The chrome-containing catalyst and method thereof (options)

 

(57) Abstract:

The invention relates to chromium catalysts and methods for their preparation used for oxidation of organic compounds, hydrogen and carbon monoxide in the gas emissions from industrial productions. The problem solved by the invention is the development of highly active chromium catalyst capable of maintaining high activity in the presence of sulfur-containing compounds with high enough, high thermal stability and contains the minimum number of CR+6and designing method thereof (options). The problem is solved using a chromium catalyst for oxidation of contained in the gas emissions of organic compounds of hydrogen and carbon monoxide, comprising compounds of chromium, the promoter, the aluminum oxide. The catalyst additionally contains at least one connection element from the group: silicon, magnesium, barium, sodium, potassium, iron, calcium, cerium, zirconium, titanium, as a promoter, the catalyst contains at least one compound of a metal selected from the group of cobalt, Nickel, iron, manganese, copper, vanadium, chromium in the catalyst is in the oxidation state of CR3+Cr6+- no more than 1, the promoter is at least one compound of a metal from the group of cobalt, Nickel, iron, manganese, copper, vanadium 5-20. At least one connection element from the group: silicon, magnesium, barium, sodium, potassium, iron, calcium, cerium, zirconium, titanium, 0.01 to 45, alumina - rest. The problem is solved by the methods of obtaining chromium catalyst for the oxidation of organic compounds, hydrogen and carbon monoxide in the gas emissions. The first method consists in mixing the components containing compounds of chromium and promoter of aluminum hydroxide with subsequent molding, drying, and calcination. The second method of preparation of the catalyst is impregnated alumina with a solution of chromium compounds, promoter, drying and calcination. The difference of the catalyst from the well-known is the low content of CR6+that does not increase during storage in air and in the period of its operation. The proposed catalyst has a high resistance to catalytic poisons, and the introduction of its promoters from the group of cobalt, Nickel, iron, manganese, copper, vanadium increases its catalytic activity. 3 S. and 9 C.p. f-crystals, 3 tab., 1 Il.

the ha catalytic processes, such as, the conversion of carbon monoxide with water vapor, the conversion of hydrocarbons, hydrogenation of alcohols, ketones, esters, nitrosoamines, combustion of fuels, dehydrogenation and polymerization of hydrocarbons, oxidation of organic compounds of hydrogen and carbon monoxide in the gas emissions from industrial productions, and can be used in chemical, petrochemical and other industries.

Ready chromium catalysts, depending on the composition and preparation conditions along with dominant content of chromium in the oxidation state (+3) there are significant quantities of highly toxic carcinogenic compounds IG6+.

Recently imposed more stringent requirements for chromium catalysts. In many countries, legislation prohibits the use and recycling of catalysts containing compounds of CR+6.

So urgent is the development of chrome-containing catalysts and methods for their production, is highly active and at the same time containing a minimum number of highly toxic components.

Known methods of preparing catalysts that use stage vétheuil from the catalyst composition, method of its preparation, operating conditions in a certain process stage of recovery can be very different.

In the patent 2098180 (IPC6B 01 J 37/04, 1997) proposed a method of obtaining a catalyst not containing CR6+and is highly active in the oxidation of organic compounds and carbon monoxide in the gas emissions. The catalyst was prepared by mixing together the compounds of copper and chromium in the desired proportions to form a homogeneous powder. Preferably as copper compounds used malachite - basic carbonate of copper (II), and chromium compounds chromium anhydride SGAs3. Copper-chromium powder is mixed with aluminum hydroxide, and then the resulting mixture was molded, dried, calcined at a temperature of 470-750oC, cooled in a current of inert gas to a temperature recovery, and processed the reducing gas mixture at a temperature of 150-300oC.

The catalyst has high activity, however, in the presence of sulfur compounds, the catalyst rapidly loses activity.

Currently under active exploration and development of new catalysts based on chromium, with wasabe (Patent US 5665322, MCP 01 D 53/50, 1997) for purification of exhaust gases containing ABOUT2, solid particles, SO2, unburned hydrocarbons and CO, use the reactor, in which the direction of gas flow place two different catalyst.

