Oxidation catalyst

FIELD: process engineering.

SUBSTANCE: invention relates to oxide catalysts for catalytic processes of hydrocarbon oxidative dehydration, in particular to oxidation catalysts. Oxidation catalyst for catalytic processes of hydrocarbon oxidative dehydration based on oxides of transition metals or mixes thereof selected from the group comprising Mo, V, Te, Nb of empirical formula MoaVbTecNbd, where a, b, c, d are gram-atomic proportions of corresponding elements, represents a geometrically structured solid calcinated structure with content of lattice oxygen not below 0.4 mmole of O2/g and containing the components in the following molar ratios: molybdenum (a) - >1.00-1.50; vanadium (b) - 0.20-2.00; tellurium (c) - 0.20-1.50; niobium (d) - 0.01-1.50.

EFFECT: yield of product not lower than 1000 g per kg of catalyst at high conversion (approx 30-50%) and selectivity not worse than 95-97%.

2 ex, 1 tbl

 

The invention relates to oxide catalysts for catalytic oxidative dehydrogenation of hydrocarbons, particularly for the heterogeneous oxidation catalysts.

These catalysts are usually complex solid oxides. Catalytic oxidation with application usually takes place in two stages. First, the lattice oxygen of the oxide is captured adsorbed on the oxide surface molecule of hydrocarbon. The hydrocarbon when it is oxidized, and the oxide is regenerated, interacting with oxygen from the air and returns to its original state.

The use of catalysts to control the chemical processes of oxidative dehydrogenation of hydrocarbons is of great scientific and practical importance. In some cases, the oxidation should be complete, for example, by neutralizing WITH and hydrocarbon pollution in the exhaust gases of vehicles. More often, however, it is necessary that the oxidation was incomplete, for example, many widely used in industry processes conversion of hydrocarbons into valuable intermediates, for example, ethane into ethylene.

Known alumina catalysts coated with oxide systems of magnesium and chromium; copper and chromium; copper, magnesium and chromium; iron oxide (RU Pat. No. 2332251, CL B01D 53/86 (2006.01), publ. 27.2008.08).

Described catalyst to produce synthesis gas, containing the th as active components, a cobalt oxide, manganese oxide and barium oxide, as a carrier, a heat - resistant reinforced metalloprotein media (RU Pat. No. 2320408, CL B01J 23/84 (2006.01), publ. 2008.03.27).

Catalytic dehydrogenation of propane carried out using as catalyst an aluminum oxide or oxides of vanadium, tungsten, chromium, calcium deposited on the aluminum oxide (RU Pat. No. 2280021, CL SS 5/46 (2006.01), publ. 2006.07.20).

Described is a catalyst for the process of dehydrogenation of hydrocarbons, containing in its composition chromium oxide, alkali metal supported on a carrier. The carrier is a composite material including alumina and aluminium (EN Pat. No. 2256499, CL B01J 23/26, publ. 2005.07.20).

The claimed catalyst composition for oxidation of ethane to ethylene and/or acetic acid and/or oxidation of ethylene to acetic acid, which in combination with oxygen includes the following elements: molybdenum, vanadium, niobium and gold in the absence of palladium according to the empirical formula MoaWbAucVdNbeYf(I)in which Y represents one or more elements selected from the group including Pt, Co, Rh, Ir, Cu, Ag, Fe, Ru, Os and Ni; where a, b, C, d, e and f indicate such gram-atom ratios of the elements, where: 0<a≤b<1 and a+b=1, 10-5<≤f≤2 (RU Pat. No. 2238144, CL B01J 23/68, publ. 2004.10.20).

