Light paraffin oxidative dehydrogenation process

FIELD: petrochemical processes.

SUBSTANCE: feed stream is passed with admixed oxygen and diluent through catalyst bed at 400-500°C and constant flow rate 50 mL/min, said catalyst being catalytic system for heterogeneous reactions and representing geometrically structured system including microfibers of high-silica fibrous carrier, which is characterized by presence in IR absorption band of hydroxyl groups with wave number ν=3620-3650 cm-1 and half-width 65-75 cm-1. The carrier has specific surface as measured according to BET method from heat desorption of argon SAr=0.5-30 m2/g, surface area as measured by alkali titration method SNa=5-150 m2/g at ratio SNa/SAr=5-50, and at least one active element, whose principal portion is composed in the form of charged either metallic, or bimetallic clusters characterized in UV-vis diffuse reflection spectrum by specific bands in the region 34000-42000 cm-1 and ratio of integral intensity of band attributed to charged either metallic, or bimetallic clusters to integral intensity of band belonging to, respectively, either metallic, or bimetallic particles is not less than 1.0.

EFFECT: increased choice of oxidative dehydrogenation catalysts.

4 cl, 5 ex

 

The invention relates to the field of chemistry, and in particular to methods of oxidative dehydrogenation of light paraffins.

Research towards developing the process of oxidative dehydrogenation of light paraffins, is based on the fact that the chemical industry largely depends on the availability of raw materials containing propylene and other olefins. For example, according to official estimates, the demand for propylene has increased by 4.5% annually between 1991 and 2000.

The olefins produced by thermal cracking of hydrocarbons by dehydrogenation and oxidative dehydrogenation of paraffins. Catalytic oxidative dehydrogenation (AR) is the most attractive method of producing olefins for several reasons. In contrast to thermal cracking, catalytic OD process is thermodynamically allowed at low temperatures. In addition, in contrast to catalytic dehydrogenation, oxidative dehydrogenation minimum deactivation of the catalyst due to coking due to the presence of oxygen in the initial reaction mixture.

There is a method of oxidative dehydrogenation of light paraffins, namely ethane, using a catalyst consisting of a mixture of oxides of molybdenum, vanadium and transition metal (E.M. Thorsteinson et al., "The Oxidative Dehydrogenatio of Ethane over Catalyst Containing Mixed oxide of Molybdenum and Vanadium," J. Catalysis, 1978, v.52, p.116).

There is also known a method of oxidative dehydrogenation of light paraffins, in which the use of vanadium oxide catalysts supported on alumina, the composition of which is determined by the formula MV and MVSb, where M is Ni, Co, Bi and Sn (R.Juarez Lopez et al., "Oxidative Dehydrogenation of Ethane on Supported Vanadium-Containing Oxides," Applied Catalysis A: General, 1995, v.124, p.281).

There is also known a method of oxidative dehydrogenation of light paraffins, which use a catalyst containing nenalezena oxides of iron, cobalt and Nickel, that are active in the oxidative dehydrogenation of ethane (Y.Schuurman et al., "Low Temperature Oxidative Dehydrogenation of Ethane over Catalysts Based on Group VIII Metals," 1997, Applied Catalysis A: General, v.163, p.227).

The disadvantage of this method is not sufficiently high catalytic activity and its associated need for a process at a high temperature, which requires high energy consumption and leads to a low selectivity of the conversion of the original wax. These shortcomings prevent industrial use of processes on the basis of these catalysts.

The activity of oxide catalysts increases as a result of incorporating the platinum metals.

There is a method of oxidative dehydrogenation of light paraffins, mainly isobutane, n-butane, propane, including the conversion of paraffin to olefin in OUTSTA oxygen using a catalyst, consisting of a platinum group metal, is fixed on the media selected as the prototype (U.S. Patent RE37663, "Catalysis", B01J 023/00, publ. 16.04.2002). The dehydrogenation process is carried out at a temperature of about 450-550°C. the Catalyst is a Pt supported on a carrier consisting of a mixture of tin oxide and zirconium oxide. The Pt content ranges from 0.1 wt.%. up to 3 wt.%. This method of dehydrogenation of paraffins differs by one or more indicators, such as high yield of olefins, the high selectivity of the formation of olefins, low temperature reactions, the simplicity of the system and weak deactivation of the catalyst.

The disadvantage of this method is the high cost of the catalyst due to high content of platinum metal, namely platinum.

The authors sought to develop a way of oxidative dehydrogenation of light paraffins, the cost of which would be lower due to the use of a catalyst with a lower weight content of platinum, providing high yield and selectivity in oxidative dehydrogenation of light paraffins.