The first part consists of a catalyst with low density thickness 5-2000 μm and represents a catalyst consisting of at least one alkali metal and one or more elements from among Sn, Fe, Co, Ni, V, Nb, TA, Cr, Mo, W, Mn and Re. The second direction of gas flow portion with a higher density represents the catalyst from among Ru, Rh, Pd, Os, Ir and Pt, contributing to the conversion of solid particles, unburned hydrocarbons and CO. At the same time suppressed the formation of SO3.

In this method of cleaning exhaust gases problem cleaning WITH especially in the presence of sulfur compounds is solved through the use of two catalysts, which leads to higher process flue gases.

In addition to this approach to improve the purification of gas mixtures from SB, there is a tendency to complication of the catalyst composition.

So in the patent (US 5502019, IPC B 01 J 23/72, 1996) proposed a catalyst which comprises a mixture of oxides: Co, Mn, Al, Bi, Cr, cu, Fe, Ti, Zn, Zr, etc. where atomic With respect to other metals from 50:1 is P>o
C.

The catalyst has high activity in the oxidation process, but there are connections IG+6and additionally, the catalyst does not have a sufficiently high activity.

Known catalysts for deep oxidation of hydrocarbons (A. C. the USSR 760993, IPC B 01 J 23/86, 1980) containing the oxides of chromium and cobalt on silica carrier, which further comprises iron oxide.

The catalyst is highly stable, but contains CR6+in a large number.

Known catalysts for deep oxidation of hydrocarbons (RF Patent 2010597, IPC B 01 J 23/89, 1994), containing the oxides of chromium and cobalt in fiber, for example, silica carrier, which additionally contains copper oxide and platinum.

The disadvantage of this catalyst is that it contains an element of the platinum group, it is sensitive to catalytic poisons.

The closest solution to the claimed is the catalyst for purification of exhaust gases of industrial plants from organic and chlorinated organic compounds (RF Patent 2050976, IPC B 01 J 32/86, 1995), which contains the oxides of chromium, cobalt and zirconium oxide and aluminum carrier, and optionally sterioid cobalt - 0,5-1,0

Zirconium oxide - 0,05-0,1

The barium oxide or manganese oxide is 0.1 to 1.8

Alumina - Rest

The disadvantage of this catalyst is the low activity and high content of CR6+.

The problem solved by the present invention is the development of highly active chromium catalyst capable of maintaining high activity in the presence of sulfur-containing compounds with high enough, high thermal stability and contains the minimum number of CR+6and designing method thereof (options).

The problem is solved using a chromium catalyst for oxidation of contained in the gas emissions of organic compounds of hydrogen and carbon monoxide, comprising compounds of chromium, the promoter, the aluminum oxide. The catalyst additionally contains at least one connection element from the group: silicon, magnesium, barium, sodium, potassium, iron, calcium, cerium, zirconium, titanium in an amount of 0.01 to 45 wt.%, as a promoter, the catalyst contains at least one compound of a metal selected from the group of cobalt, Nickel, iron, manganese, copper, vanadium in an amount of 5-20 wt.%, chromium in the catalyst is in the flat the following composition (in terms of oxides), wt.%:

The chromium oxide - 5-20,

including Cr6+- No more than 1

The promoter is at least one compound of a metal from the group of cobalt, Nickel, iron, manganese, copper, vanadium - 5-20

At least one connection element from the group: silicon, magnesium, barium, sodium, potassium, iron, calcium, cerium, zirconium, titanium, 0.01 to 45.

Alumina - Rest

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

The chromium oxide - 6-10

Including Cr6+- No more than 510-3< / BR>
The cobalt oxide - 9-13

The silicon oxide - 20-45

Alumina - Rest

The precursor of aluminium oxide is preferably a product obtained by the rapid dehydration of trihydroxide aluminum and having a composition of Al2O3n N2Oh, where n=0,03 to 2.0, and containing at least one connection element from the group of sodium, potassium, iron, silicon in an amount of 0.01-2.0 wt.%.