Acetic acid is obtained gas-phase oxidation is Tana and/or ethylene with oxygen using a catalyst, which contains the elements Mo, Pd, X and Y in combination with oxygen, the formula MoaPdbXcYdwhere X and Y have the following meanings: X is V, and optionally one or more elements selected from the group of TA, and W; Y represents Nb, Ca and Sb, and optionally one or more elements selected from the group of Bi, Cu, Ag, Au, Li, K, Rb, Cs, Mg, Sr, Ba, Zr, Hf; indices a, b, C and d denote the gram-atom ratios of the respective elements, with a=1, b=0,0001-0,01 with=0,4-1 and d=0.005 to 1 (RU Pat. No. 2245322, CL B01J 23/44, publ. 2005.01.27).

Describes a catalyst for the oxidation of ethane to ethylene with an empirical formula MoaPdbXcYdin which X denotes one or more of Cr, Mn, Nb, TA, Ti, V, Te and W; Y represents one or more of B, Al, Ga, In, Pt, Zn, Cd, Bi, Ce, Co, Rh, Ir, Cu, Ag, Au, Fe, Ru, Os, K, Rb, Cs, Mg, Ca, Sr, Ba, Nb, Zr, Hf, Ni, P, Pb, Sb, Si, Sn, Ti and U, and represents 1, b represents a number from 0.0001 to 0.01, with denotes a number from 0.4 to 1, and d denotes a number from 0,005 to 1 (RU application No. 2005126960, B01J 21/04 (2006.01), publ. 2006.04.27).

Oxidation catalysts are carriers of oxygen and operate in a cyclic mode: after the stage of obtaining the target product recovered catalyst are oxidized by air. Thus, to obtain the target product does not require pure oxygen and increases the security of the process of oxidative dehydrogenation of hydrocarbons.

The activity of the catalysts of oxidation depending on their structure and composition of the oxide is determined by the capacity of the catalyst lattice oxygen, his mobility and reaction conditions of oxidative dehydrogenation. It is established that the greatest mobility has lattice oxygen mixed oxides, in particular the catalysts based on the oxides MoVNb. The catalysts of these compounds are described in the following patents (US 4524236 (1985), JP - 10175885(1988), EP 0294845, WO-99/13980).

The disadvantage of using catalysts based on oxides MoVNb is the low selectivity of the yield of the target products (at no more than 75%) and non-industrial production the conversion of hydrocarbons (at the level of less than 20%).

The closest in composition from the above, the prototype of the present invention is the catalyst according to the patent US 7319179 - B2, CL B01J 23/00, publ. 2008.01.15).

The present invention is to develop a composition of heterogeneous oxidation catalyst based on oxides or mixed oxides of transition metals selected from the group consisting of Mo, V, Te, Nb, ensuring during the oxidative dehydrogenation of hydrocarbons yield not lower than 1000 g per kilogram of catalyst while maintaining a high conversion (at the level of 30-50%) and selectivity of not lower than 95-97%.

To solve this problem is proposed the oxidation catalyst for oxidative dehydrogenation of hydrocarbons on the basis of the oxides of transition metals selected from the group containing Mo, V, Te, Nb, (empirical formula MoaVbTecNbdwhere a-, b-, C-, d-), which is a geometrically structured calcined solid structure with a capacity of lattice oxygen not lower than 0.4 mmol About2/g and containing components in the following molar relationship:

molybdenum () - >to 1.00-1.50

vanadium (b) - 0.20-2,00

tellurium (C) - 0.20-1.50

niobium (d) - 0.01-1.50.

Unlike the prototype proposed in this invention, the oxidation catalyst has in its composition more metal promoters and is designed to perform the process of oxidative dehydrogenation of hydrocarbons in periodic mode by successive feed to the reactor at the beginning of the hydrocarbon, and then after a momentary flush of the reactor by the carrier gas introduction into the reactor of the required amount of air (oxygen).

Examples of preparation of the catalyst of the proposed structure.

