Catalyst, method for preparation thereof, and synthesis gas generation process

FIELD: alternative fuels.

SUBSTANCE: invention relates to catalysts and process of steam conversion of hydrocarbons to produce synthesis gas. Proposed catalyst for steam conversion of hydrocarbons contains nickel oxide (4.0-9.2%) and magnesium oxide (4.0-6.5%) supported by porous metallic nickel (balancing amount). Carrier has specific surface area 0.10-0.20 m2/g, total pore volume 0.07-0.12 cm3/g, predominant pore radius 1-30 μm, and porosity at least 40%. Described are also catalyst preparation method and generation of synthesis gas via steam conversion of hydrocarbons.

EFFECT: increased heat conductivity of catalyst resulting in stable activity in synthesis gas generation process.

8 cl, 1 tbl, 5 ex

 

The invention relates to catalysts for steam reforming of hydrocarbons, in particular methane to produce synthesis gas. Synthesis gas can be used in chemical industries, for combustion in the catalytic thermal systems, hydrogen energy, including fuel cells (SOFC).

The analysis of patent data shows that the main direction of development of catalysts for steam reforming of hydrocarbons associated with applied Nickel catalysts, including the addition of oxides of alkaline [US 3417029, 1968; RF 2194572, 2002] and alkaline earth metals [RF 1734820, 1992; SU 1502078, 1989; SU 383343, 1979; RF 2185239, 2002]introduced with the aim of improving resistance to pleodorina and increase the stability of the activity.

In publications [O.Yamasabi, K.Tomishige, K.Fujimoto "Development of highly stable Ni-catalyst for CH4steam reaction under low steam to carbon ratio". Appl. Catal. A, 136 (1996) 49; "Catalytic performance and catalyst structure of nickel-magnesia catalysts for CO2reforming of methane". J. Catal. 184 (1999) 479] it is noted that a very low ability to superusuario different Nickel catalysts obtained by reduction of Nickel oxide solid solutions of magnesium oxide.

In industrial processes, steam reforming of natural gas is widely used mixed catalysts of the type GIAP-16 and caused to type NIAP-18. The catalyst GIAP-16 is produced by mixing oxides of aluminum, barium and calcium-aluminate goal is enta in predetermined proportions with a solution of salts of Nickel, followed by pelletizing, hydrothermal processing and annealing [DSS. apothica / edited by Alamelamma. M.: Chemistry, 1986. P.71]. The catalyst NIAP-18 is produced by application of a promoted Nickel oxide at the pre-shaped ceramic carrier with a temperature of calcination 1450-1500°having the form of a ring [Vigodman, Uchpedgiz, Vnnensa, NIV, Vahdat. "Development and operation catalyst for the conversion of natural gas NIAP-18", Chem. prom. 2 (2001), 7].

For carrying out the endothermic reaction of steam reforming of hydrocarbons in need of intensive heat transfer to the reaction zone from an external source. So used, the catalyst should have high thermal conductivity. The most promising catalysts on metallic substrates. The development of catalysts with high thermal conductivity relevant to create a TE, the greatest effect which is achieved during the process of steam reforming of hydrocarbons simultaneously with the oxidation reaction of the spent anode gas containing hydrogen. When this is implemented by the combination of heat endothermic reaction of steam reforming of hydrocarbons and the exothermic oxidation of hydrogen. Above catalysts [US 3417029, 1968; RF 2194572, 2002; RF 1734820,1992; SU 1502078, 1989; SU 383343, 1979; RF 2185239, 2002; AB. apothica / ed is the Ktsia Alamannia. M.: Chemistry, 1986. P.71] prepared on the basis of ceramic substrates and have low thermal conductivity.

In the patent [SU 173375, 1965] to increase the heat transfer it is recommended that the catalyst, for example GIAP-3, fill layers with balls of steel.

Closest to the proposed catalyst is a catalyst for steam reforming of hydrocarbons containing 4.2-8.2 wt.% NiO and 3.0-6.5 wt.% MgO supported on a carrier of a porous stainless steel [RF 2268087, B01J 23/78, SW 3/38, 20.01.06]. The method of preparation of the catalyst includes a carrier impregnated with a solution of magnesium nitrate with subsequent stages of drying and calcination, then impregnated with a solution of Nickel nitrate, followed by drying and calcination. The media of porous stainless steel has a value of specific surface area of 0.10-0.15 m2/g, total pore volume - 0.09-0.12 cm3/g, predominant pore - 2-20 μm, the porosity is 45-60%. Characteristics of the catalyst prepared according to the invention prototype, in the process for production of synthesis gas from methane in the table.

