The catalyst for deep oxidation of organic compounds and carbon monoxide in the gas emissions and the method of its production (options)

 

(57) Abstract:

The invention relates to catalysts and methods of producing the oxide catalysis. The task of the invention is the development of catalysts for deep oxidation of hydrocarbons and carbon monoxide in the gas emissions that have increased resistance to catalytic poisons and stability while maintaining high activity and durability, and methods of preparation of the catalyst (options). The claimed catalyst for deep oxidation of organic compounds and carbon monoxide in the gas emissions, including oxides of chromium, copper, aluminium oxide, an additional connection. The catalyst contains as an additional connection at least one connection element from the group: silicon, magnesium, titanium, zirconium, cerium number 2-45 wt.%, and has the following composition (in terms of oxides), wt.%: the chromium oxide 5-25; copper oxide 5-25. At least one connection element from the group: silicon, magnesium, titanium, zirconium, cerium - 2-45; aluminium oxide - rest. The catalyst may further comprise at least one connection element from the group of alkali and alkaline earth metals, silicon, iron in an amount of 0.01-2.0 wt.% (in terms of what ininii with the subsequent molding, drying, calcination. The second way of obtaining catalysts for deep oxidation of organic compounds and carbon monoxide in gas emissions is the impregnation of a carrier comprising alumina, an additional connection, a solution of chromium compounds, copper, drying, calcination. 3 S. and 9 C.p. f-crystals, 2 tab., 1 Il.

The invention relates to catalysts and methods of producing oxide catalysts used in the processes of deep oxidation of organic compounds and carbon monoxide in the gas emissions from industrial productions.

Known catalyst for purification of exhaust gases of internal combustion engines from CO, hydrocarbons, NxOyand sulfur (U.S. Pat. USA 4957896, IPC5B 01 J 21/04, 21/06, 1990). The catalyst consists of a refractory carrier consisting of Al2ABOUT3, MgO and other oxides, on which a layer of active aluminum oxide. In the active layer of aluminum oxide is a mixed oxide and/or solid solution of zirconium and cerium in a certain ratio. To improve the activity and stability of the catalyst may contain noble metals Pt, Pd, Rh.

The disadvantage of the catalyst is its low resistance to catalytically the SHA 5141912, IPC5B 01 J 23/26, B 01 J 23/34, 1992), consisting of a refractory oxide carrier Al2ABOUT3impregnated with chromium oxide or manganese oxide, or their mixture, and a catalytically effective amount of one or more metals of the Pt group.

The disadvantages of the catalyst are not high enough resistance to toxic compounds and use in the composition of the catalyst noble metals.

Known catalysts for deep oxidation of hydrocarbons and oxygen-containing compounds of exhaust gases of industrial plants (Ed. mon. THE USSR 1466785, IPC4B 01 J 23/86, B 01 D 53/36, 1989) containing chromium oxide, cobalt oxide and oxide-aluminum carrier. Optionally, the catalyst contains an oxide of zirconium, and as the carrier contains technical alumina and active aluminum hydroxide.

The disadvantage of the catalyst is that it poisoned in the presence of serosoderjaschei connections.

The closest technical solution is the method of producing a catalyst for purification of exhaust gases from organic compounds (Ed. mon. THE USSR 1295570, IPC4B 01 J 37/04, 1992), which includes a mixture of components containing compounds of, free of sulfur and containing an admixture of iron oxide in a quantity of 0.05-0.1 wt.%.

The disadvantage of this method is that the resulting catalyst does not have a sufficiently high catalytic activity, mechanical strength and resistance to catalytic poisons.

The task of the invention is the development of catalysts for deep oxidation of hydrocarbons and carbon monoxide in the gas emissions that have increased resistance to catalytic poisons and stability while maintaining high activity and durability, and methods of preparation of the catalyst (options).

The problem is solved by using a catalyst for deep oxidation of organic compounds and carbon monoxide in the gas emissions, including compounds of chromium, copper, aluminum, an additional connection. The catalyst contains as an additional connection at least one connection element from the group: silicon, magnesium, titanium, zirconium, cerium in the following ratio of components (in terms of oxides), wt.%:

The chromium oxide - 5-25

The copper oxide - 5-25

At least one connection element from the group: silicon, magnesium, titanium, zirconium, Church of the product, obtained by the rapid dehydration of trihydroxide aluminum, and having a composition of Al2ABOUT3mo2Oh, where n=0,03-2,0.