The task is solved in that in the method of oxidative dehydrogenation of light paraffins, comprising passing a stream of a mixture of oxygen and diluent through the catalyst bed at a temperature of 400-500°s post is annoy speed of 50 ml/min as the catalyst used for catalytic system for heterogeneous reactions, representing geometrically structured system that includes microfiber vysokokremnezemnstogo fibrous media, which is characterized by the presence in the infrared spectrum absorption band of hydroxyl groups with wave number ν=3620-3650 cm-1and full width at half maximum 65-85 cm-1has a specific surface area measured by the BET method by thermal desorption of argon, SAr=0.5-30 m2/g, the magnitude of the surface, measured by the method of alkaline titration, SNa=5-150 m2/g at a ratio of SNa/SAr=5-50, and at least one active element, the bulk of which is formed in the form of charged either metallic or bimetallic clusters, characterized in UV-visible spectrum of the diffuse reflection of specific bands in the region 34000-42000 cm-1and the ratio of the integrated intensity of the bands related to charged either metallic or bimetallic clusters, to the integrated intensity of the band related, respectively, or to the metal or bimetallic particles, not less than 1.0. When this metal clusters formed from atoms or platinum, or palladium, or rhodium, or iridium, or silver, or zirconium, or chromium, or cobalt, or Nickel, or manganese, or copper, or tin, or gold and bimetallic clusters is ture formed from a compound of palladium atoms or, or platinum atoms, or silver, or zirconium, or chromium, or cobalt, or Nickel, or manganese, or copper, or tin, or gold. In addition, microfiber vysokokremnezemnstogo fibrous media is made with a diameter of 5-20 μm, contain 50-98 .8% SiO2and at least one element selected from the group comprising the metals titanium, aluminum, iron, molybdenum, alkali, alkaline earth and rare earth elements.

The technical effect of the proposed method is that the reaction of oxidative dehydrogenation of light paraffins are at relatively low temperatures using low-cost catalyst, low cost due to low content of metals that can be used in industry.

The inventive method is carried out as follows.

For implementing the method of the original reaction mixture, containing one or more light paraffins, oxygen and diluent is passed through a bed of catalyst comprising a geometrically structured system that includes microfiber vysokokremnezemnstogo fibrous carrier and the active element. Vysokoglinozemistyj fibrous media is characterized by the presence in the infrared spectrum absorption band of hydroxyl groups with wave number ν=3620-3650 cm-1the full width at half maximum 65-75 cm -1having a specific surface area measured by the BET method by thermal desorption of argon, SAr=0.5-30 m2/g, the magnitude of the surface, measured by the method of alkaline titration, SNA=5-150 m2/g at a ratio of SNa/SAr=5-50contains 50-98 .8% SiO2and at least one element selected from the group comprising titanium, aluminum, iron, molybdenum, alkali, alkaline earth and rare earth elements. The main part of the active component is formed in the form of charged either metallic or bimetallic clusters, characterized in UV-visible spectrum of the diffuse reflection of specific bands in the region 34000-42000 cm-1and the ratio of the integrated intensity of the bands related to charged either metallic or bimetallic clusters, to the integrated intensity of the band related, respectively, or to the metal or bimetallic particles, not less than 1.0. Metal clusters are formed from atoms or platinum, or palladium, or rhodium, or iridium, or silver, or zirconium, or chromium, or cobalt, or Nickel, or manganese, or copper, or tin, or gold. And bimetallic clusters formed from compound atoms or palladium, or platinum atoms, or silver, or zirconium, or chromium, or cobalt, or Nickel, or m is of Lanza, either copper or tin, or gold.

The catalytic system is prepared by surface treatment of silica material complex compounds of metals or inorganic or organic salts of the metals. For example, in the case of palladium it can be a chloride, nitrate or sulfate, palladium (II), tetrammine palladium (II) chloride. In the case of platinum can be used platinochloride acid, tetrachloroplatinate potassium, terminationid.

Apply the usual application methods, in particular, can be used procedures impregnation, adsorption, deposition. Application procedure can be carried out once or several times. After drying the carrier with active component is subjected to heat treatment at a temperature of 100 to 600°either in air or in a stream of nitrogen, and then kept in a current of hydrogen or with hydrogen gas at a temperature of 100-300°C.

The finished catalyst system contain 0.001-0.01 wt.% platinum metal, which is significantly less than the content of platinum in the catalyst of the prototype.

Platinum metals are a big part in the form of clusters, which in the UV spectrum band in the area 34000-42000 cm-1. The presence of such clusters provides high activity of the catalytic system in oxidative dehydrogenation of paraffins.

The proposed pic is b allows for the oxidative dehydrogenation of paraffins with the formation of alkenes. Oxidative dehydrogenation is carried out in a flow reactor, placed in it by the catalytic system. Microfiber structure vysokokremnezemnstogo media simplifies the placement and fixation of the catalyst system in the reactor, provides an effective contact catalytically active surface with a stream of reactants and prevents the entrainment of particles from a flow of reactants.

