The method of preparation of the catalyst and the catalyst for purification of exhaust gases of internal combustion engines

 

(57) Abstract:

Describes the method of preparation of the metallic bulk catalyst honeycomb structure to neutralize the harmful gas emissions, including pre-processing of the inert carrier, applied on the surface of the intermediate coating of a modified aluminum oxide and one or more catalytically active platinum group metals. At first the media, representing the unit of the Al-containing foil, annealed at a temperature of 850-920C in a stream of air or oxygen for 12-15 hours, and then apply to it the intermediate coating - modified alumina in the slurry at room temperature. Describes also the catalyst for purification of exhaust gases of internal combustion engines. The technical result - the reduction of time of technological process of applying the intermediate coating by reducing the number of process steps, reducing the additional costs of electricity and labor costs, thereby reducing the cost of catalyst and catalyst, which has high efficiency in the processes of purification of gas emissions. 2 S. and 1 C.p. f-crystals.

Isoo combustion and exhaust gases of industrial plants.

Known methods of preparing catalysts on a block of metal and ceramic media cell structure. Due to the fact that the original surface of such carriers is very small (Sbeats= 0,01 - 0,6 m2/d), catalysts based on them have low catalytic activity. The main task in the preparation of such catalysts is a creation of the media intermediate layer with a developed surface. The presence of high specific surface provides the necessary dispersion of the active components (Pt, Pd, Rh), resulting in the obtained catalysts are characterized by high catalytic activity and durability in the process of neutralization of gas emissions from toxic components.

Known catalysts for purification of gas emissions from CO, CHx, NOxin bulk carriers of cellular structure, the surface of which increases in a variety of ways.

Thus, the known method of preparing the catalyst on the carrier of the aluminium-containing alloy of iron [U.S. Pat. 4096095 USA, 1979]. This alloy is subjected to a preliminary heat treatment to form on the surface of the aluminum oxide and the oxide of the transition metal (e.g. iron oxide). Katal is this way, does not have the necessary surface area. The catalyst prepared using this method is not effective enough and durable.

Described [U.S. Pat. 2411378 Germany, 1979] the preparation method of the catalyst for purification of exhaust gases from internal combustion engines is that the metal frame is made of carbon steel without ligious additives covered with primer fibre-aluminium silicate, which is dried at 100-250oC. Then it put a layer of aluminum hydroxide, which is dried at 100-250oC and calcined at 800-1200oC. Next, the resulting layer is impregnated with one or more salts of platinum group metals and calcined. However, implementation of this method involves many stages. In addition, the intermediate annealing of the oxide coating at 1200oC leads to the formation on the surface of the carrier corundum with a small specific surface, and applying a metal carrier of carbon steel reduces the service life of the catalyst.

Known method of preparing a block of metal catalyst [U.S. Pat. 2080179 of the Russian Federation, 1997], characterized in that the intermediate coating of metal oxides (Al, Ce and others) and the catalytically active components (Pt, Pd) is applied on the source memoru in the form of longitudinal channels shirring tape and folding it into the block. The described method is quite complicated for General use, and energy-intensive. In addition, the formation of the cell structure after application of the intermediate layer and the active components leads to a mechanical deformation of the coating along the lines of bending, resulting in the coating flaking, which reduces the activity of the catalyst.

In [U.S. Pat. 4132673 USA, 1979] described a method of applying an intermediate coating of a suspension of aluminum oxide, in which dispersed particles of noble metals (Pt, Pd). This suspension is applied on an inert carrier, then remove the water during drying and calcination. However, this method does not provide strong adhesion of the coating to the surface of the inert carrier, and the damage thus particles of platinum and palladium have low catalytic activity.

In [U.S. Pat. 2005538 of the Russian Federation, 1992] described a method of applying a block on a metal carrier layer Al2O3of sodium aluminate by dissolving aluminum shavings in aqueous sodium hydroxide solution, followed by drying and calcination. After that, the carrier with the intermediate layer impregnated with an aqueous solution of Ce(NO3)2and calcined system prior to the formation of cerium oxide. Then the Ute in a stream of hydrogen.