The disadvantage of the catalyst is relatively low stability of activity in the reaction of steam reforming of methane, due to the formation of iron oxide under the influence of the reaction medium, blocking the active ingredient. In the catalyst, and taken after the tests in the reaction, phase Fe2About3and the product of its interaction with the MgO-MgFe2O4set rentgenograficheski.

The invention solves the problem of increasing the stability of the catalyst activity in the reaction of steam reforming of methane with the aim of obtaining synthesis gas.

The problem is solved by applying media, resistant to oxidation under the influence of the reaction medium, high conductivity, repeatable patterns, mechanical strength.

As a metal carrier proposed to use a porous Nickel metal produced from the Nickel powder by powder metallurgy technology of porous rent. This technology provides high repeatability, mechanical strength, conductivity and uniformity of the structure due to selection of powders required fractions.

Thus, the task is solved by a catalyst to produce synthesis gas steam reforming of hydrocarbons containing Nickel oxide deposited on a porous Nickel metal with modifying additive of magnesium oxide in a ratio of components in the catalyst, wt.%: Nickel oxide 4.0-9.2, magnesium oxide 4.0-6.5, metal porous Nickel - rest.

Metal porous Nickel has a value of specific surface area 0.10-0.20 m2/g, total pore volume - 0.07-0.12 cm3/g, p is obladaushi pore size - 1-30 μm, the porosity is 40-50%.

Metal porous Nickel made of powder by powder rolling.

The task is also solved by a method of preparation of a catalyst which comprises impregnating a porous support in the form of a plate thickness of 1 mm solution of magnesium nitrate with subsequent stages of drying at a temperature of 110-120°C, annealing at a temperature of 550-600°With the current of the N2or H2and then impregnated with a solution of Nickel nitrate, followed by drying at a temperature of 110-120°and annealing at a temperature of 430-450°With the current of the N2or H2. Metal porous carrier has a value of specific surface area of not less than 0.10 m2/g, a total pore volume of not less than 0.07 cm3/g, predominant pore size is 1-30 μm, the porosity is not less than 40%.

Metal porous carrier made of powder by powder rolling.

The task is also solved by a method for production of synthesis gas steam reforming hydrocarbons at a temperature of 450-850°in the presence of the above catalyst.

The resulting catalysts are characterized by high conductivity, activity and stability of activity in the reaction of steam reforming of methane at a temperature of 450-850°C.

Distinctive features of the proposed catalyst are:

1. The composition of the catalyst, vkluchaysya as a carrier metal porous Nickel, retrieved from metal powder, with a modifying additive of magnesium oxide containing, wt.%: (4.0-9.2)NiO, (3.0-6.5)MgO, and the rest-metallic porous media. Introduction to the catalyst composition of magnesium oxide helps increase the activity of the catalyst, the stability of the catalyst to superusuario, enhance the stability of the activity. Use as a carrier plates metal porous Nickel improves the stability of the catalyst activity, increases thermal conductivity, and also makes possible the manufacture of a structured block of the catalyst.

2. The nature of the porous structure of the carrier with a small total pore volume (more than 0.7 cm3/g) and the presence of major transport pore size of 1-30 μm, which increases the utilization of the active component.

The catalytic activity of the proposed catalyst define a flow-circulation method at atmospheric pressure, a temperature of 750°With a molar ratio of N2O/CH4=2, the feeding speed of the original mixture - 11.8 l/H. the Proposed catalyst was tested in the form of a plate 7 cm × 1cm × 0.1 cm (volume of 0.7 cm3). The catalytic activity is characterized by the magnitude of the rate constants, referred to the unit volume of catalyst.

Charged to the reactor 0.7 cm3catalyst, heat the tip of H 2to a temperature of 750°and recover for 1 h, and then replace the hydrogen on the reaction mixture, incubated for 1 h and performs the measurements.

The invention is illustrated by the following examples.

Example 1

Plate metal porous Nickel with a thickness of 1 mm with a value of specific surface area of 0.1 m2/g with a total pore volume 0.09 cm3/g, predominant pore 5-30 μm, a porosity of 45% is impregnated with the aqueous solution of magnesium nitrate with a concentration of 98 gMg/L. the Sample is dried at a temperature of 110-120°C, calcined at a temperature of 550-600°in a stream of hydrogen; impregnation process with a solution of magnesium nitrate with subsequent drying and calcination are repeated twice. Plate carrier with a substrate of magnesium oxide is impregnated with a solution of Nickel nitrate with a concentration of 190 GM/l, dried at a temperature of 110-120°C, calcined at a temperature of 430-450°in a stream of nitrogen and then subjected to another impregnation with a solution of Nickel nitrate, followed by drying and calcination in the same conditions as and following the first impregnation. The resulting catalyst has a composition, wt.%: 6.6 NiO, 5.0 MgO, 88.4 media.