In contact with a catalytic system flow of the reactants contains a gaseous paraffin or pairs of paraffin, the oxygen in the amount of 1-10% vol. and the diluent in the amount of 0-10%. The diluent may be nitrogen, hydrogen or water vapor.

The method can be carried out at a temperature of 400-500°C. Both high and too low temperature adversely affects system performance.

At low temperature catalytic system can exhibit a low activity. High temperature for adverse reactions because it causes deep oxidation of paraffins with the formation of carbon oxides and, thus, wastes paraffins.

Oxidative dehydrogenation generally proceeds at atmospheric pressure, but may be conducted at elevated pressures.

The volumetric rate of the gas mixture of 50 ml/min

The advantage of the proposed method lies in the high activity of cat the political system under reduced compared with the prototype of the content of platinum. The essential features of the proposed method make it cheaper compared to the prototype that allows to apply it in industry.

Example 1.

The way the oxidative dehydrogenation of propane carried out by passing a stream of a mixture of 95% propane and 5% oxygen through a catalyst (1 g) at a temperature of 400-500°With a constant speed50 ml/minAs the catalyst used for catalytic system for heterogeneous reactions, representing geometrically structured system that includes microfiber vysokokremnezemnstogo fibrous media with a diameter of 20 μm, composed of 97.2 wt% SiO2, 0.12 wt% Na, 1.4 wt% of Al, which is characterized by the presence in the infrared spectrum absorption band of hydroxyl groups with wave number ν=3620 cm-1and a width of 75 cm-1has a specific surface area measured by the BET method by thermal desorption of argon, SAr=1.2 m2/g, the magnitude of the surface, measured by the method of alkaline titration, SNa=5.5 m2/g at a ratio of SNa/SAr=5. The catalytic system contains 0.005 wt.% Pt, the main part of which formed a cluster with UV-visible spectrum of the diffuse reflection of a specific band with a maximum at 36000 cm-1. The ratio of the integral intensity of the band relating to the charged CL is the firewood (I cluster), to the intensity of the bands due to metal particles (Imeth)is 2 (Imeth=0,95). According to the results of chromatographic analysis of the gas at the outlet of the reactor, the yield of propylene is 7 mol.%.

The catalyst of the prototype, containing 1 wt.% Pt, under the same conditions in the oxidative dehydrogenation of propane gives the yield of propylene from 12 to 19%.

Example 2.

The way the oxidative dehydrogenation of propane carried out by passing a stream of a mixture of 95% of isobutene with 5% of oxygen through the catalyst (1 g) at a temperature of 400-500°With a constant speed of 50 ml/min. as a catalyst used in catalytic system for which the parameters of the media described in Example 1, containing 0.005 wt.% Pd and having a UV-visible spectrum of the diffuse reflection of a specific band with a maximum at 35000 cm-1. The ratio of Icluster/Imeth=1.2. The yield of isobutene is 4 mol.%.

Example 3.

The way the oxidative dehydrogenation of propane carried out by passing a stream of a mixture of 85% propane, 5% oxygen and 10% of the water through the catalyst (1 g) at a temperature of 400-500°With a constant speed of 50 ml/min. as a catalyst used in catalytic system for which the parameters of the media described in Example 1, containing 0.005 wt.% Pt and 0.002 wt.% Au and having a UV-visible spectrum of the diffuse reflection specific is aloso with a maximum at 38000 cm -1. The ratio of Icluster/Imeth=1.2. The yield of propylene is 12 mol.%.

Example 4.

The way the oxidative dehydrogenation of propane is carried out, as described in Example 1. As the catalyst used for catalytic system for which the parameters of the media described in Example 1, containing 0.005 wt.% Pt and 0.05 wt.% Cu and having a UV-visible spectrum of the diffuse reflection of a specific band with a maximum at 40500 cm-1. The ratio of Icluster/Imeth=1.2. According to the results of chromatographic analysis of the gas at the outlet of the reactor, the yield of propylene is about 13 mol.%.

Example 5.

The way the oxidative dehydrogenation of propane is carried out, as described in Example 1. As the catalyst used for catalytic system for heterogeneous reactions, representing geometrically structured system that includes microfiber vysokokremnezemnstogo fibrous media with a diameter of 5 μm, consisting of 96.2 wt.% SiO2, 0.008 wt.% Na, 0.09 wt.% Al and rare earth elements: 0.31 wt% La, 0.26 wt% Y, 0.91 wt% CE, 0.39 wt.% Pr, 0.17 wt.% Nd, 0.17 wt.% Sm, 0.69 wt.% Er, which is characterized by the presence in the infrared spectrum absorption band of hydroxyl groups with wave number ν=3650 cm-1and a width of 70 cm-1has a specific surface area measured by the BET method on a heat desorbs and argon, SAr=0.5 m2/g, the magnitude of the surface, measured by the method of alkaline titration, SNa=5 m2/g at a ratio of SNa/SAr=10, and 0.005 wt.% Pd, the main part of which formed a cluster with UV-visible spectrum of the diffuse reflection of a specific band with a maximum at 36000 cm-1. The ratio of the integral intensity of the band relating to the charged clusters (Icluster), to the intensity of the bands due to metal particles (Imeth), is 1.4.

