The method of preparation of the catalyst based on cobalt oxide (ii)


(57) Abstract:

The method of producing catalyst based on cobalt (2) exercise by mixing powders of electrolytic cobalt and urea content of the urea in a mixture of 20 to 30 wt.%. The resulting mixture tabletirujut under pressure, after which the tablets after their discharge aluminum oxide calcined in air at 910 - 1150C to remove the urea, then after separation of the alumina pills again calcined at 1100 - 1200C. Calcined as indicated tablets cooled, impregnated with a calcium salt solution and again calcined at 300 to 800C. table 1.

The invention relates to oxide type catalysts obtained on the basis of cobalt oxide, and can be used for oxidation of carbon monoxide.

Of analogues known method of preparation of the catalyst based on oxides: cobalt (III), manganese (IV), copper (II) and silver (hopcalite catalyst) specified in the chemical encyclopedia (volume I, M.: Soviet encyclopedia, 1961, S. 987).

The method is carried out by mixing aqueous suspensions of these oxides with subsequent filtering, drying, pressing the obtained solid phase and crushing the obtained compacts the grain of certain razmutie L. Hofer J). and others in the journal "ICatalysis" [J. Catal. , 1964, 3, 5, 451]. The method is carried out by deposition of cobalt nitrate solution of potassium carbonate at 80aboutWith subsequent drying and calcining at 700aboutWith the obtained precipitate.

The disadvantage of the methods is the low strength of the resulting catalysts.

You know the more stable catalyst of cobalt oxide (II) aluminum oxide, referred to in the description of the patent France [FR. Pat., class. In 01, 1318764, 14, 1963].

The specified catalyst was prepared by impregnating pellets of aluminum oxide with a solution of cobalt nitrate, followed by drying and calcining the pellets at 550aboutC.

However, obtained at the specified way catalyst reduces its activity due to the formation of catalytically inactive cobalt aluminate.

The closest in technical essence to the claimed method is a method of obtaining a catalyst of cobalt oxide (II), magnesium oxide, described in the French patent is U.S. Pat. 1318764, Appl. 11.01.62, publ. 14.01.63.

The way the prototype includes the melting of magnesium oxide in an electric furnace; cooling the melt to a solid phase; dispersing the obtained melt to the size of the cha is the mixture with water; molding the mixture obtained under item 5 in the form of granules; drying the granules; calcining the granules at a temperature of 1500aboutC; impregnating the granules with a solution of nitrate of cobalt; drying the impregnated granules; calcining the dried pellets at a temperature of 550aboutC.

The catalyst obtained by the prototype contains cobalt oxide (II) 5% , of magnesium oxide - 95%, stable at 800aboutWith, abrasion resistant, has a surface - 0.2 m2/g, a porosity of 60%.

The disadvantage of the prototype is the low content of the active component - cobalt oxide (II).

The technical essence of the claimed method consists in the fact that a catalyst based on cobalt oxide includes the following stages mixing powders of electrolytic cobalt and urea content of the urea in a mixture of 20-30 wt. % ; molding the obtained powder mixture under pressure; a glowing molded pellets in air at a temperature of 910-1150aboutWith mixed with aluminum oxide to remove urea; the calcination calcined granules at 1100-1200aboutWithout access of air within 20-60 min; impregnation of calcined granules of a calcium salt solution; drying the impregnated granules, calcining the dried granules to complete dissolution of salt calove oxide cobalt (II) oxide content of cobalt (II) not less than 20% and with high performance.

The table below shows comparative data of the prototype and the proposed method.

As can be seen from the table, the proposed method is compared with the prototype allows to increase the content of the active component is not less than 4 times, while maintaining high operational characteristics: thermal stability and abrasion resistance.

The claimed method is as follows.

1. Prepare a mixture containing 0.76 kg of electrolytic cobalt and 0.24 kg of urea.

2. The resulting mixture was molded in the form of cylindrical tablets having a height and a diameter of 5 mm, under pressure 900-1000 .

3. Received under item (2 tablets mixed with a granular aluminum oxide in a ratio of 1:1 by weight.

4. Received on p. 3 the mixture is calcined in air at 950 25aboutTo complete burnout of urea.

5. From calcined under item 4 mixture by sifting delete previously entered in the granules of aluminum oxide.

6. Remaining after screening on p. 5 tablets calcined at 1150aboutWith without air for 30 minutes

7. Calcined under item 6 tablets impregnated with a 17% solution of calcium nitrate.

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The result is a catalyst with the following characteristics: Specific surface area of 1 m2/g bulk density of 1.9 g/cm3The porosity of 62% Mechanical tensile strength abrasion 97% of the Content in the catalyst of cobalt oxide (II) 29% of the Content in the catalyst of cobalt metal 68% of the Content in the catalyst compounds of calcium 3% of the Activity of the catalyst is the temperature of half-transformation of carbon monoxide on the catalyst in the oxidation of carbon monoxide 178aboutWith the Activity defined in the facility and under the conditions described Belov, A. A., and others in the journal "Theory. and experimental. chemistry, 1991, T. 27, No. 5, S. 591.

The METHOD of preparation of the CATALYST BASED ON COBALT OXIDE (II), comprising mixing powdered components, granulating the mixture, calcining the granules and their impregnation with a salt solution followed by heat treatment to decompose the salt and obtain the target product, wherein the mixture is subjected to electrolytic cobalt and urea content of the urea in a mixture of 20 to 30 wt.%, the resulting mixture tabletirujut under pressure, then tablets lace alumina and calcined in air at 910 - 1150oTo complete removal of urea, after which the tab is promote to room temperature and impregnated with a solution of calcium salts followed by calcination at 330 - 800oC.


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