The catalytic activity is shown in the table.

Example 2

Similar to example 1. The difference is that the operation of impregnation with a solution of Nickel nitrate is followed by drying and calcination was repeated 3 times. The resulting catalyst has a composition, wt.%: 9.2 NiO, 5.0 MgO, 85.8 media.

The catalytic activity is shown in the table.

Example 3

Similar to example 1. The difference is that after the operation of impregnation with a solution of nitrate of magnesium stage drying and calcination is carried out in a stream of nitrogen. The resulting catalyst has a composition, wt.%: 6.4 NiO, 5.0 MgO, 88.6 media.

The catalytic activity is shown in the table.

Example 4

Similar to example 1. The difference is that permeate plate metal porous Nickel with a value of specific surface area of 0.20 m2/g, predominant pore 1-10 μm, a total pore volume of 0.12 cm3/g, a porosity of 50% and that the operation of impregnation with a solution of magnesium nitrate with subsequent drying and calcination repeat 2 times. The resulting catalyst has a composition, wt.%: 7.0 NiO, 4.0 MgO, 89.0 media.

Catalytic properties shown in the table.

Example 5

Plate metal porous Nickel with a thickness of 1 mm with a value of specific surface area of 0.15 m2/g with a total pore volume of 0.07 cm3/g, predominant pore 1-15 μm, a porosity of 40% is impregnated with the aqueous solution of magnesium nitrate with a concentration of 98 gMg/L. the Sample is dried at a temperature of 110-120°C, calcined at a temperature of 550-600°in a stream of hydrogen; impregnation process p is the target magnesium nitrate, followed by drying and calcination are repeated three times. Plate carrier with a substrate of magnesium oxide is impregnated with a solution of Nickel nitrate with a concentration of 190 gNi/ml, dried at a temperature of 110-120°and calcined at a temperature of 430-450°in a stream of hydrogen. The resulting catalyst has a composition, wt.%: 4.0 NiO, MgO 6.5, 89.5 media.

The catalytic activity is shown in the table.

As can be seen from the above data, the proposed catalyst allows the process of steam reforming of hydrocarbons to produce synthesis gas with a higher stability of the activity.

Table
Catalytic properties of Nickel-containing catalysts
# exampleThe catalyst, wt.%The rate constant for the steam reforming of methane to synthesis gas, cm3(ml CT)-1c-1ATM-1
NiOMgOmediainitialafter 50 h
16.65.088.43132
29.25.085.87067
36.45.088.638 37
47.04.089.02927
54.06.589.53232
media*)3.43.1
the placeholder7.63.089.4199.8
*)comparative example; plate of porous Nickel with a value of specific surface area of 0.20 m2/g

1. Catalyst for production of synthesis gas steam reforming hydrocarbons comprising Nickel oxide, magnesium oxide and metallic porous media, wherein the media it contains resistant to oxidation under the conditions of the reaction medium porous Nickel metal.

2. The catalyst according to claim 1, characterized in that the ratio of components in the catalyst, wt.%: Nickel oxide 4,0-9,2, magnesium oxide 3,0-6,5, metal porous Nickel - rest.

3. The catalyst according to claim 1, characterized in that it is resistant to oxidation under the conditions of the reaction medium metallic porous Nickel has a value of specific surface area of 0.10-0.20 m2/g, total pore volume 0,07-0,12 cm3/g, predominant pore 1-30 μm, the porosity is not me is it 40%.

4. The catalyst according to claim 1, wherein the oxidation resistant porous metal made of Nickel powder by powder rolling.

5. The preparation method of catalyst for production of synthesis gas steam reforming hydrocarbons which comprises the impregnation of the support with a solution of magnesium nitrate with subsequent stages of drying and calcination, then impregnated with a solution of Nickel nitrate, followed by drying and calcination, characterized in that as the carrier used is resistant to oxidation under the conditions of the reaction medium porous Nickel metal, you get a catalyst of the following composition, wt.%: Nickel oxide 4,0-9,2, magnesium oxide 3,0-6,5, metal porous Nickel - rest.

6. The method according to claim 5, characterized in that the metallic porous Nickel has a value of specific surface area of 0.10-0.20 m2/g, total pore volume 0,07-0,12 cm3/g, predominant pore 1-30 μm, a porosity of not less than 40%.

