Nicelullaby catalyst for hydrogenation of organic compounds, for mahanirvana co and co2and other processes and method thereof

 

(57) Abstract:

The invention relates to methods for nicolacopoulos catalyst used in industry for hydrogenation, for example, organic compounds, for mahanirvana co and CO2and other processes. Describes nicelullaby catalyst for hydrogenation of organic compounds, for mahanirvana co and CO2and other processes containing Nickel in an amount of 20-50 wt.%, oxide chromium (III) in an amount of 10-30 wt.%, the carrier based on alumina - else, while the catalyst containing the medium on the basis of aluminum oxide that includes at least one connection element of the group K, Na, Si, Fe, Ca in the amount of 0.001-0.5 wt.% in terms of the oxide. Also described is a method of obtaining nicolacopoulos catalyst for hydrogenation of organic compounds, for mahanirvana co and CO2and other processes, which includes a mixture of compounds of Nickel, chromium, aluminum, followed by drying, calcination and restoration to gidratirovannom compound of aluminium of the formula Al2O3nH2O, where 1,1n2,0, containing at least one compound of element of group K, Na, Si, Fe, Ca in the amount of 0.001-0.5 wt.%, islamnyj module 0,05-1,0, introducing oxygen-containing compounds of Nickel and chromium, stirred, followed by molding by extrusion, drying, calcination and recovery. The technical result - obtaining a catalyst with simplified technology with high mechanical strength and maintain high catalytic activity. 2 S. and 6 C.p. f-crystals, 3 tables.

The invention relates to methods for nicolacopoulos catalyst used in industry for hydrogenation, for example, organic compounds, for mahanirvana co and CO2and other processes.

A method of obtaining nicolacopoulos catalyst for hydrogenation (and. C. the USSR 229467, class B 01 J 37/02, 1969), for example, organic compounds by co-deposition solution of soda ash basic Nickel carbonate and hydroxides of chromium and aluminum from their nitrate salts at 50-90oC and a constant pH, followed by filtering the mixture, washing to complete absence of the nitrate ion, drying, calcination, pelletizing and recovery.

There is a method allows to obtain a catalyst with high catalytic activity, however, the existence of stages of filtration, washing to full nickelchromium catalyst for hydrogenation of organic compounds.with. The USSR 382425, IPC 01 J 37/02, 1973), where as the aluminum compounds take the fine powder of oxide or aluminum hydroxide with a particle size of not more than 50 μm.

The introduction of aluminum compounds in the form of a fine powder of a hydroxide or oxide of aluminum provides legalentity and reproducible in its properties the sediment, but is unable to escape from wastewater generated during the flushing of sediment, which is a disadvantage of the method of preparation of the catalyst.

There is a method of cooking nickelchromium catalyst for the hydrogenation of benzene by deposition of active nickelchromium composition from a solution containing Nickel nitrate and chromium compound, in the presence of the precipitator, dehydration, drying and calcining the obtained mass (RF patent 2054319, IPC B 01 J 23/86, 37/03, 1996). As chromium compounds are used chromic anhydride, and as precipitator - urea, taken in an amount of 30-60 wt. % from stoichiometric to the amount of Nickel and chromium.

The disadvantage of this method of preparation of the catalyst are high energy costs.

The closest method is a method of obtaining nicolacopoulos catalyst for hydrogenation arteriosa impurities.with. The USSR 403429, IPC B 01 J 37/04, 1977) by mixing compounds of Nickel, aluminum and chromium, followed by drying, calcination, pelletizing and restoration, in which a paste or a dry mixture of the basic Nickel carbonate and hydroxide or aluminum oxide is treated with a solution of chromium trioxide. The resulting mass is dried, calcined, mixed with graphite and tabletirujut.

The disadvantage of this catalyst is low resistance, large work (stage tabletting), the high cost.

The present invention is to obtain a catalyst with high mechanical strength and maintain high catalytic activity.

The problem is solved using nicolacopoulos catalyst for hydrogenation of organic compounds, for mahanirvana co and CO2and other processes containing Nickel in an amount of 20-50 wt.%, oxide chromium (III) in an amount of 10-30 wt.%, where the carrier on the basis of aluminum oxide contains at least one compound of element of group K, Na, Si, Fe, Ca in the amount of 0.001-0.5 wt.%.

To obtain a catalyst of high activity, it is preferable to use chromium oxide (III) with g is also solved by the proposed method of preparation of the above catalyst, where as the aluminum compounds used hydrated compound of aluminium of the formula Al2ABOUT3nH2O, where 1,1n2,0, containing at least one compound of element of group K, Na, Si, Fe, Ca in the amount of 0.001-0.5 wt.%, when mixing the components add nitric acid in a quantity of 0.05-1.0 mol NGO31 mol Al2ABOUT3(acid module is equal to 0,05-1,0), mixed, molded by extrusion, dried, calcined and restore.

To obtain a catalyst of the following composition: Ni - 45-50 wt.%, CR2ABOUT3- 24-30 wt. %, Al2ABOUT3with the content of the additional compounds else to gidratirovannom connection aluminum add nitric acid in the amount of 0.25 to 1.0 mol, NGO31 mol Al2ABOUT3(acid module is 0.25 to 1.0).