The catalyst may further comprise at least one connection element from the group of alkali and alkaline earth metals, silicon, iron in an amount of 0.01 to 2.0 (in terms of oxides), wt.%.

The catalyst preferably contains a compound of silicon in the amount of 20-45 (in terms of oxide), wt.%, and preferably has a composition in the following ratio of components (in terms of oxides), wt.%:

The chromium oxide - 9-13

The copper oxide - 8-12

The silicon oxide - 20-45

The aluminum oxide with at least one connection element from the group of alkali and alkaline earth metals, silicon, iron 0,01-2,0 - Rest

The problem is solved by the methods (variants) of obtaining the above-described catalysts for deep oxidation of organic compounds and carbon monoxide in the gas emissions.

The first method consists in mixing chromium compounds, copper, aluminum, an additional connection with the subsequent molding, drying, and calcination.

As the aluminum compounds used hydrated compound aluminum is, is AutoRAE mixed with at least one additional connection element from the group: silicon, magnesium, titanium, zirconium, cerium. In the resulting composition add oxygen-containing compounds of chromium and copper, type plasticizer to obtain a plastic mass is formed into subsequent crop has wilted granules, dried, calcined at a temperature of 500-600oWith and receive the catalyst in the following ratio of components (in terms of oxides), wt.%:

The chromium oxide - 5-25

The copper oxide - 5-25

At least one connection element from the group: silicon, magnesium, titanium, zirconium, cerium - 2-45

Alumina - Rest

As the plasticizer used organic or inorganic acid capable of forming soluble basic aluminium salts.

As a precursor to aluminum compounds used is preferably a product obtained by the rapid dehydration of trihydroxide aluminum, and having a composition of Al2ABOUT3mo2Oh, where n=0,03-2,0, and which optionally may contain at least one connection element from the group of alkali and alkaline earth metals, silicon, iron in an amount of 0.01 to 2.0 (in terms of oxides), wt.%, (for example, patent of the Russian Federation Ni and carbon monoxide in gas emissions is the impregnation of the carrier, including the connection of aluminum, an additional connection, a solution of chromium compounds, copper, drying, calcination.

As the carrier is used the composition of the aluminum compounds with at least one additional connection element from the group: silicon, magnesium, titanium, zirconium, cerium, which is impregnated with a solution containing compounds of chromium, copper, calcined impregnated carrier at a temperature of 500 to 600oC and get the catalyst in the following ratio of components (in terms of oxides), wt.%:

The chromium oxide - 5-25

The copper oxide - 5-25

At least one connection element from the group: silicon, magnesium, titanium, zirconium, cerium - 2-45

Alumina - Rest

The predecessor of the aluminium compound is preferably a product obtained by the rapid dehydration of trihydroxide aluminum and having a composition of Al2O3nH2O, where n=0,03-2,0, and which optionally may contain at least one connection element from the group of alkali and alkaline earth metals, silicon, iron in an amount of 0.01 to 2.0 (in terms of oxides), wt.%, (for example, patent of the Russian Federation 2148017 from 27.04.2000).

The proposed methods allow to obtain a catalyst different is remesa and other If you implement both methods of preparation of the catalyst no toxic gas emissions and waste water.

In the proposed solution for the preparation of the catalyst used hydrated compound of aluminum, which can be obtained by known methods: nitrate, sulfate or aluminate technologies, presidenial, thermoactivation Al(Oh)3, rapid dehydration of aluminum hydroxide (hydrargillite, technical alumina), impact of thermal processing hydrargillite etc. But to obtain the preferred catalyst is the product of the composition of Al2ABOUT3nH2O, where n=0,03 to 2.0, which is obtained by rapid dehydration of trihydroxide aluminum, has a layered x-ray amorphous structure and capable of combining with acids, soluble basic aluminium salts. This product may contain at least one connection element from the group of alkali and alkaline earth metals, silicon, iron in an amount of 0.01 to 2.0 (in terms of oxides), wt.%, (for example, patent of the Russian Federation 2148017 from 27.04.2000), which can partially be in the original product, or they are administered before a quick partial dehydration by any known method the data aluminum compounds is the formation of the catalyst on the modified surface of the aluminum compounds, that ensures the formation of strong ties aluminum compounds with other components of the catalyst, and as a result, results in a catalyst with higher performance: strength, stability.

