the ratio aniline : formalin = 1.6 : 1.1 in the presence of hydrogen and fixed palladium catalyst in ethyl or methyl alcohol at temperature 55-65°C and under pressure 0.2-0.4 MPa. The process is carried out in the cylindrical reactor fixed with a rocker with rocking number 120-160 min-1 wherein in its mean part the porous block cellular palladium catalyst is placed and this catalyst comprises an active layer modified with palladium nanoparticles with porosity value 70-95% and the palladium content 1.8-3.7%. In this process hydrogen is fed through a connecting pipe of reactor lid. Method provides declining energy consumption and to decrease part of by-side substances.

EFFECT: improved alkylating method.

4 ex

FIELD: organic chemistry, petroleum chemical synthesis and chemical technology.

SUBSTANCE: invention relates to the improved method for preparing N-methylaniline by reductive N-alkylation reaction of aniline with methanol. Proposed method is carried out at enhanced temperature but usually at temperature 180-280°C on copper-containing catalysts comprising copper in the concentration 9-60 wt.-% as measured for copper oxide and involving reduction of catalyst at temperature 180-200°C and the following isolation of the end product from catalyzate by rectification. The stage of N-alkylation reaction of aniline and reduction of catalyst are carried out in the presence of exhausting gases of this process with the volume rate of raw feeding 0.3-0.7 h-1 and in the mole ratio aniline/exhausting gases = 1:(1-10). Method provides high conversion and yield of the end N-methylaniline, simplifying the technological process and to diminish the cost of the process significantly.

EFFECT: improved preparing method.

2 cl, 7 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to the improved method for preparing N-methylaniline from nitrobenzene, methanol and hydrogen in gaseous phase on a copper-containing catalyst comprising zinc and chrome compounds. The process is carried for two stages in two in-line connected contact reactors and nitrobenzene and methanol or their mixture are fed into each reactor: nitrobenzene is fed into the first reactor and methanol - into the second reactor using in layers charging the catalyst in the first contact reactor and forming "frontal layer" wherein temperature must not exceed 350°C and volume is 10-50% of the total volume of catalyst used in this contact reactor. The preferable mole ratio nitrobenzene : methanol : hydrogen = 1:3:15, respectively. The separate feeding of reagents is possible. For example, all nitrobenzene is fed into the first contact reactor and feeding methanol is carried out into the first and the second contact reactors in the mole ratio 1:2 or 2:1, or all nitrobenzene is fed into the first contact reactor and methanol is fed into the second contact reactor in the amount 1.5 mole per a mole of nitrobenzene. As a rule, 50-70% of all nitrobenzene used is fed into the first contact reactor and 30-50% is fed into the second reactor. In both contact reactor a copper-containing catalyst of the following composition is used mainly, wt.-%: copper oxide, 37-40; chrome oxide 18-20; zinc oxide, 20, and aluminum oxide, the balance, or in both contact reactors a copper-containing catalyst of the following composition is used, wt.-%: copper oxide, 21.4-26.4; chrome oxide, 3.4-5.8; aluminum oxide, 3.3-22.3; binary copper and zinc chromite of empirical formula: ZnxCuyCr2O4 wherein x = 0.8-10; y = 0.4-0.9, 54.5-71.9. Usually, aluminum oxide granules impregnated with copper, chrome and zinc salts in the ratio of active components = 2:1:1, respectively, are used in upper part of the first contact reactor.

EFFECT: improved preparing method.

8 cl, 8 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to the improved method for preparing aniline and N-methylaniline. Method involves gas-phase catalytic reduction of nitrobenzene with methanol or formaldehyde aqueous solutions in preparing aniline and N-methylaniline and formaldehyde aqueous solutions in preparing aniline. Preferably, in preparing aniline and N-methylaniline method involves reduction with methanol an aqueous solution in the concentration 60-80 wt.-% in the molar ratio nitrobenzene to methanol = 1:(1.1-3.5). In preparing aniline method involves preferable reduction with formaldehyde aqueous solution in the mole ratio nitrobenzene to formaldehyde = 1:(1.5-4.0) and temperature 220-250°C. Also, invention relates to applying catalyst in preparing aniline and N-methylaniline comprising zinc, copper and chrome oxides on aluminum oxide and promoting with metal oxides from group comprising iron, manganese, bismuth, cobalt and molybdenum. The content of zinc is 0.1-10% of the catalyst mass, the total content of cooper and chrome is 0.05-15% to zinc mass, and the total content of other metals is 1.0-3.0% to the mass of zinc-copper-chrome components. Proposed method provides carrying out the process without feeding molecular hydrogen to the system with conversion of nitrobenzene up to 100% and the preferable preparing aniline and N-methylaniline depending on parameters of the process. On its base the effective manufacturing aniline and N-methylaniline can be organized using free powers of gas-phase catalytic manufactures.