The catalyst obtained in this way is taken as a prototype. Oxide coating it has the following characteristics: the content of Al2O3- 10-20 wt.%; specific surface 100-120 m2/g, a total pore volume of 0.3 - 0.6 m3/, However, the intermediate coating catalyst has a relatively low adhesion to the carrier and irregularity, which reduces the quality of the catalyst and its use. In addition, this method of preparation of the catalyst has the following disadvantages. First, the process of deposition of aluminum oxide on the source media is long enough (20-25 hours). Secondly, the application of cerium oxide on the surface - this is a separate stage, which further increases the time of preparation of the catalyst. Increase the duration of the technological process promotes increased energy and labor costs and, accordingly, increase the cost of the catalyst. Thirdly, the process of applying the aluminum oxide used in this method is accompanied by release gazoobraznogo hydrogen, i.e., is explosive and flammable.

The closest method of preparation of the catalyst to the claimed method is described in [U.S. Pat. 4587231 USA, 1986] (prototype method), by which zarabatyvat alumina suspension, in which the dispersed powder aluminum oxide containing cerium oxide, and cerium oxide is formed by pre-impregnation of the alumina powder of the cerium salt solution and subsequent calcination. The treated suspension media and calcined to oxide-aluminum coating applied active substances - platinum group metals. For this purpose, the intermediate coating is applied an aqueous solution of each of deposited compounds of noble metal (platinum, rhodium) separately and subjected to its thermal decomposition.

The disadvantages described above suspension method include a low adhesion coating of aluminum oxide with the original metal surface, resulting in reduced service life of the catalyst due to the detachment of the intermediate layer with the active substances. In addition, separate deposition of noble metals on the carrier with the intermediate coating significantly complicates the technology and increases the time of preparation of the catalyst.

The problem solved by the invention is an acceleration and a simplification of the preparation of block catalyst for purification of exhaust gases from internal combustion engines and industrial plants with high the th coverage by suspension polymerization, block media pre heat-treated in a stream of air (or O2to create on the surface of the aluminium-containing steel foil germinal centers of adsorption, which greatly enhances the adhesion of the subsequent intermediate layer of oxide; 2) use of the suspension of certain chemical composition, allowing for one cycle to get high-quality coating that provides a high specific surface value of the medium and the dispersion caused precious metals; 3) introduction of a stabilizing additive (CeO2directly in the composition of the suspension in the form of Ce(NO3)2that leads to a reduction in time of the process.

As the inert carrier use the ribbon of steel foil (corrugated and folded block) brand HU or HU containing about 5% aluminum. This foil is subjected to heat treatment at a temperature 850-920oC in a stream of air or oxygen during 12-15 oclock When this mode, first, the migration of Al atoms to the surface of the tape and, secondly, the oxidation of Al to Al2O3. Formed on the surface of the aluminum oxide is necessary to increase the adhesion of the intermediate layer to the surface of the steel foil. the STI its coupling with the source media.

On the thus treated carrier is applied by suspension polymerization intermediate floor. The excess suspension otdovat compressed air (or nitrogen) into the container with the suspension. The temperature of the suspension room. After this block provalivajut on the air for several hours. Then it is dried at a temperature of 100-120oC and calcined at 400-500oC in a stream of air (or nitrogen).

The suspension is an aqueous-alcoholic (e.g., ethanol) solution (the ratio of water-alcohol - 1:1), in which dispersed from 22 to 32 wt. % Al(OH)3and dissolved from 2 to 4 wt.% Al(NO3)3and from 2 to 5 wt.% Ce(NO3)2.

The use of the proposed suspension allows for once (one dive) apply to block the media from 7 to 14 wt.% aluminium oxide as an intermediate coating, which significantly reduces the time of preparation of the catalyst. Adding aluminum nitrate to the system is aimed to plastifitsirovanie suspension to the required level, for enhancing the adhesion of the intermediate layer to the surface of a metal carrier. The introduction of Ce(NO3)2directly into the suspension has the advantage that it reduces the total kolgotochki cerium, followed by drying and calcination to education CeO2or at the stage of preparation of the mixture of aluminum oxide and cerium, as described in the prototypes. The cerium oxide is the "oven" additive intermediate layer of aluminum oxide using a catalyst in terms of possible thermal shocks.

A single application of an intermediate coating on the metal block the media from the proposed suspension is quite enough for the preparation of an effective catalyst with well-adhered layer of Al2O3having developed specific surface area.

Optionally, to increase the mass of the intermediate layer, after the stage of drying the block is dipped into a slurry again and then hold the stage of wilting, drying and calcination.

After applying the intermediate layer, it is impregnated with aqueous solutions of H2PtCl6, PdCl2or RhCl3and where necessary the introduction of the catalyst of several noble metals such as Pt-Rh, Pt-Pd, Pt-Pd-Rh, the composition of the impregnating solution is injected all source connections simultaneously, which also differs from the prototype in which the impregnation of these compounds was carried out consistently with intermediate recovery. This protege labor and energy costs.