The introduction of the proposed catalyst compounds of an element from the group: silicon, magnesium, titanium, zirconium, cerium number 2-45 (in terms of oxides), wt.%, leads to increased stability of the catalyst, resistance to catalytic poisons and increases the service life of the catalysts.

Thus, the proposed catalyst maintains high catalytic activity and stability in the reaction of deep oxidation of carbon monoxide at high water vapor content, which refer to the variety of catalytic poisons. The hydrothermal treatment of the catalyst prepared according to example 6, under the following conditions: a temperature of 450oWith, the composition of the initial reaction mixture is FROM:air:N2About=0,3:29,7:70 (vol.%) over 107 hours does not lead to a noticeable change in catalytic properties and decrease the activity of the catalyst (see drawing).

The catalyst activity was determined on the true grain flow-circulation installed in the process of deep oxide the lytic activity of the catalyst in the reaction of deep oxidation of n-butane adopted by the reaction rate (cm3C4H10/G Kats) oxidation of n-butane at 400oC. the higher the speed of reaction of complete oxidation of n-butane corresponds to a more active catalyst.

For measure the catalytic activity of the catalyst in the reaction of deep oxidation of carbon monoxide adopted the temperature at which achieved 85% degree of oxidation of carbon monoxide. The lower the temperature reach 85% degree of oxidation of carbon monoxide, the higher the catalyst activity.

The mechanical strength of the pellet crush strength by forming was determined on the device MP-9S. For measure the mechanical strength made the ultimate compressive stress, which results in the destruction of granules allocated to the conditional section.

The following examples illustrate the invention.

Example 1

For the preparation of the catalyst used 931,5 g of hydrated aluminum compounds composition of Al2ABOUT3mo2Oh, where n=2.0 to add to the connection of aluminum 10 g of wood flour and as additional connections 20 g of oxygen-containing compounds of zirconium (zirconium oxide) and stirred. Then the composition is administered 328,9 g of oxygen-containing compounds of chromium is of mponents. Plasticization of the catalyst mixture is conducted 574 ml of an aqueous solution of nitric acid at a rate of 0.1 mole of nitric acid per mole of alumina (52,5 ml HNO3the concentration of 800 g/l), is then formed by extrusion of granules with a diameter of 4.5 mm carried out the stage of wilting on the air for 10-12 hours, dried at 120oWith 6 hours and calcined at 600oWith 4 hours.

The proposed catalyst has the following composition (in terms of oxides), wt.%:

The chromium oxide - 25,0

The copper oxide - 5,0

Zirconium oxide - 2,0

Alumina - Rest

According to x-ray analysis of the catalyst composition is a structure, including simple and complex oxides of the elements and oxygen-containing compounds of several elements (aluminum, copper, zirconium, chromium) with the structure of solid solutions.

Example 2

822 g of hydrated aluminum compounds composition of Al2ABOUT3mo2Oh, where n= 1.5, mixed with 10 g of polyethylene oxide and additional compounds: 80 g of magnesium oxide and 20 g of the cerium oxide. In the resulting composition add 65.8 g of chromium oxide, 250 g of copper oxide (obtained by thermal decomposition of basic carbonate of copper) and continue mixing. Plastification catalyst mass is formed by extrusion in the form of rings (external diameter of 10-15 mm). Conduct stage of wilting in the air, dried at 120oC and calcined at 500oC.

The proposed catalyst has the following composition (in terms of oxides), wt.%:

The chromium oxide - 5,0

The copper oxide - 25,0

Magnesium oxide - 8,0

The cerium oxide - 2,0

Alumina - Rest

The phase composition of the catalyst is a structure consisting of oxygen-containing compounds of several elements (aluminum, magnesium, copper, cerium) with the structure of solid solutions of simple and complex oxides of elements.