EFFECT: improved preparing method.

5 cl, 1 tbl, 7 ex

The invention relates to an improved method of obtaining N-methylaniline by alkylation of nitrobenzene formaldehyde or its mixture with methanol on copper oxide catalysts at 220-260C. the Molar ratio of nitrobenzene : alkylating agent is usually 1:(2,5-6,0), and the optimum molar ratio of formaldehyde and methanol in the alkylating agent is 1:1, and formaldehyde can be used in the form of its aqueous solution

The invention relates to a method for producing N-methylaniline by the catalytic hydrogenation of nitrobenzene with hydrogen in the presence of methanol on the catalyst megaromania
The invention relates to an improved method of allocating N-monomethylaniline from catalization N-hydroalkylation of aniline with methanol

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a liquid-phase catalytic method for preparing alkylated aniline used as additive to gasoline for elevating its octane number. Method involves alkylation of aniline with formalin in the ratio aniline : formalin = 1.6 : 1.1 in the presence of hydrogen and fixed palladium catalyst in ethyl or methyl alcohol at temperature 55-65°C and under pressure 0.2-0.4 MPa. The process is carried out in the cylindrical reactor fixed with a rocker with rocking number 120-160 min-1 wherein in its mean part the porous block cellular palladium catalyst is placed and this catalyst comprises an active layer modified with palladium nanoparticles with porosity value 70-95% and the palladium content 1.8-3.7%. In this process hydrogen is fed through a connecting pipe of reactor lid. Method provides declining energy consumption and to decrease part of by-side substances.

EFFECT: improved alkylating method.

4 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to the improved method for preparing N-methylaniline from nitrobenzene, methanol and hydrogen in gaseous phase on a copper-containing catalyst comprising zinc and chrome compounds. The process is carried for two stages in two in-line connected contact reactors and nitrobenzene and methanol or their mixture are fed into each reactor: nitrobenzene is fed into the first reactor and methanol - into the second reactor using in layers charging the catalyst in the first contact reactor and forming "frontal layer" wherein temperature must not exceed 350°C and volume is 10-50% of the total volume of catalyst used in this contact reactor. The preferable mole ratio nitrobenzene : methanol : hydrogen = 1:3:15, respectively. The separate feeding of reagents is possible. For example, all nitrobenzene is fed into the first contact reactor and feeding methanol is carried out into the first and the second contact reactors in the mole ratio 1:2 or 2:1, or all nitrobenzene is fed into the first contact reactor and methanol is fed into the second contact reactor in the amount 1.5 mole per a mole of nitrobenzene. As a rule, 50-70% of all nitrobenzene used is fed into the first contact reactor and 30-50% is fed into the second reactor. In both contact reactor a copper-containing catalyst of the following composition is used mainly, wt.-%: copper oxide, 37-40; chrome oxide 18-20; zinc oxide, 20, and aluminum oxide, the balance, or in both contact reactors a copper-containing catalyst of the following composition is used, wt.-%: copper oxide, 21.4-26.4; chrome oxide, 3.4-5.8; aluminum oxide, 3.3-22.3; binary copper and zinc chromite of empirical formula: ZnxCuyCr2O4 wherein x = 0.8-10; y = 0.4-0.9, 54.5-71.9. Usually, aluminum oxide granules impregnated with copper, chrome and zinc salts in the ratio of active components = 2:1:1, respectively, are used in upper part of the first contact reactor.

EFFECT: improved preparing method.

8 cl, 8 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to the improved method for preparing aniline and N-methylaniline. Method involves gas-phase catalytic reduction of nitrobenzene with methanol or formaldehyde aqueous solutions in preparing aniline and N-methylaniline and formaldehyde aqueous solutions in preparing aniline. Preferably, in preparing aniline and N-methylaniline method involves reduction with methanol an aqueous solution in the concentration 60-80 wt.-% in the molar ratio nitrobenzene to methanol = 1:(1.1-3.5). In preparing aniline method involves preferable reduction with formaldehyde aqueous solution in the mole ratio nitrobenzene to formaldehyde = 1:(1.5-4.0) and temperature 220-250°C. Also, invention relates to applying catalyst in preparing aniline and N-methylaniline comprising zinc, copper and chrome oxides on aluminum oxide and promoting with metal oxides from group comprising iron, manganese, bismuth, cobalt and molybdenum. The content of zinc is 0.1-10% of the catalyst mass, the total content of cooper and chrome is 0.05-15% to zinc mass, and the total content of other metals is 1.0-3.0% to the mass of zinc-copper-chrome components. Proposed method provides carrying out the process without feeding molecular hydrogen to the system with conversion of nitrobenzene up to 100% and the preferable preparing aniline and N-methylaniline depending on parameters of the process. On its base the effective manufacturing aniline and N-methylaniline can be organized using free powers of gas-phase catalytic manufactures.