To obtain a catalyst composition: Ni - 25-41 wt.%, CR203- 10-20 wt. %, Al2ABOUT3with the content of the additional compounds else to gidratirovannom connection aluminum add nitric acid in a quantity of 0.05-0.25 mol NGO31 mol Al2ABOUT3(acid module 0,05-0,25).

The catalyst after the extrusion has the shape of a cylinder, sphere, ring. To increase the act is.

To improve the molding properties of the catalyst in the mixture is further added polyethylene oxide in an amount up to 1 wt.%, wood flour in an amount up to 5 wt.%.

A significant difference between the claimed catalyst is that the medium contains at least one compound of an element from groups: K, Na, Si, Fe, Ca in the amount of 0.001-0.5 wt.%.

In the proposed solution used for preparation of the catalyst hydrated compound of aluminium of the formula Al2ABOUT3mo2Oh, where 1,1n2,0, which can be obtained by any known means, such as rehydration product rapid dehydration hydrargillite, bayerite, nordstrandite, boehmite, Diaspora, containing in its composition optionally modifying compound K, Na, Si, Fe, Ca in the amount of 0.001-0.5 wt.%, that may be partially present in the original products, or they are introduced into the original aluminum hydroxide before rapid dehydration by any known means, for example by impregnation or coprecipitation. When the heat treatment of the granules of the catalyst on the basis of such a hydrated aluminum compounds is the formation of the catalyst on the modified surface of the carrier that provides the formation of strong ties ASS="ptx2">

This set of tools task allows to obtain a catalyst with high mechanical strength and maintain high catalytic activity, long life.

The catalyst is prepared as follows.

For the preparation of the catalyst used hydrated compound of aluminum with the gross formula Al2ABOUT3mo2Oh, where 1,1n2,0, containing at least one compound of an element from groups: K, Na, Si, Fe, Ca in the amount of 0.001-0.5 wt.%.

This compound can be obtained by any known means, for example, patent of the Russian Federation 2064435 (IPC C 01 F 7/44, 1996) or presidenial technical hydrate of alumina (C. A. Ziska. "Fundamentals methods of preparation of catalysts", ed. Nauka, Novosibirsk, 1983).

In the mixer load proposed hydrated compound, is added to the carrying out of plasticization nitric acid in a quantity of 0.05-1.0 mol HNO31 mol Al2ABOUT3(acid module is equal to 0,05-1,0), then add the active components. As oxygen-containing compounds of Nickel and chromium use any other compounds, such as Nickel nitrate, chromium oxide (III). To improve the plastic properties in the mix, is then formed by extrusion. If necessary, conduct stage of wilting, then the catalyst was dried, calcined at 400-450oWith and recover in a stream of hydrogen containing gas.

Composition and physico-chemical properties of the obtained catalyst is determined as follows:

- the content of Ni, Cr, K, Na, Si, Fe, Ca - the x-ray fluorescence method;

the crushing strength - on device MP -9;

Data on the method of preparation of the catalyst and its composition is shown in table 1.

The proposed catalyst was tested in the reaction of hydrogenation of benzene to cyclohexane. Testing is carried out in the reactor flow-circulation type.

The test results presented in table 2.

The catalyst was tested in the reaction of mahanirvana flow-circulation method.

The activity of the catalyst is determined by the reaction rate of the hydrogenation of carbon monoxide at a temperature of (1601)oC, a pressure of 0.1 MPa (1 ATM), the initial volume concentration of 1.0 to 1.5%, the volume percentage of carbon monoxide in the cycle of 0.3%.

Data test results nicolacopoulos catalyst in the reaction of mahanirvana are shown in table 3.

The invention of illustrare the Nickel, 2,03 kg aluminium hydroxide, pre-shredded in a vibrating mill, and 3.5 l of water. The mixture is stirred for 0.5-1 h at room temperature and slowly poured a solution of chromic anhydride (384 g SGAs3in 1.15 l of water). The mass is stirred for 30 min at room temperature and 2-4 h at 70-90oC.

The resulting thick mass is dried in a baking sheet at 100-130oC for 10 h, and calcined at 450oC in air for 10 h, tabletirujut with graphite, restore and Passepartout.

Example 2. In 500 ml of water is poured 285 ml NGO3(56%) and parts of the load 690 g of hydrated aluminum compounds of the formula Al2ABOUT31,8 H2Oh, containing 0.1 wt.% sodium (in terms of oxide). Next add Nickel nitrate (2.7 kg in terms of oxide), 1,075 kg of chromium oxide hexagonal structure, 0,152 kg wood flour, stirred the mass for 1 h, add 339 ml of a 5% solution of polyethylene oxide, stirred for 5 min, the mass ekstragiruyut, rolled, dried at 100-110oC, calcined at 400-450oC for 6 h, restore and Passepartout, and get the catalyst of the following composition: Ni, with 47.4 wt.%, CR2ABOUT3- 25 wt.%.