Example 1

6.4 g of molybdoarsenate ammonium [(NH4)6TeMo6O247H2O] was dissolved in 20 ml of water to this solution is poured a solution of 2.37 g vanadyl sulfate in 10 ml of water. The resulting suspension is stirred for 5 minutes. Then the suspension is added a solution of 2.33 g of niobium oxalate (V) in 10 ml of water. The resulting mixture was intensively stirred for 10 minutes and transferred into the autoclave with the phone is nowym liner. The air in the autoclave displace the inert gas, the autoclave is sealed and heated to 175°C, kept at this temperature for 50 hours Then the contents of the autoclave was filtered, washed with distilled water and dried at 90°C. the Obtained active phase annealed at 600°C for 2 hours in a stream of inert gas, the heating rate is 1.67°C in minutes the Powder is then pressed and sieved to the desired fraction of fine dispersion. X-ray phase and spectral analysis identified the following relations of the elements included in the composition of the catalyst of the empirical formula MoaVbTecNbd

Molybdenum (a)>1,00
Vanadium (b)0.29
Tellurium (C)0.20
Niobium (d)0.15

Example 2

2.559 g of ammonium molybdate (NH4)6Mo7O244H2Oh was dissolved in 20 ml of water, this solution add 2.394 g teo2. In the resulting suspension under stirring to make a solution 3.260 g vanadyl sulfate in 15 ml of water. The resulting suspension is stirred for 5 minutes. Then the suspension is added a solution of 3.987 g of niobium oxalate (V) in 20 ml of water.

Receiving the ing the mixture is intensively stirred for 10 minutes and transferred into the autoclave with a Teflon liner. The air in the autoclave displace the inert gas, the autoclave is sealed and heated to 175°C, kept at this temperature for 50 hours Then the contents of the autoclave was filtered, washed with distilled water and dried at 90°C. the Obtained active phase annealed at 600°C for 2 hours in a stream of inert gas, the heating rate is 1.67°C in minutes the Powder is then pressed and sieved to the desired fraction of fine dispersion. X-ray phase and spectral analysis identified the following gram-atom ratios of the elements included in the composition of the catalyst of the empirical formula MoaVbTecNbd:

Molybdenum (a)1.50
Vanadium (b)2,00
Tellurium (C)1.50
Niobium (d1.50

The efficiency of the oxidation catalyst according to the present invention, as in the prototype (US 7319179 - B2)was determined on a sample of its use in the process of oxidative dehydrogenation of ethane with obtaining ethylene. Comparative figures are given in tables 1

Indicators of performance the STI process in the presence of an oxide catalyst based on oxides of Mo, V, Te, Nb
Number example p/pThe reaction temperature, °CThe conversion of ethane, %The selectivity for ethylene, %Performance, g2H4/g(cat) h
The prototype EP 1479438 (800 h-1)40049,169,60.1-0.2
The catalyst of the present invention (10000 h-1)40065981.0

The oxidation catalyst for oxidative dehydrogenation of hydrocarbons on the basis of the oxides of transition metals or mixtures thereof, selected from the group consisting of Mo, V, Te, Nb, empirical formula MoaVbTecNbdwhere a, b, c, d - gram-atomic ratio of the respective elements representing geometrically structured calcined solid structure with a capacity of lattice oxygen not lower than 0.4 mmol O2/g and containing components in the following molar relationship:

molybdenum (a)>1.00-1.50
vanadium (b)0.20-2.00
tellurium (C)0.20-1.50
niobium (d)0.01-1.50



 

Same patents:

FIELD: chemistry.

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FIELD: chemistry.

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19 cl, 1 tbl, 1 dwg, 2 ex

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3 cl, 1 tbl, 14 ex

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5 cl, 2 tbl, 11 ex, 1 dwg

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3 cl, 1 tbl, 2 dwg, 16 ex

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EFFECT: method improvement.

32 cl, 1 tbl, 1 ex, 3 dwg

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1 tbl

The invention relates to a method for producing vinyl acetate and a catalyst intended for use in this method

FIELD: chemistry.