After impregnation the catalyst is dried and restore the current H2at step rise in temperature and exposure for 350-400oC for 6 h

The output for the specified parameters leads to a decrease in catalytic activity and lifetime of the catalyst. This is because, firstly, the qualitative and quantitative composition of the suspension directly related to the quality and quantity of the applied intermediate layer: coating may be too thin and then the surface is insufficiently developed to obtain a highly active catalyst, or uneven, with the possible occurrence of cracks in the process of stabilization, that will lead to the partial shedding of the coating. Secondly, the specified temperature and time settings provide the optimal values of the structural characteristics, in particular, the specific surface area of catalysts.

The invention is illustrated by the following example:

For the preparation of the catalyst used block of corrugated foil stamps HU diameter and height of 20 mm In calcining furnaces were metal block media progulivali at a temperature of 900oC in a stream of air. The duration of the process prokalivanie the nitrate aluminum - 2 wt.%, nitrate cerium - 3 wt.%, water - alcohol (1:1 ratio) - the rest. Then pulled out, blew air in excess of the channels and pravalivai in the air about 5 o'clock the Next block was dried at a temperature of 100-120oC for 2 h and subjected to heat treatment in calcining furnaces were in a stream of nitrogen at step raising the temperature at a speed of 20-30oper hour up to 450oC, maintaining at this temperature for 2 hours After that, heating was off. The block was slowly cooled in the furnace to room temperature, were unloaded and the method was determined by weighing the mass of the deposited intermediate layer, which in this case amounted to 10 wt.%. The specific surface area, determined by the method of low-temperature adsorption of nitrogen, was 125 m2/g Al2O3.

Then on the intermediate coating by impregnation inflicted active phase - platinum group metals at a rate of 0.1% Pt + 0,02% Rh in the sample. This metal block with an intermediate coating impregnated with a corresponding amount of water solutions of hexachloroplatinic acid (PVC) and rhodium chloride. The sample was dried at a temperature of 100-120oC and was reduced by hydrogen in the reducing furnace at step rise is having experienced in the oxidation of CO to CO2laboratory running the installation under the following operating conditions: gas mixture of CO, 1%, O2- 2 vol.%, the rest of the nitrogen, the volumetric rate of gas flow - 30000 h-1.

Experiments have shown that the catalytic activity in the reaction of neutralization of carbon monoxide, characterized by the temperature to reach 90% conversion of CO, 205oC.

The block samples of the catalyst were prepared on metal blocks of steel HU and HU similarly, using the claimed composition suspension: Al(OH)3- 22-32 wt.%, Al(NO3)3- 2-4 wt.%, Ce(NO3)2- 2-5 wt.%, the rest is water-ethanol in a ratio of 1:1. As the active phase was applied at 0.1% Pt or 0.1% Pt+0,02% Rh or 0.25% Pd+0,01% Rh. Measurement of the catalytic activity of the prepared samples showed that this parameter is almost not less than the value of the activity of a sample of the catalyst described in example (90% degree of conversion of CO at a temperature of 205oC).

T. O. the inventive method can significantly reduce the time of the technological process of applying the intermediate coating by reducing the number of process steps, to avoid additional costs of electroen the high efficiency in the processes of purification of gas emissions.

1. The method of preparation of the metallic bulk catalyst honeycomb structure to neutralize the harmful gas emissions, including pre-processing of the inert carrier, applied on the surface of the intermediate coating of a modified aluminum oxide and one or more catalytically active platinum group metals, wherein the first carrier, representing a unit of the Al-containing foil, annealed at a temperature of 850-920C in a stream of air or oxygen for 12-15 hours, and then apply to it the intermediate coating - modified alumina in the slurry at room temperature.

2. The method according to p. 1, characterized in that the coating of the suspension is carried out at the following ratio of components, wt.%:

The aluminum hydroxide - 22 - 32

Nitrate aluminum - 2 - 4

Nitrate cerium - 2 - 5

Water - alcohol ratio of 1:1 To 100

3. The catalyst obtained by the PP.1 and 2, consisting of a block of metal carrier, the surface of which has an intermediate floor of a modified aluminum oxide coated active phase of the noble metals of the platinum group, characterized in that it is keepnote Al2O3- 120 - 130 m2/g

Content SEO2in Al2O3- 8 - 15 wt.%

 

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