The problem is solved by the methods of obtaining chromium catalyst for the oxidation of organic compounds, hydrogen and carbon monoxide in the gas emissions.

The first method consists in mixing the components containing compounds of chromium, promo is mixed with at least one connection element from the group of silicon, magnesium, barium, sodium, potassium, iron, calcium, cerium, zirconium, titanium in an amount of 0.01 to 45 wt.%, add connection-reducing agents, oxygen-containing compounds of chromium, the promoter is at least one compound of a metal from the group of cobalt, Nickel, iron, manganese, copper, vanadium in an amount of 5-20 wt.%, calcined at a temperature of 380-500oWith and obtain a catalyst of the following composition (in terms of oxides), wt.%:

The chromium oxide - 5-20,

including CR6+- No more than 1

The promoter is at least one compound of a metal from the group of cobalt, Nickel, iron, manganese, copper, vanadium - 5-20

At least one connection element from the group: silicon, magnesium, barium, sodium, potassium, iron, calcium, cerium, zirconium, titanium of 0.01-45

Alumina - Rest

As compounds of the reducing agents used are preferably compounds of organic or inorganic origin in the amount of 2-40 wt. %.

As a precursor of aluminum hydroxide is preferably used product rapid dehydration trihydroxide aluminum, having the composition A12O3n N2Oh, where n=0,03 to 2.0, and containing at least one connection element from the group of sodium, potassium, glands is ical acid, capable of forming water-soluble aluminum compounds.

The catalyst was calcined in a stream of inert gas (nitrogen, argon, helium) or in a stream of air with an inert gas or in vacuum, or without access of air.

The second method of preparation of the catalyst is impregnated alumina with a solution of chromium compounds, promoter, drying and calcination.

The aluminum oxide with at least one connection element from the group: silicon, magnesium, barium, sodium, potassium, iron, calcium, cerium, zirconium, titanium in an amount of 0.01 to 45 wt.% impregnated with a solution containing compounds of chromium, the promoter is at least one compound of a metal selected from the group of cobalt, Nickel, iron, manganese, copper, vanadium in an amount of 5-20 wt. %, compound-reducing agent in the amount of 2-40 wt.%, the catalyst is calcined at a temperature up to 500oWith and obtain a catalyst of the following composition (in terms of oxides), wt.%:

The chromium oxide - 5-20

including Cr6+- No more than 1

The promoter is at least one compound of a metal from the group of cobalt, Nickel, iron, manganese, copper, vanadium - 5-20

At least one connection element from the group: silicon, magnesium, barium, sodium, potassium, jelly the representatives used are preferably compounds of organic or inorganic origin in the amount of 2-40 wt. %.

The catalyst was calcined in a stream of inert gas (nitrogen, argon, helium) or in a stream of air with an inert gas or in vacuum, or without access of air.

As the precursor of aluminium oxide preferably use the product fast dehydration trihydroxide aluminum, having the composition A12O3n H2O, where n=0,03 to 2.0, and containing at least one connection element from the group of sodium, potassium, iron, silicon in an amount of 0.01-2.0 wt.%.

For the preparation of the catalyst used, the oxide or hydroxide of aluminum with at least one connection element from the group: silicon, magnesium, barium, sodium, potassium, iron, calcium, cerium, zirconium, titanium in an amount of 0.01 to 45 wt. %. As the promoter used is at least one compound of a metal selected from the group of cobalt, Nickel, iron, manganese, copper, vanadium in an amount of 5-20 wt.%. Preferably as a promoter use cobalt.

The difference of the catalyst from the well-known is the low content of CR6+that does not increase during storage in air and in the period of its operation.

The resulting catalyst has a high resistance to catalytic poisons.

The introduction of the catalyst promoter from the group of cobalt, Nickel, iron, manganese, copper, vanadium leads to increased catalytic activity of the proposed catalyst.

Active components and promoters introduced into the catalyst by any known means.