The yield of propylene is 3 mol.%.

1. The way the oxidative dehydrogenation of light paraffins, comprising passing a stream of a mixture of oxygen and diluent through the catalyst bed at a temperature of 400-500°With a constant speed of 50 ml/min, characterized in that the catalyst used for catalytic system for heterogeneous reactions, representing geometrically structured system that includes microfiber vysokokremnezemnstogo fibrous media, which is characterized by the presence in the infrared spectrum absorption band of hydroxyl groups with the wave number v=3620-3650 cm-1and the width of 65-75 cm-1having a specific surface area measured by the BET method by thermal desorption of argon, SAr=0.5 to 30 m2/g, the magnitude of the surface, measured met the house alkali titrations, SNa=5-150 m2/g at a ratio of SNa/SAr=5-50, and at least one active element, the bulk of which is formed in the form of charged either metallic or bimetallic clusters, characterized in UV-visible spectrum of the diffuse reflection of specific bands in the region 34000-42000 cm-1and the ratio of the integrated intensity of the bands related to charged either metallic or bimetallic clusters to the integrated intensity of the band related, respectively, or to the metal or bimetallic particles is not less than 1.0.

2. The way the oxidative dehydrogenation of light paraffins according to claim 1, characterized in that the metal clusters are formed from atoms or platinum, or palladium, or rhodium, or iridium, or silver, or zirconium, or chromium, or cobalt, or Nickel, or manganese, or copper, or tin, or gold.

3. The way the oxidative dehydrogenation of light paraffins according to claim 1, characterized in that the bimetallic clusters formed from compound atoms or palladium, or platinum atoms, or silver, or zirconium, or chromium, or cobalt, or Nickel, or manganese, or copper, or tin, or gold.

4. The way the oxidative dehydrogenation of light paraffins according to claim 1, wherein the microfiber vyakarnam timetogo fibrous media is made with a diameter of 5-20 μm, contain 50-98,8% SiO2and at least one element selected from the group comprising the metals titanium, aluminum, iron, molybdenum, alkali, alkaline earth and rare earth elements.



 

Same patents:

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8 cl, 4 tbl, 11 ex

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5 tbl

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1 tbl, 8 ex

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12 cl, 2 tbl

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22 cl, 2 tbl, 16 ex

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61 cl, 2 tbl, 2 dwg, 2 ex

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1 tbl, 6 ex

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9 cl, 1 dwg, 3 tbl, 7 ex

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EFFECT: the invention ensures the high activity of the produced catalytic agents.

14 cl, 3 tbl, 97 ex

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2 cl, 7 tbl, 7 ex

FIELD: organic chemistry, chemical technology, catalysts.

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EFFECT: improved preparing method.

14 cl, 1 tbl, 6 ex

The invention relates to the field of petrochemistry and oil refining and can be used in the preparation of reforming catalysts

The invention relates to the process of obtaining mixtures of hydrogen and carbon monoxide by catalytic conversion of hydrocarbons in the presence of oxygen-containing gases and/or water vapor

The invention relates to a new method for selective receipt of acetic acid and used in the catalyst

The invention relates to a method of catalytic conversion of hydrocarbons into aromatic compounds, which can be used for reforming of gasoline and the production of aromatic compounds

The invention relates to a method of preparation of the catalysts for purification of exhaust gases from nitrogen oxides, in particular gases of metallurgical production, thermal power plants

FIELD: hydrocarbon conversion processes and catalysts.

SUBSTANCE: invention, in particular, relates to selectively upgrading paraffin feedstock via isomerization. Catalyst comprises support and sulfated oxide or hydroxide of at least one of the elements of group IVB deposited thereon; a first component selected from group consisting of consisting of lutetium, ytterbium, thulium, erbium, holmium, and combinations thereof; and a second component comprising at least one platinum-group metal component. Catalyst preparation process comprises sulfating oxide or hydroxide of at least one of the elements of group IVB to form sulfated support; depositing the first component onto prepared support; and further depositing the second component. Invention also relates to hydrocarbon conversion process in presence of above-defined catalyst.

EFFECT: improved catalyst characteristics and stability in naphta isomerization process to increase content of isoparaffins.

13 cl, 2 dwg, 1 tbl

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