7. The method according to claim 5, characterized in that the porous metal made of Nickel powder by powder rolling.

8. Method for production of synthesis gas steam reforming hydrocarbons at a temperature of 450-850°C, characterized in that the process is carried out with the use of the catalyst according to any one of claims 1 to 4 or prepared according to any one of pp.5-7.



 

Same patents:

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SUBSTANCE: proposed method is carried out at temperature of 750-900 C due to external heating of tubular furnace reaction tubes filled with catalyst; mixture of natural gas and superheated steam is fed to reaction tubes. External heating of reaction tubes filled with catalyst is first performed by burning the natural gas in air; after attaining the required mode of operation, external heating is carried out by burning the synthesis-gas fed from tubular furnace outlet to reaction tube external heating chamber. Device proposed for realization of this method includes tubular furnace with reaction tubes filled with catalyst, chamber for mixing the natural gas with superheated steam and external heating chamber for heating the reaction tubes filled with catalyst for maintenance of conversion process; heating chamber is provided with air inlet. Device is also provided with gas change-over point whose one inlet is used for delivery of natural gas fed to chamber of external heating tubular furnace reaction tubes during starting the mode of steam conversion process; other inlet of gas change-over point is used for delivery of synthesis-gas from tubular furnace outlet through distributing synthesis-gas delivery point. Device is also provided with regulator for control of delivery of synthesis-gas to reaction tube external heating chamber required for combustion.

EFFECT: enhanced economical efficiency of process.

3 cl, 1 dwg

FIELD: steam catalytic conversion of natural gas into synthesis-gas with the use of thermal and kinetic energy of synthesis-gas.

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3 cl, 1 dwg

FIELD: processing of hydrocarbon raw materials; oxidizing conversion of hydrocarbon gases into synthesis-gas.

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9 cl, 2 dwg, 11 ex

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1 tbl, 3 ex

FIELD: alternative fuels.

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6 cl, 1 tbl, 3 ex

FIELD: gas treatment.

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20 cl, 3 dwg, 8 ex

FIELD: electronic industry; petrochemical industry; other industries; plasma converters of the gaseous and liquid hydrocarbon raw and the fuels into the synthesis gas on the basis of microwave discharge.

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6 cl, 2 dwg

FIELD: petrochemical processes.

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9 cl, 2 dwg, 2 tbl

FIELD: alternate fuels.

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FIELD: chemical, petrochemical, and petroleum processing industries.

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87 ex

FIELD: alternative fuels.

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6 cl, 1 tbl, 3 ex

FIELD: petrochemical processes and catalysts.

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7 cl, 2 tbl, 7 ex

FIELD: hydrogenation-dehydrogenation catalysts.

SUBSTANCE: invention relates to a method for preparing spherical supported metal catalysts with metal content from 10 to 70%, to spherical metal catalyst, to a process of hydrogenation of aromatic compounds wherein the latter are hydrogenised using spherical metal catalyst, and to a process of hydrogenation of aromatic compounds wherein the latter are hydrogenised using spherical supported metal catalyst.

EFFECT: increased activity and selectivity of catalyst having high porosity and uniform pore size distribution.

13 cl, 5 tbl, 12 ex

FIELD: reduction-oxidation catalysts.

SUBSTANCE: invention relates to mono- and bimetallic palladium and platinum catalysts if carbon carriers that can be used in processes involving oxygen and/or hydrogen. A method for preparing catalyst is described comprising pretreatment of carbon carrier in 3-15 M nitric acid at temperature not exceeding 80°C, impregnation of resulting carrier by nitric acid solutions of chloride-free compounds of palladium and/or platinum or palladium and at least one group I metal, drying at temperature up to 105°C, decomposition at 150-350°C, and reduction in hydrogen flow at 110-350°C. Specified preparation conditions allow one to obtain fine particles of platinum group metals 1-10 nm in size localized in pores 2-20 nm in size, concentrations of deposited palladium and/or platinum being 3 to 50 wt % or palladium and/or platinum and silver 0.1 to 1.4 wt %. Catalyst is suitable for use in processes of oxidation of alcohols into aldehydes and carboxylic acids; hydrogenation of olefin, acetylene, and diene bonds in aliphatic and carbocyclic compounds; hydrogenation of nitro compounds into amines or intermediate compounds; disproportionation of abietic and other resin acids contained in colophony and similar natural- or artificial-origin mixtures.

EFFECT: augmented assortment of redox catalysts and optimized methods of preparation thereof.