Example 3

The catalyst is prepared analogously to example 2, but to create a composition using 479,5 g of hydrated aluminum compounds, 10 g of wood flour, as additional connections 450 g of silicon oxide, pre-shredded. The components of the composition are thoroughly mixed, then it is injected 138,2 chromium trioxide and 95 g of copper oxide and continue mixing. Plasticization of the catalyst mixture is conducted in an aqueous solution of nitric acid based MK=0,2.

The proposed catalyst has the following composition (in terms of oxides), wt.%:

The chromium oxide - 10,5

The copper oxide - 9,5

The silicon oxide - 45,0

Nitric oxide alumina oxides of elements oxygen-containing compounds of elements (chromium, copper, aluminium) with the structure of the spinel type.

Example 4

The catalyst is prepared analogously to example 2, but to create a composition using 808,2 g of hydrated aluminum compounds containing compound of sodium, 30 g of wood flour, as an additional connection -200 g shredded silicon oxide. The components of the composition are thoroughly mixed, then it is injected 118,4 g of chromium oxide, 120 g of copper oxide and continue mixing. Plasticization of the catalyst mixture is conducted in an aqueous solution of a mixture of nitric and oxalic acids based MK=0,22.

The proposed catalyst has the following composition (in terms of oxides), wt.%:

The chromium oxide - 9,0

The copper oxide to 12.0

The silicon oxide - 20,0

Aluminum oxide - the Rest, including the sodium oxide - 0,01

The phase composition of the catalyst is a structure consisting of simple and complex oxides of the elements, oxygen-containing compounds of elements with the structure of solid solutions and the type of spinel.

Example 5

For the preparation of the catalyst used 945,2 g of hydrated aluminum compounds composition of Al2ABOUT3mo2Oh, where n=d, as an additional connection - 100 g of oxygen-containing compounds of titanium (titanium oxide) and mix thoroughly.

In the resulting composition is injected 172,2 g of chromium trioxide, of 111.2 g of basic carbonate of copper. The mixture is thoroughly mixed and plastificator aqueous solution of a mixture of formic and nitric acids based MK=0,22.

When ready catalyst mass is formed into a ring-shaped outer diameter of 15 mm extrudates provalivajut in air at room temperature for 10-12 hours, dried and subjected to a heat treatment step to a temperature of 600oC.

The proposed catalyst has the following composition (in terms of oxides), wt.%:

The chromium oxide - 13

The copper oxide - 8

The titanium oxide - 10

Aluminum oxide - the Rest, including oxides: of sodium - 0,08, potassium - 0,02, silicon - 0,9, calcium - 1,0.

According to the results of x-ray phase analysis of the composition of the catalyst is a structure comprising oxygen-containing compounds of several elements (aluminum, copper, sodium, potassium, calcium) with the structure of solid solutions and compounds of elements (aluminum, copper, chromium) with the structure of spinel and unidentified compounds.

2/g, a water capacity of 1.0 ml/g, the cylinder diameter 4.2 mm), which is then soaked in water holding capacity water solution with concentration of elements (mg/ml: chrome 110,9; copper 67,7. As chromium compounds and copper using acetic acid salt. The carrier impregnated impregnation solution was performed at room temperature in propitiated with a rotating drum dried impregnated carrier in a stream of hot air at 120oWith the calcined catalyst at a temperature of up to 550oC.

The proposed catalyst has the following composition (in terms of oxides), wt.%:

The chromium oxide is 13.0

The copper oxide - 6,8

The silicon oxide - 2,0

Alumina - Rest

The phase composition of the catalyst is a structure comprising oxygen-containing compounds of elements (copper, chromium, aluminum) with the structure of the spinel type, simple and complex oxides of elements.

Example 7

Using 438,4 g of hydrated aluminum compounds composition of Al2O3mo2the silicon compound (silicon oxide), pre-crushed and 231,46 g of hydrated compounds of magnesium, a method of mixing a composition is prepared porous media (770 g) (specific surface of the carrier 205 m2/g, a water capacity of 1.0 ml/g, the cylinder diameter 4.0 mm).