The proposed methods allow to obtain the catalyst of different composition, which can be chosen depending on the operating conditions, gas humidity, presence of impurities, etc. When implementing both methods of preparation of the catalyst no toxic gas emissions and waste water.

The introduction of the proposed catalyst compounds of an element from the group: silicon, magnesium, barium, sodium, potassium, calcium, iron, cerium, zirconium, titanium, as promoter - metal compounds from the group of cobalt, Nickel, iron, margana the resistance to catalytic poisons, increased thermostability, increased service life of the catalyst and the catalyst contains minor amounts of CR6+.

Thus, additional heat treatment of the proposed catalyst at high temperatures (see table. 3) causes a slight decrease in its activity, but also after heat treatment of the catalyst at 900oSince it is comparable with the activity of the original prototype.

The proposed catalyst maintains high catalytic activity and stability in the oxidation of a model mixture containing 0.5 vol.% propane and mixtures containing 0.5% vol. propane and 0.1 vol.% SO2compared with the prototype (see drawing).

The catalyst activity was determined on a true grain, on a flow-circulation installed in the process of deep oxidation in oxygen excess of model mixtures containing n-butane or hydrogen, or carbon monoxide.

For measure the catalytic activity of the catalyst in the oxidation of n-butane adopted by the reaction rate (cm3C4H10/Gcats) 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 matura, which is achieved 85% degree of oxidation of hydrogen or carbon monoxide. The lower the temperature reach 85% degree of oxidation, the higher the catalyst activity.

The activity and stability of catalyst with respect to catalytic poisons identified in the oxidation of a model mixture containing 0.5 vol.% propane, and a mixture containing 0.5 vol. % propane + 0,1% vol. S02in excess oxygen at a temperature of 500oWith and evaluated by the degree of oxidation of propane at the same temperature.

thermal stability of the catalyst was evaluated by the rate of the oxidation of n-butane and specific surface, after calcination of the catalyst at temperatures: 500; 600; 700; 800; 900oC.

The following examples illustrate the invention.

Example 1

For the preparation of the catalyst to 132 g of hydrated aluminum compounds of the formula Al2ABOUT3n N2Oh, where n=2,0 containing the oxide of sodium, added 96 g of silicon oxide, pre-shredded, 60 g of oxalic acid and the components are mixed. Then the mixture is injected to 16.8 g of chromium oxide, and 31.2 g of cobalt oxide, 4.8 g of wood flour and continue mixing. Plasticization of Katalizator. Then the catalyst mass is formed by extrusion in the form of rings (external diameter of 10-15 mm). Conduct stage of dropping on the air for 10-12 hours, the dried catalyst at 120oWith 6 h and calcined at 400oWith 2 hours Calcination of the catalyst is conducted without access of air (muffle furnaces).

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

The chromium oxide - 7, including SG6+= 510-4< / BR>
The cobalt oxide - 13

The silicon oxide - 40

Alumina - 40, including the sodium oxide - 0,01

Example 2

The catalyst is prepared analogously to example 1, but the catalyst mixture contains: 835,6 g of aluminum hydroxide (n = 1.5), 200 g of silicon oxide, 400 g of oxalic acid, 100 g of chromium oxide, 90 g of cobalt oxide, 20 g of wood flour. The catalyst was calcined at 380oWith the current of inert gas (argon, nitrogen, helium).

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

The chromium oxide - 10,0, including SG6+=310-3< / BR>
The cobalt oxide - 9,0

The silicon oxide - 20,0

Alumina - 61

Example 3

The catalyst is prepared analogously to example 1, but the catalyst mixture contains: 493,2 g of hydrated aluminum oxide, 450 g izmelchennogo 330 ml of an aqueous solution of a mixture of nitrogen and glacial acetic acid. Calcined catalyst at 500oC in vacuum (P = 0.2 ATM).