8 cl, 1 tbl, 34 ex

FIELD: chemical industry; non-ferrous metallurgy industry; other industries; methods of production of the catalyst for oxidization of the vanadium oxide particles in the gaseous phase with the definite size distribution.

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EFFECT: the invention allows to achieve the high efficiency of the coating.

6 cl, 2 ex

FIELD: waste water treatment.

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EFFECT: enhanced phenol oxidation activity of catalyst, simplified catalyst preparation technology needing utilization of lesser amounts of expensive chemicals.

3 cl, 3 tbl, 18 ex

FIELD: petroleum processing catalysts.

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EFFECT: increased catalytic activity and resistance of catalyst against deactivation in presence of diesel fuel hydrocarbon components and sulfur compound of thiophene and its derivatives series.

8 cl, 1 tbl, 7 ex

FIELD: oxidation catalysts.

SUBSTANCE: invention concerns preparation of heterogeneous phthalocyanine catalyst for use in liquid-phase oxidation of sulfur-containing compounds and provides a method, which involves preparing nonwoven polypropylene carrier by treating it with boiling alkaline solution of sodium peroxycarbonate, 3.2-4.6 g/L, at pH 9-10 followed by treatment cobalt phthalocyanine-disulfonate, 3.2-4.6 g/L, and final treatment, which consists in washing preliminarily treated carrier with sodium hydroxide solution in concentration 0.1-0.5 g/L.

EFFECT: increased catalytic activity up to 92% and simplified catalyst preparation procedure.

2 cl, 1 tbl, 5 ex

FIELD: petroleum processing catalysts.

SUBSTANCE: invention relates to catalysts for production of low-sulfur motor fuels and methods for preparing such catalysts. Hydrodesulfurization catalyst according to invention is characterized by pore volume 0.3-0.7 mL/g, specific surface 200-350 m2/g, and average pore diameter 9-13 nm and containing following components, wt %: cobalt compounds (calculated as CoO) 2.5-7.5, molybdenum compounds (as MoO3), citric acid 15-35, boron compounds (as B2O3) 0.5-3.0, aluminum oxide - the rest, cobalt, molybdenum, citric acid, and boron optionally being part of complex compound having different stoichiometry. Catalyst is prepared by impregnating catalyst support with impregnation solution obtained by dissolving, in water or aqueous solution, following compounds: citric acid, ammonium paramolybdate (NH4)6Mo7O24·4H2O, at least one cobalt compound, and at least boron compound, addition order and component dissolution conditions being such as to provide formation of complex compounds, whereas concentration of components in solution is selected such that catalyst obtained after drying would contain components in above-indicated concentrations.

EFFECT: maximized activity of desired reactions ensuring production of diesel fuels with sulfur level below 50 ppm.

9 cl, 8 ex

FIELD: catalysts in petroleum processing and petrochemistry.

SUBSTANCE: proposed catalyst is composed of 12.0-25.0% MoO3, 3.3-6.5% CoO, 0.5-1.0% P2O5, and Al2O3 to the balance. Catalyst preparation comprises one- or two-step impregnation of support with solution obtained by mixing solutions of ammonium paramolybdate, cobalt nitrate, phosphoric and citric acids taken at ratios P/Mo = 0.06-0.15 and citric acid monohydrate/Co = 1±0.1, or mixing solutions of ammonium paramolybdate and phosphoric acid at ratio P/Mo 0.06-0.15 and cobalt acetate followed by drying and calcination stages. Diesel fraction hydrodesulfurization process is carried out in presence of above-defined catalyst at 340-360°C and H2-to-feedstock ratio = 500.

EFFECT: intensified diesel fraction desulfurization.

7 cl, 2 tbl, 13 ex

FIELD: carbon monoxide conversion catalysts.

SUBSTANCE: invention relates to a method of preparing catalysts for middle-temperature conversion of carbon monoxide, which can be used in industry when producing nitrogen-hydrogen mix for ammonia synthesis. Preparation of catalyst for middle-temperature conversion of carbon monoxide with water steam, comprising precipitation of iron hydroxide from iron nitrate solution with ammonia-containing solvent, washing of iron hydroxide with water to remove nitrate ions, mixing with calcium and copper ions, mechanical activation of components, molding, drying, and calcination of granules, is characterized by that, in the component mixing step, lanthanum oxide is supplementary added, in which case molar ratio of components is as follows: Fe2O3/CaO/CuO/La2O3 = 1:(0.8-0.9):(0.045-0.08):(0.005-0.01).

EFFECT: increased catalytic activity and more than thrice reduced content of by-products in condensate.

1 tbl, 3 ex

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