EFFECT: improved preparing method.

5 cl, 1 tbl, 7 ex

The invention relates to an improved method of obtaining N-methylaniline by alkylation of nitrobenzene formaldehyde or its mixture with methanol on copper oxide catalysts at 220-260C. the Molar ratio of nitrobenzene : alkylating agent is usually 1:(2,5-6,0), and the optimum molar ratio of formaldehyde and methanol in the alkylating agent is 1:1, and formaldehyde can be used in the form of its aqueous solution
The invention relates to an improved method of allocating N-monomethylaniline from catalization N-hydroalkylation of aniline with methanol

The invention relates to an improved method of obtaining 2-methyl-2,4-diaminopentane, which is an important intermediate product, for example, as raw materials for the paint industry

The invention relates to catalysts for the reductive alkylation of 4-aminodiphenylamine acetone and hydrogen to N-isopropyl-N-phenyl-p-phenylenediamine (diafana OP, IPPD) and methods for their preparation

FIELD: catalyst preparation methods.

SUBSTANCE: invention relates to a method for preparing catalyst and to catalyst no honeycomb-structure block ceramic and metallic carrier. Preparation procedure includes preliminarily calcining inert honeycomb block carrier and simultaneously applying onto its surface intermediate coating composed of modified alumina and active phase of one or several platinum group metals from water-alcohol suspension containing, wt %: boehmite 15-30, aluminum nitrate 1-2, cerium nitrate 4-8, 25% ammonium hydroxide solution 10-20, one or several precipitate group metal salts (calculated as metals) 0.020-0.052, water-to-alcohol weight ratio being 1:5 to 1:10; drying; and reduction. Thus prepared catalyst has following characteristics: specific coating area 100-200 m2/g, Al2O3 content 5-13%, CeO2 content 0.5-1,3%, active phase (on conversion to platinum group metals) 0.12-0.26%.

EFFECT: simplified technology due to reduced number of stages, accelerated operation, and high-efficiency catalyst.

5 cl, 1 tbl, 10 ex

FIELD: catalyst preparation methods.

SUBSTANCE: method involves preparing porous carrier and forming catalyst layer by impregnation of carrier with aqueous solution of transition group metal salts followed by drying and calcination. Porous catalyst carrier is a porous substrate of organic polymer material: polyurethane or polypropylene, which is dipped into aqueous suspension of powdered metal selected from metals having magnetic susceptibility χ from 3.6·106 to 150·106 Gs·e/g: iron, cobalt, chromium, nickel, or alloys thereof, or vanadium and polyvinylacetate glue as binder until leaving of air from substrate is completed, after which carrier blank is dried at ambient temperature and then fired at 750°C in vacuum oven and caked at 900-1300°C. Caked blank is molded and then subjected to rolling of outside surface to produce carrier having variable-density structure with density maximum located on emitting area. Formation of catalyst layer is achieved by multiple impregnations of the carrier with aqueous solution of acetates or sulfates of transition group metals: iron, cobalt, chromium, nickel, or alloys thereof in alternative order with dryings at ambient temperature and calcinations to produced catalyst bed 50-80 μm in thickness. In another embodiment of invention, formation of catalyst layer on carrier is accomplished by placing carrier in oven followed by forcing transition group metal carbonate vapors into oven for 60-120 min while gradually raising oven temperature to 850°C until layer of catalyst is grown up to its thickness 50-80 μm.

EFFECT: improved quality of catalyst and reduced its hydrodynamic resistance.

8 cl, 1 tbl, 3 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to technology for preparing caprolactam by the cyclization reaction of derivatives of aminocaproic acid. Method is carried out by cyclizing hydrolysis of compound chosen from the group comprising aminocaproic acid esters or amides, or their mixtures. The process is carried out in the presence of water, in vapor phase at temperature 200-450°C in the presence of a solid catalyst comprising of aluminum oxide that comprises at least one macroporosity with pores volume corresponding to pores with diameter above 500 Å taken in the concentration 5 ml/100 g of above. Preferably, the specific square of catalyst particles is above 10 m2/g and the total volume of pores is 10 ml/100 g or above wherein pores volume corresponds to pores with diameter above 500 Å is 10 ml/100 g or above. Invention provides improving the process indices due to the improved properties of the solid catalyst.

EFFECT: improved preparing method.

5 cl, 2 ex

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