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37 cl, 6 ex, 5 tbl

FIELD: chemistry.

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EFFECT: increased degree of molybdenum extraction (45,38% - 98,36%) from the worked out alkali solution independently of its composition.

1 dwg, 2 tbl, 6 ex

FIELD: chemistry.

SUBSTANCE: invention refers to the catalyst composition; to the method of its preparation and to the method of ethane and/or ethylene selective oxidation to acetic acid. The catalyst composition for ethane and/or ethylene selective oxidation to acetic acid on the carrier includes the following elements: molybdenum, vanadium, niobium and titanium in combination with oxygen corresponding to the empiric formula MoaTicVdNbeOx, where a, c, d, e are such gram-atomic element ratio whereat 0<a≤1; 0.05<c≤2; 0<d≤2; 0<e≤1 and x is element valency in the said composition. The described above catalyst composition includes the following stages: (a) preparation of the mixture containing molybdenum, vanadium, niobium and titanium in the solution; (b) drying of the obtained solid material and (c) calcination of the dried solid material with obtaining of the catalyst composition. The method of acetic acid selective preparation from the gaseous mixture containing ethane and/or ethylene includes contacting of the gaseous mixture with oxygen-containing gas at increased temperature in the presence of the described above catalyst composition.

EFFECT: increase of catalyst composition selectivity in relation to acetic acid.

22 cl, 3 tbl, 5 ex

FIELD: chemistry.

SUBSTANCE: present invention relates to mixed metal oxide oxidation catalysts and ammonolysis of propane and isobutane, methods of obtaining them and usage. Described is a mixed metal-oxide system, containing molybdenum, vanadium, niobium, antimony, germanium and oxygen or molybdenum, vanadium, tantalum, antimony, germanium and oxygen, with the following stoichiometric ratios of elements: molybdenum to antimony from 1:0.1 to approximately 1:0.5, and molybdenum to germanium from 1:>0.2 to approximately 1:1. Description is given of a catalyst, which is a mixed metal-oxide system, effective in vapour-phase conversion of propane to acrylic acid or acrylonitrile or conversion of isobutane to methacrylic acid or methacrylonitrile. The mixed metal-oxide system has an empirical formula Mo1VaNbbSbcGedOx or Mo1VaTabSbcGedOx, in which a ranges between 0.1 and 0.6, b ranges between 0.02 and 0.12, c ranges between 0.1 and 0.5, d ranges from more than 0.2 to 1, and x depends on the oxidation number of other elements in the mixed metal-oxide system. Described also is a method of obtaining the system described above, involving the following stages: addition into a reaction vessel of precursors Mo, V, Nb or Ta, Ge and Sb in an aqueous solvent to form a reaction medium with initial pH 4 or less, and optional addition of another aqueous solvent into the reaction vessel; sealing the reaction vessel; reaction of the reaction mixture at temperature above 100°C and pressure above atmospheric pressure for a period of time, sufficient for formation of a mixed metal-oxide system; optional cooling of the reaction mixture; and extraction of the mixed metal-oxide system from the reaction mixture. Description is given of a method of converting propane into acrylonitrile and isobutane into methacrylonitrile using the catalyst described above.

EFFECT: simple technology of making catalyst, increased catalyst activity and output of the target product in reactions of oxidative ammonolysis of propane and isobutane.

27 cl, 8 tbl, 50 ex, 1 dwg

FIELD: chemistry.