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

The chromium oxide - 6,0, including Cr6+=2,510-4< / BR>
The cobalt oxide is 13.0

The silicon oxide - 45,0

Alumina - 36

Example 4

The catalyst is prepared analogously to example 1, but the catalyst mixture contains: 1027,3 g of aluminum hydroxide, 0.1 g of cerium oxide, 50 g of wood flour, 100 g of urea, 50 g of chromium oxide, 70 g of copper oxide, 50 g of iron oxide, 50 g of manganese oxide, 30 g of Nickel oxide. The catalyst is calcined at a temperature of 420oWith the current of air with an inert gas (argon, nitrogen, helium).

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

The chromium oxide - 5,0, including SG6+<310-4< / BR>
The cobalt oxide - 5,0

Calcium oxide - 5,0

The barium oxide - 5,0

Zirconium oxide - 3,0

Alumina - 72

Example 8

The catalyst is prepared analogously to example 7, but first prepare 840 g refractory porous carrier with a specific surface area of 200 m2/g, the moisture capacity of 1.0 mg/ml using a hydrated compound of aluminum and silicon oxides, magnesium and calcium, which is then impregnated on capacity protochnogo solution using acetic acid salts of chromium, copper and iron (II). The share of ethanol is 25% of the total volume of impregnating solution. Calcined catalyst step at a temperature of from 150 to 500oC.

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

The chromium oxide is 9,85, including SG6+=710-4< / BR>
The copper oxide - 5,15

Iron oxide - 1,0

The silicon oxide - 20,0

Magnesium oxide - 9,0

Calcium oxide - 4,0

Alumina - 51

Example 9

The catalyst is prepared analogously to example 7, but it differs in composition, the content of the additional element and promoter.

Example 10 (prototype)

The catalyst is prepared as follows: medium (78,27 g of alumina and 58,49 g of aluminum hydroxide) in a mortar and triturated and stirred for 8-10 minutes Here to sleep, and again mix of 2.13 g of carbon dioxide cobalt, 0.15 g of zirconium dioxide and 0.29 grams of barium carbonate. Then prepare a solution of chromic acid, dissolving 37.5 g of chromic anhydride in 100 ml of distilled water. Poured this solution to a mixture of powders of alumina, aluminum hydroxide, carbon, cobalt, zirconium dioxide and barium carbonate. The resulting paste is rubbed to the elastic state and SUP>C for 6 h, then activate at 550oWith over 6 hours "Worm" crushed granules 3x4 mm

Get a catalyst of the following composition (in terms of oxides), wt.%: the chromium oxide 19; cobalt oxide 1,0; zirconium oxide is 0.1; the oxide of barium 0,15, aluminum oxide 79,75.

Data on the composition of the catalysts according to the given examples are presented in table. 1.

In table. 2 shows the test data of the inventive catalyst in the reactions of oxidation of n-butane, hydrogen and carbon monoxide. As can be seen from the table.2, the inventive catalyst has a higher catalytic activity in the above oxidation reaction and contains a much smaller amount of CR6+compared to the prototype.

In table. 3 shows the results on the study of thermal stability of the catalyst, namely the change of catalytic activity in the oxidation of n-butane and specific surface area.

The drawing shows the test results of the proposed catalyst solution in the oxidation of propane and a mixture of propane with 0,1% vol. SO2.

1. The chrome-containing catalyst for the oxidation of organic compounds, hydrogen and carbon monoxide in the gas emissions, including Soi least one connection element from the group of silicon, magnesium, barium, sodium, potassium, iron, calcium, cerium, zirconium, titanium in an amount of 0.01 to 45 wt.%, as a promoter, the catalyst contains at least one compound of a metal selected from the group of cobalt, Nickel, iron, manganese, copper, vanadium in an amount of 5-20 wt.%, chromium in the catalyst is in the oxidation state of CR3+, CR6+and the content of CR6+is not more than 1 wt.% and the catalyst has the following composition (in terms of oxides), wt.%:

The chromium oxide - 5-20

Including CR6+- No more than 1

The promoter is at least one compound of a metal from the group of cobalt, Nickel, iron, manganese, copper, vanadium - 5-20

At least one connection element from the group: silicon, magnesium, barium, sodium, potassium, iron, calcium, cerium, zirconium, titanium of 0.01-45

Alumina - Rest

2. The catalyst p. 1, characterized in that it has the following composition (in terms of oxides), wt.%:

The chromium oxide - 6-10

Including CR6+- No more than 510-3< / BR>
The cobalt oxide - 9-13

The silicon oxide - 20-45

Alumina - Rest

3. Catalyst under item 1 or 2, characterized in that the precursor of aluminium oxide is the product obtained by the rapid dehydration o at least one connection element from the group of sodium, potassium, iron, silicon.