Then the composition of the carrier impregnated on capacity water solution with concentration of elements (mg/ml: chrome 104,85; copper 116,18. As chromium compounds and use copper oxides of the elements. The impregnated carrier was performed at room temperature with constant stirring. The wet granules are dried in a stream of hot air at temperatures up to 200oWith and subjected to the heat treatment step to a temperature of 600oC.

The proposed catalyst has the following composition (in terms of oxides), wt.%:

The chromium oxide and 11.8

The copper oxide to 11.2

The silicon oxide - 29,0

Magnesium oxide is 16.0

Aluminum oxide - the Rest, including the oxides of magnesium, 0.5 to iron 0,1, barium 0,4.

The phase composition of the catalyst is a structure including a mixed connection elements (aluminum, copper, chromium, magnesium) with the structure of the spinel type, connection elements with the structure of solid solutions implementation and complex oxides of elements.

When the UB>2O3mo2Oh, where n=1,0 containing compound of silicon. To connect aluminum add 50 g of wood flour and an additional connection - 450 g of oxygen-containing silicon compound (silicon oxide), pre-chopped, and mix thoroughly.

In the resulting composition is injected 144,74 g of oxygen-containing compounds of chromium (chromium trioxide) and 50 g of copper oxide and continue mixing. Catalyst charge plastificator aqueous solution of nitric acid based MK= 0,25. When ready from the mass by extrusion is formed into cylinders with a diameter of 4.2 mm carried out the stage of wilting in the air, dried and subjected to heat treatment at a temperature of 500oC.

The proposed catalyst has the following composition (in terms of oxides), wt.%:

The chromium oxide - 11,0

The copper oxide - 5,0

The silicon oxide - 45,0

Aluminum oxide - the Rest, including the silicon oxide 2,0

The phase composition of the catalyst is a structure, including simple and complex oxides of the elements, connection elements (copper, chromium, aluminum) with the structure of the spinel type.

Example 9

Using 547,95 g of hydrated aluminum compounds composition of Al2O3mo2Oh, desterrado silicon compound (silicon oxide) and 300 g of magnesium oxide, pre-crushed, by a method of mixing a composition is prepared refractory porous media (850 g) (specific surface area of 190 m2/g, moisture - 0.9 mg/ml, the cylinder diameter is 4.2 mm).

Then the composition of the carrier impregnated on capacity water solution with concentration of elements (mg/ml: chrome 71,55, copper 73,08. As compounds of copper and chromium use oxides of elements. The impregnated carrier was performed at room temperature with constant stirring. The wet granules are dried in a stream of hot air and calcined at a temperature of 500oC.

The proposed catalyst has the following composition (in terms of oxides), wt.%:

The chromium oxide - 8,0

The copper oxide - 7,0

The silicon oxide - 15,0

Magnesium oxide - 30,0

Aluminum oxide - the Rest, including oxides: silicon 1,0, magnesium 1,0

The phase composition of the catalyst is a structure, including simple and complex oxides of the elements, oxygen-containing compounds of elements (aluminum, copper, chromium, magnesium) with the structure of the spinel type.

Example 10 (prototype)

7,8 g basic carbonate of copper, 6.4 g of chromic anhydride, 0.33 g of barium oxide and 35.5 g of aluminum hydroxide pour 40 ml of water and stirred devout on the air 24 hours dried and calcined at 400-450oWith 6 hours.

The catalyst has the following composition, wt.%:

CR2ABOUT3- 14,5

CuO - 12,5

HLW - 2

Al3O3- Rest

Data on the composition of the catalysts, as described in the examples presented in table. 1.

In table. 2 presents data on the catalytic activity in the reaction of deep oxidation of n-butane and carbon monoxide and the mechanical strength of the inventive catalyst and the prototype. As can be seen from the table, the inventive catalyst has a higher catalytic activity in the above oxidation reaction and mechanical strength compared with the prototype.

