The method of preparation of granulated economedes of complete oxidation catalyst

 

(57) Abstract:

The invention relates to chemistry, namely the production of catalysts for complete oxidation of hydrocarbons. Such catalysts are used in installations for the purification of industrial gaseous emissions containing incompletely burned hydrocarbons, other organic matter and carbon monoxide, for example, for sanctuaries cleaning. Purpose: preparation of granulated catalyst for complete oxidation of the copper oxide having high strength and preserving the activity of the solid catalyst. The inventive method provides for mixing and joint grinding powders of copper oxide and a binder - ray amorphous aluminum oxide in the amount of 5-10 wt. % shaping by extrusion in the form of rings, cuttings and blocks cell structure. The method also provides for the introduction in the finished mass before forming lanthanum-containing compounds in amounts of 2 wt.% La2O3and/or magnesium-containing compound in an amount of 3 wt.% MgO based on the aluminum oxide contained in the mass. 5 C.p. f-crystals.

The invention relates to chemistry, namely the production of catalysts for complete oxidation of using hydrocarbon incompletely burned hydrocarbons, other organic substances and carbon monoxide.

In the catalytic processes complete oxidation of the organic impurities contained in industrial waste gases, along with catalysts containing noble metals, using catalysts containing copper, chromium, cobalt, manganese.

Feature of the catalytic purification of industrial gas emissions is generally low concentration of organic compounds. In this regard, the catalysts used in the processes of purification of gas emissions, should have a high specific surface. Typically, solid oxide catalysts have a low specific surface area, which reduces their effectiveness. Therefore find wide application caused the catalyst system of the carrier of the active component). However, the interaction of the active ingredient with the carrier can reduce the activity of the catalysts [1]

In addition, industry use, as a rule, granular catalysts. Granulation of powders by using a binder, which is used as water-based adhesives, aluminum oxide or silica gel. However, the introduction of nevyhodami (mineral-based) adhesives-svyset necessary strength of the catalysts.

To solve increase strength and activity use of mechanochemical activation [2], thanks to which it is possible to increase the activity and in some cases, the mechanical strength of granular catalysts.

The closest in technical essence to the present invention is a method [3] describes the preparation economedes catalyst by mechanochemical activation powder of copper oxide (malachite). The milled powder is mixed with water and molded to the screw-press in the form of cuttings, which are then dried and glue.

The invention solves the problem of making pelletized catalyst. Applies such a catalyst for purification of exhaust gases, including sunkatatithesthai method for the oxidation of hydrocarbons.

The proposed method involves the use as a binder x-ray amorphous aluminum oxide obtained by the amorphization of the gibbsite in the catalytic heat generator. This x-ray amorphous aluminum oxide (RAO) has high reactivity when interacting with water, mineral acids and alkalis [4] and can be used for the preparation of the catalyst.

Using RAO as with sdaetsa high hydration ability RAO in contact with water during cooking extrusion mass, that provides (even when the content of RAO 10 wt.) sufficient strength of the catalyst. And low maintenance RAO (not more than 10 wt.) as a binder in the extrusion mass allows you to save catalytic activity economedes catalyst.

Since the catalysts for purification of exhaust gases operate at high temperatures and possible local overheating of the granules until 1100oC, for example due to disturbances of gas-dynamic processes in the apparatus, a very important factor is thermal stability of the catalyst. It is known that in Aromamedia systems at a temperature of approximately 1000oC copper has the mineralizing action, accelerating the education - Al2O3due to the destruction spielautomat phase (copper oxide aluminum) education - Al2O3[5] This leads to a decrease both in the activity and durability of the catalyst.

In the proposed method, to prevent the mineralizing action of copper ions and increase thermal stability and mechanical strength of the catalyst mass before forming impose additional connection of lanthanum and/or magnesium calculated as 2% La2O3and/or 3% of MgO to the aluminum oxide contained in the mass.and the temperature rise of more than 700oC.

Note that the known method [6] preparation of granulated catalyst based on copper oxide with the addition in the extrusion mass as a binder of copper oxide with addition of the extrusion mass as a binder of aluminum oxide (up to 30 wt.). However, obtained in a known manner, the catalyst does not meet the requirements of catalysts for complete oxidation of working in hard modes outlined above. The best examples of the catalyst obtained by the method (6), had the strength of granules is not more than 17 kg/cm2and the activity of these catalysts in the oxidation of butane in comparable with the inventive method conditions (400oC) fell about 1.4 times compared to the massive copper oxide. Taking into account the requirements for the complete oxidation catalyst, and the problem to be solved by the invention, as the prototype of the method that you chose [3]

Distinctive features of the prototype characteristics of the proposed method are the use as a binder RAO in the amount of 5-10 wt. from the extrusion mass, and in addition, the introduction in the extrusion mass 2 mass. La2O3and/or 3 wt. MgO by weight of aluminum oxide.

Almost the way Oswestry (mechanical activation) in a ball mill for 10 seconds Then in the milled mixture was added water to obtain a plastic mass with a total moisture content Owner. = 35% Then the mass is formed on the screw press in the form of cuttings, rings or blocks of honeycomb structure, which are then dried and calcined. Upon receipt of the catalysts with enhanced thermal and mechanical stability, in mass before forming impose additional powder salt of lanthanum based on 2% of La2O3and/or salts of magnesium 3% Mg on Al2O3.