4. The method of obtaining chromium catalyst for the oxidation of organic compounds, hydrogen and carbon monoxide in the gas emissions by mixing the components containing compounds of chromium and promoter of aluminum hydroxide with subsequent molding, drying, calcination, wherein the aluminum hydroxide is mixed with at least one connection element from the group: silicon, magnesium, barium, sodium, potassium, iron, calcium, cerium, zirconium, titanium in an amount of 0.01 to 45 wt.%, add connection-reducing agents, oxygen-containing compounds of chromium, the promoter is at least one compound of a metal from the group of cobalt, Nickel, iron, manganese, copper, vanadium in an amount of 5-20 wt.%, calcined at a temperature of 380-500oWith and obtain a catalyst of the following composition (in terms of oxides), wt.%:

The chromium oxide - 5-20

Including CR6+- No more than 1

The promoter is at least one compound of a metal from the group of cobalt, Nickel, iron, manganese, copper, vanadium - 5-20

At least one connection element from the group: silicon, magnesium, barium, sodium, potassium, iron, calcium, cerium, zirconium, titanium of 0.01-45

Alumina - Rest

5. SPO is whether inorganic origin in the amount of 2-40 wt.%.

6. The method according to p. 4, characterized in that as the precursor of aluminum hydroxide use the product fast dehydration trihydroxide having the composition of Al2O3n N2Oh, where n=0.03 to 2.0 and containing at least one connection element from the group of sodium, potassium, iron, silicon in an amount of 0.01-2.0 wt.%.

7. The method according to p. 4, characterized in that the plasticizer used organic or inorganic acid capable of forming water-soluble aluminum compounds.

8. The method according to p. 4, characterized in that the catalyst is calcined in a stream of inert gas (nitrogen, argon, helium), or in a stream of air with an inert gas or in vacuum, or without access of air.

9. The method of obtaining chromium catalyst for the oxidation of organic compounds, hydrogen and carbon monoxide in the gas emissions, including impregnation of the alumina with a solution of chromium compounds, promoter, drying and calcination, wherein the aluminum oxide with at least one connection element from the group: silicon, magnesium, barium, sodium, potassium, iron, calcium, cerium, zirconium, titanium in an amount of 0.01 to 45 wt.%, impregnated with a solution containing compounds of chromium, the promoter - who in the amount of 5-20 wt.%, compound-reducing agent, the catalyst is calcined at a temperature up to 500oWith and obtain a catalyst of the following composition (in terms of oxides), wt.%:

The chromium oxide - 5-20

Including CR6+- no more than 1

The promoter is at least one compound of a metal from the group of cobalt, Nickel, iron, manganese, copper, vanadium - 5-20

At least one connection element from the group: silicon, magnesium, barium, sodium, potassium, iron, calcium, cerium, zirconium, titanium of 0.01-45

Alumina - Rest

10. The method according to p. 9, characterized in that compounds of the reducing agent used compounds of organic or inorganic origin in the amount of 2-40 wt.%.

11. The method according to p. 9, characterized in that the catalyst is calcined in a stream of inert gas (nitrogen, argon, helium), or in a stream of air with an inert gas or in vacuum, or without access of air.

12. The method according to p. 9, characterized in that as the precursor of aluminium oxide use the product fast dehydration trihydroxide aluminum, having a composition of Al2O3n N2Oh, where n=0.03 to 2.0 and containing at least one connection element from the group of sodium, potassium, iron, silicon in the amount of

 

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