SUBSTANCE: described is mass of metal oxides, intended as catalyst for heterogeneously-catalysed partial oxidation and/or ammoxidation of at least one saturated and/or unsaturated hydrocarbon, of general stechiometry I MO1VaM1bM2cM3dOn (I), were M1= stands for Te; M2=stands for Nb; M3= stands for at least one of elements from group, which includes Pb, Ni, Co, Bi and Pd; a = 0.05 to 0.6, b= 0.01 to 0.5, c= 0.01 to 0.5, d = 0.0005 to 0.5 and n= equals the number determined by valence and number of different from oxygen elements in (I), whose X-ray diffractogragm has diffraction reflexes h, i and k , whose peaks are at diffraction angles (2Θ) 22.2±0.5° (h), 27.3±0.5° (i) and 28.2±0.5° (k), and - diffraction reflex h in the range of X-ray diffractogram is the most intensive and has peak half-width maximal value 0.5°, intensity Pi of diffraction reflex i and intensity Pk fulfill ratio 0.65≤R≤0.85, in which R is determined by formula R=Pi/(Pi+Pk) intensity ratio, and - half-width of diffraction reflex i and diffraction reflex k each constitute ≤1°, and at least one mass of metal oxides (I) represents such, X-ray diffractogram of which does not have diffraction reflex with peak position 2Θ=50.0±0.3°. Described is mass of metal oxides, which contains equal or more than 80 wt % of at least one mass of metal oxides, indicated above, and whose X-ray diffractogram has diffraction reflex with peak 2Θ=50.0±0.3°.Also described are methods of heterogeneously catalysed partial gas phase oxidation or ammoxidation of at least one saturated or unsaturated hydrocarbon, using as catalytic active mass at least one mass of metal oxides, described above. Described is method of obtaining metal oxides mass by mixing sources of its elementary components, calcination of dry mixture at 350-700°C and washing by organic and/or inorganic acid solution.

EFFECT: increasing target product selectivity.

17 cl, 1 tbl, 16 ex, 17 dwg

FIELD: chemistry.

SUBSTANCE: catalytic composition contains compounds of formula: Mo1VaSbbNbcMdOx, in which Mo represents molybdenum, V stands for vanadium, Sb stands for antimony, Nb stands for niobium, M represents gallium, a constitutes from 0.01 to 1, b constitutes from 0.01 to 1, c constitutes from 0.01 to 1, d constitutes from 0.01 to 1, and x is determined by requirements of valency of other present elements.

EFFECT: increase of alkane conversion degree, increase of selectivity of catalytic composition in one stage process of alkane transformation into unsaturated carbonic acid.

9 cl, 1 tbl, 12 ex

FIELD: technological processes; chemistry.

SUBSTANCE: method involves reaction of raw material containing organic component with a catalyst composition. Processing method is selected out of alkylation, acylation, hydrotreatment, demetallisation, catalytic deparaffinisation, Fischer-Tropsch process and cracking. Catalyst composition includes mainly mesoporous silicon dioxide structure containing at least 97 vol.% of pores with size in the interval from ca. 15 Å to ca. 300 Å, and at least ca. 0.01 cm3/g of micropores. Mesoporous structure features at least one catalytically and/or chemically active heteroatom in amount of at least ca. 0.02 mass %, selected out of a group including Al, Ti, V, Cr, Zn, Fe, Sn, Mo, Ga, Ni, Co, In, Zr, Mn, Cu, Mg, Pd, Ru, Pt, W and their combinations. The catalyst composition radiograph has one 0.3° to ca. 3.5° peak at 2θ.

EFFECT: highly efficient method of organic compound processing in the presence of catalyst composition without zeolite.

20 cl, 31 ex, 17 tbl, 22 dwg

FIELD: petrochemical industry; natural gas industry; manufacture of the three-dimensional catalytic nets braided in two or more layers.

SUBSTANCE: the invention is pertaining to the catalytic nets braided in two or more layers and used for the gaseous reactions. The nets are braided in two or more layers from the noble metals wire, the meshes of the separate layers are connected to each other by the interlinking threads filaments. The filling threads are inserted between the layers. The catalytic nets allow to increase activity and productivity and to use the smaller amount of the noble metal.

EFFECT: the invention ensures, that the catalytic nets allow to increase activity and productivity and to use the smaller amount of the noble metal.

15 cl, 2 dwg, 2 ex

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