Example 3. In 90 ml of water prelaw>ABOUT31,5 H2O, treated with nitrate of iron in the amount of 0.05 wt.% in terms of Fe2ABOUT3. The mass is stirred for 10 minutes Then add Nickel nitrate in the amount of 171 g in terms of Nickel oxide, 50 g of chromium oxide rhombohedral structure with lattice parameters of ao=equal to 4.97 co=13,57 z=6, 6,7 wood flour, stirred for 10 minutes Then a lot ekstragiruyut, rolled, dried at 100-110oC, calcined at 450oC for 6 h, restore, and Passepartout, and get the catalyst of the following composition: Ni - 41,0 wt.%, CR203- 12 wt.%.

Example 4. Similar to example 2, only the acid module Mtois 1.0, before drying the catalyst provalivajut for 2 h in air, and it has the following composition: Ni and 47.0 wt.%, CR2ABOUT3- 28 wt.%.

Example 5. Similar to example 2, only the acid module Mtois 0.66, hydrated compound of aluminum contains 0.04 wt.% CaO and content of the wood flour is 5 wt.% The catalyst has the following composition: Ni - to 48.0 wt.%, CR2ABOUT3- 27 wt.%.

Example 6. Similar to example 2, only the Nickel content is 50 wt. %, the content of chromium oxide is 30 mA the example 3, only acid-module Mto0.25, hydrated compound contains aluminum to 0.12 wt.% TO2Oh and content of wood flour is 5 wt.%. The catalyst has the following composition: Ni - to 25.0 wt.%, CR2ABOUT3- 10 wt.%.

Example 8. Similar to example 3 except that the acid module Mto0.15, hydrated compound of aluminum contains 0.5 wt.% Na2Oh and the catalyst has the following composition: Ni - 41 wt.%, CR2ABOUT3- 20 wt.%.

Example 9.

Similar to example 3 except that the acid module Mtois 0.05 g, hydrated compound of aluminum contains Na2About in an amount of 0.01 wt.%, SIO, SIS2- 0.2 wt.%, the amount of wood flour is 2.5 wt.% and the catalyst has the following composition: Ni - 25 wt.%, CR2ABOUT3- 10 wt.%.

Example 10. Similar to example 7, only the Nickel content is 20 wt.%, the content of chromium oxide (III) is 25 wt.%.

Example 11. Similar to example 4, only the Nickel content of 45 wt.%, and the content of chromium oxide (III) is 24 wt.%.

Example 12. Similar to example 3 except that the content of chromium oxide (III) is 10 wt.% and acid module Mto=0,25.

The application.

Example 14. Similar to example 6, only the Nickel content is 24 wt.%.

As can be seen from the table, the proposed catalyst in contrast to the known has a high mechanical strength and activity. Using the proposed method to obtain nicolacopoulos catalyst allows to simplify the technology of its production, to increase the mechanical strength and catalytic activity of the catalysts.

1. Nicelullaby catalyst for hydrogenation of organic compounds, for mahanirvana co and CO2and other processes containing Nickel in an amount of 20-50 wt. % chromium oxide (III) in an amount of 10-30 wt. % media-based alumina - rest, characterized in that the medium contains at least one compound of an element from groups: K, Na, Si, Fe, Ca in the amount of 0.001-0.5 wt. % in terms of oxide.

2. The catalyst p. 1, characterized in that the oxide chromium (III) has a hexagonal structure with lattice parametersabout= 4,954about= 13,584 z= 6.

3. The method of obtaining nicolacopoulos catalyst for hydrogenation of organic compounds, for mahanirvana co and CO2and other processes involving the mixing of oxygen with drying, with annealing, characterized in that as the aluminum compounds used hydrated compound of aluminum A12O3nH2O, where 1,1n2,0, containing at least one compound of element of group K, Na, Si, Fe, Ca in the amount of 0.001-0.5 wt. % in terms of oxide, when mixed components add nitric acid in a quantity of 0.05-1.0 mol HNO31 mol A12ABOUT3acidic module is 0.05 to 1.0, then injected compounds of Nickel and chromium, mix the catalyst mixture, followed by molding by extrusion, drying, calcination and recovery.

4. The method according to p. 3, wherein gidratirovannom connection aluminum add nitric acid in the amount of 0.25 to 1.0 mol HNO31 mol A12ABOUT3acidic module is 0.25 to 1.0, then injected compounds of Nickel and chromium in an amount necessary to obtain a catalyst of the following composition, wt. %:

Nickel - 45-50

Oxide chromium (III) - 24-30

Media - Rest

5. The method according to p. 3, wherein gidratirovannom connection aluminum add nitric acid in a quantity of 0.05-0.25 mol HNO31 mol A12ABOUT3acidic module 0,05-0,25, then typing>/BR>Nickel - 25-41

Oxide chromium (III) 10-20

Media - Rest

6. The method according to p. 3, characterized in that the catalyst is in the form of cylinders, spheres, rings.

7. The method according to p. 3, characterized in that the catalyst mixture is further added polyethylene oxide in an amount up to 1% and/or wood flour in an amount up to 5% by weight of a catalyst mixture.

8. The method according to p. 3, characterized in that before drying the catalyst provalivajut.

 

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