Example 1 (known way). A portion of the powder of copper oxide produced by the decomposition of the basic copper carbonate (malachite) and washed of impurities compounds sodium content of 0.03 wt. Na2O dried at 110oC for 6 h, and then dried powder of copper oxide is subjected to grinding in a planetary ball mill with the acceleration of 50g when the ratio of the mass of balls and powder 10:1 and a grinding time of 10 sec. To the milled powder add water to obtain the extrusion mass, with a total moisture content of 35 wt. A lot is made in the form of cuttings with a diameter of 4 mm screw-press. Next, the granules are dried at room temperature for 12 h at 110oC for 6 hours Heat treatment is carried out at 500oC 2 o'clock Obtain a catalyst with the following x a value of Pcf(arr)14 kg cm2, catalytic activity (stationary, the rate of oxidation of butane at temperatures 300(W300and 400oC (W400): W300102= 0,52 cm3/GS; W4001025.6 cm3/HS.

Example 2. A portion of the powder of copper oxide produced by the decomposition of the basic carbonate of copper and impurities washed from compounds of sodium, up to 0.03 wt. in Na2O, dried at 110oC for 6 h and then mixed with the sample powder rentgenoamorfnogo of aluminum oxide obtained by thermal decomposition of gibbsite in the catalytic heat generator, in the ratio of 95% CuO + 5% Al2O3. The mixture of powders is subjected to grinding in a planetary ball mill with the acceleration of 50g when the ratio of the mass of balls and powder 10:1 and a grinding time of 10 sec. Later in the obtained powder add water at the rate of receipt of the extrusion mass, with a total moisture content of 34-36 wt. mixed and molded in the cuttings with a diameter of 4 mm screw-press. Next, the granules are dried at room temperature for 12 h at 110oC 6 h, the heat treatment is carried out at 500oC for 2 hours Get the catalyst with the following characteristics: Sbeats= 28 m2/g, Pcf(arr)= 28 kg/cm2, W3002O3. Next, the mass grind analogously to example 2 and molded by extrusion in the form of rings with an external diameter of 6 mm and an inner diameter of 2 mm Pellets, dried and calcined as in example 2. Get the catalyst with the following characteristics: Sbeats= 40 m2/g, Pcf(arr)= 31 kg/cm2, W300102(fracc) of 0.43 cm3/HS, W400102(fracc) 5.0 cm3/HS.

Example 4. Mass for molding is prepared analogously to example 2, but before molding add in the mass of powder compounds of lanthanum (2 wt. La2O3Al2O3contained in the mass). The mass is formed into the form of blocks of cellular structures with dimensions: cell diameter 2-4 mm, wall thickness of 1-2 mm, the block size of 50-70 mm, Then the blocks are dried and calcined as in example 2.

Get the catalyst with the following characteristics: Sbeats= 35 m2/g, Pcf(arr)= 34 kg/cm2, W300102(fracc) of 0.48 cm3/HS, W400102(fracc) 5.6 cm3/HS.

Example 5. Mass for molding is prepared analogously to example 3, but before molding add in the mass of powder compounds of magnesium at the rate of 3% MgO Al2 dried and calcined as in example 2. The resulting catalyst with the following characteristics: Sbeats= 38m2/g, Pcf(arr)= 40 kg/cm2, W300102(fracc) 0,42 cm3/HS, W400102(fracc) 4.8 cm3/GS. Example 6. Mass for molding is prepared analogously to example 3, but before the molding mass is added powders of magnesium compounds and lanthanum rate of 3% MgO and 2% La2O3Al2O3contained in the mass. A lot is made in the form of cuttings, dried and calcined similar to examples 2 and 5. Get the catalyst with the following characteristics: Sbeats= 37m2/g, Pcf(arr)= 42 kg/cm2, W300102(fracc) of 0.48 cm3/HS, W400102(fracc) 5.5 cm3/HS.

The proposed method allows to prepare a granulated catalyst for complete oxidation of the copper oxide, the activity of which is not lower than the activity of a massive economedes catalyst, and the strength is such that it can be used in the apparatus with a fluidized bed of catalyst. As can be seen from the description of examples of embodiment, for the preparation of the catalyst of the proposed method using standard equipment.

1. The method of preparation of granulated economedes produce the mixture, forming by extrusion, characterized in that the binder used powder x-ray amorphous aluminum oxide.

2. The method according to p. 1, wherein the powder x-ray amorphous aluminum oxide is administered in an amount of not more than 15 wt.

3. The method according to p. 1, characterized in that in the finished mass before forming impose additional lanthanum-containing compound and/or magisteriate connection.

4. The method according to PP. 1 and 2, characterized in that the catalyst is formed by extrusion in the form of rings, cuttings and blocks cell structure.

5. The method according to PP. 1 and 3, characterized in that the weight of the molding is injected lanthanum-containing compound in amounts of 2 to 5 wt. from Al2O3contained in the mass, and/or magisteriate connection quantity: 2-4 wt. from Al2O3contained in the mass.

6. The method according to PP. 1 and 3, characterized in that the total content of lanthanum-containing and magnesium-containing compounds are introduced into the mass to form, does not exceed 10 wt. in terms of Al2O3.

 

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