All the prepared catalysts show high stability and resistance to catalytic poisons. Thus, the drawing shows data on the impact of the duration of hydrothermal treatment on the activity of the inventive catalyst prepared according to example 6, on reaction of deep oxidation of carbon monoxide. Despite the hard conditions of the test, the catalyst maintains high activity, stability and resistance to water vapor.

1. The catalyst for deep oxidation of organic connection is inania, characterized in that the catalyst contains as an additional connection at least one connection element from the group: silicon, magnesium, titanium, zirconium, cerium, in the following ratio of components (in terms of oxides), wt.%:

The chromium oxide - 5-25

The copper oxide - 5-25

At least one connection element from the group: silicon, magnesium, titanium, zirconium, cerium - 2-45

Alumina - Rest

2. The catalyst p. 1, characterized in that the precursor compound of aluminium is the product obtained by the rapid dehydration of trihydroxide aluminum and having a composition of Al2ABOUT3mo2Oh, where n=0,03-2,0.

3. Catalyst under item 1 or 2, characterized in that it further comprises at least one connection element from the group of alkali and alkaline earth metals, silicon, iron in an amount of 0.01 to 2.0 (in terms of oxides) wt.%.

4. The catalyst p. 1, characterized in that it contains a compound of silicon in the amount of 20-45 (in terms of oxide), wt.%.

5. The catalyst according to any one of paragraphs.1-4, characterized in that the composition has the following ratio of components (in terms of oxides), wt.%:

The chromium oxide - 9-13

The copper oxide - 8-12

Oxide earth metals silicon, iron 0,01-2,0 - Rest

6. A method of producing a catalyst for deep oxidation of organic compounds and carbon monoxide in the gas emissions by mixing chromium compounds, copper, aluminum, an additional connection with the subsequent molding, drying, and calcination, wherein as the aluminum compounds used hydrated compound of aluminum composition of Al2ABOUT3mo2Oh, where n= 0,03-2,0, capable of combining with acids, basic salts of aluminum, which is mixed with at least one additional connection element from the group: silicon, magnesium, titanium, zirconium, cerium, in the resulting composition add oxygen-containing compounds of chromium, copper, then type plasticizer to obtain a plastic mass is formed into subsequent crop has wilted granules, dried, calcined at a temperature of 500-600oWith and receive the catalyst in the following ratio of components (in terms of oxides), wt.%:

The chromium oxide - 5-25

The copper oxide - 5-25

At least one connection element from the group: silicon, magnesium, titanium, zirconium, cerium - 2-45

Alumina - Rest

7. The method according to p. 6, characterized in that the plasticizer used is ASS="ptx2">

8. The method according to p. 6, characterized in that the hydrated compound of aluminum composition of Al2ABOUT3mo2Oh, where n=0,03-2,0, further comprises at least one connection element from the group of alkali and alkaline earth metals, silicon, iron in an amount of 0.01 to 2.0 (in terms of oxides), wt.%.

9. The method according to p. 6, characterized in that the precursor compound of aluminium is the product obtained by the rapid dehydration of trihydroxide aluminum and having a composition of Al2ABOUT3mo2Oh, where n=0,03-2,0.

10. A method of producing a catalyst for deep oxidation of organic compounds and carbon monoxide in the gas emissions by impregnation of the carrier, including the connection of aluminum, an additional connection, a solution of chromium compounds, copper, drying and calcination, characterized in that as the carrier is used the composition of the aluminum compounds with at least one additional connection element from the group: silicon, magnesium, titanium, zirconium, cerium, which is impregnated with a solution containing compounds of chromium, copper, calcined impregnated carrier at a temperature of 500 to 600oWith and receive the catalyst in the following ratio of components (in terms of the group: silicon, magnesium, titanium, zirconium, cerium - 2-45

Alumina - Rest

11. The method according to p. 10, characterized in that the connection of aluminum further comprises at least one connection element from the group of alkali and alkaline earth metals, silicon, iron in an amount of 0.01 to 2.0 (in terms of oxides), wt.%.

12. The method according to p. 10, characterized in that the precursor compound of aluminium is the product obtained by the rapid dehydration of trihydroxide aluminum and having a composition of Al2ABOUT3mo2Oh, where n=0,03-2,0.

 

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