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

 

(57) Abstract:

The invention relates to methods of producing catalysts for purification of exhaust gases of internal combustion engines. The method involves the use as a carrier cheaper heat-resistant foil with a chromium content of 15 to 23% and aluminum 4,5 - 5,1% with a coating of aluminum oxide deposited in caustic soda solution with a concentration of 0.7 to 1.5% by direct dissolution therein of aluminum shavings, followed by drying and calcining. Based on the specified carrier with a coating of aluminum oxide is preparing a catalyst containing as the active components of platinum and rhodium deposited by impregnation from aqueous solutions of their hydrochloric acid salts, which reduce the current of gaseous hydrogen.

The invention relates to methods of producing catalysts for purification of exhaust gases of internal combustion engines (ice).

Known methods of preparing catalysts on supports cell structure with many holes in the direction of flow of the gas stream. Source specific surface of such block of carriers is small (0.01 to 0.65 m2/g) and catalysts based on them have low catalytic the x media widely practiced by applying the intermediate substrate. Known catalysts for purification of EXHAUST gas of internal combustion engine on metal and ceramic media block structure, the surface of which increases in a variety of ways. [1] the catalyst prepared on the media of the aluminium-containing alloy of iron, which is subjected to heat treatment to form on the surface coating of refractory oxide and aluminum oxide of the transition metal (e.g. iron oxide), the active substance is applied on the formed oxide coating. The intermediate coating obtained in the described manner, does not have the required specific surface is flaking off and the resulting catalyst does not have sufficient efficiency and durability.

In [2] described a method of applying a coating of a suspension of aluminum oxide, in which dispersed particles of metals (platinum, palladium, their alloys). This suspension is applied on an inert carrier, then remove the water in the drying and calcination. This method does not provide strong adhesion of the coating to the surface of the inert carrier, and the damage this way, the metal particles of platinum and palladium have low catalytic activity.

Described in [3] the method of preparation of the catalyst clear elastic primer from fibers of aluminum silicate, which dried at 100-250aboutAnd then it put a layer of aluminium hydroxide, then dried at 100-250aboutC and calcined at 800-1200aboutC. the resulting layer is impregnated with one or more platinum group metals and calcined. This method involves many stages, is-low-tech. The intermediate annealing of the oxide coating at 1200aboutWith leads to the formation of corundum (Al2O3with a small specific surface area. The use of a metal carrier of carbon steel reduces the service life of the catalyst prepared in this medium, hard modes of operation, for example when cleaning the exhaust gases of the engine.

The closest in technical essence and the achieved effect is the way (prototype), described in [4] , where the purpose of obtaining a block of the catalyst for purification of EXHAUST gas of internal combustion engine original monolithic media repeatedly treated with alumina suspension in which the dispersion - girvan the alumina powder containing cerium oxide. (The cerium oxide is formed by impregnation of the alumina powder of the cerium salt solution and calcination). The treated suspension media and calcined to oxide-aluminum coating precipitated active weekago compounds of noble metal (platinum, rhodium) separately and subjected to its thermal decomposition.

The main disadvantage of this method of preparation of the catalyst (suspension) is low, the adhesive strength of a coating of aluminum oxide to the surface of inert carrier, uneven coating, resulting in reduced service life of the catalyst. The mass number of the applied oxide coating does not exceed 10% , which is clearly insufficient to obtain the required specific surface area and catalyst efficiency. In addition, separate deposition of noble metals on the carrier with the intermediate coating significantly complicates the technology. The described method of preparation of the catalyst is-low-tech, multi-phase and labor-intensive.

The purpose of the invention is to simplify and cheapen the technology of preparation of the catalyst for purification of exhaust gases of internal combustion engines.

The essence of the proposed method of preparation of the catalyst is as follows.

As the inert carrier take a steel foil with a chromium content of 15-23% , aluminum 1-8% , as is the content of these components improves the oxidation resistance of the foil. But because with the increased content of chromium and aluminum is a neigh chromium 15-20% , aluminum 4,5-5,1% . Steel foil corrugate, rolled into the unit and is subjected to oxidation in air at 900-950aboutC.

On heat-treated block are coated with aluminum oxide 0.7 to 1.5% caustic soda solution with the direct dissolution therein of aluminum shavings at 60-80aboutWith subsequent washing, drying and heat treatment at 500aboutC.

A coating of aluminum oxide impregnated with aqueous solutions of salts of Ce(NO3)2H2PtCl6and RhCl3followed by drying and recovery of active substances (Pt and Rh) hydrogen.

The inventive method allows to obtain a catalyst having high activity in the processes of purification of gas emissions from CO, NOx, CHx.

Applied uniformly, strongly bound with the inert carrier substrate of aluminum oxide having high thermal stability and adarevaralest provides the desired service life of the catalyst - 80.000 km, which is confirmed by tests at the landfill US.

The proposed method for the preparation of the catalyst makes it possible to simplify the manufacturing technology of the carrier with a coating of aluminum oxide, in advance to adjust the thickness of the oxide coating, and also exclusively the IDA aluminum has a high specific surface area (30-40 m2/g), calculated on the total weight of the inert carrier coated with the alumina content of from 10-30 wt. % that provides the necessary performance characteristics of catalysts.

Reduction of aluminum oxide leads to a decrease of the catalyst activity, and the increase to the increase in gas-dynamic resistance.

P R I m e R 1. Of the corrugated foil stamps HU 0.05 mm thick and 30 mm wide by imposing corrugated and flat strips fold unit with a diameter of 25 mm Unit oxidizes in air at 900-950aboutC for 20 h, treated with 10% sodium hydroxide solution at boiling for 1 h, washed and dried at 100-120aboutC.

Unit mass of 9.6 g placed in a beaker with 100 ml of a 0.7% aqueous sodium hydroxide solution, heated contents in a water bath up to 60-80aboutWith add 2 g of aluminum shavings (sod. Al 99,0-99,9% ) and incubated in a water bath for 5 h and then at room temperature for 15-20 hours Unit removed, thoroughly washed, dried at 100-120about2 h and calcined at 250aboutWith 2 hours and at 500about3 o'clock

Block with a coating of aluminum oxide weighs 10.7 g, the content of Al2O3is 10 wt. % .

In 25 ml of 1% aqueous solution of Ce(NO3about2 h and calcined at 450about3 o'clock

After calcination unit weighs 10,81 g and contains CeO210% based on the weight of the coating of Al2O3(1.1 g), which is 1.0% by weight of the block.

In 100 ml of distilled water dissolve 29 mg H2PtCl66H2O and 5.8 mg of RhCl34H2O, put the block and incubated in the solution at room temperature for 20-24 hours the Unit is removed and dried at 100-120aboutWith 2 hours

Restore the active components are in hydrogen at a temperature of 400about5 o'clock

The catalyst weighs 10,82 g and contains: Al2O3- 10 wt. % CeO2to 1.0 wt. %

Pt - 0.1 wt. %

Rh - 0.02 wt. % the rest of the steel HU, sod. Cr - 20%

sod. Al - 5,1%

P R I m m e R 2. Analogously to example 1, but to increase the number of coatings of aluminum oxide after exposure unit at room temperature for 15 h, the glass block again put on a water bath, and the cycle is repeated. Next, as in example 1. After calcination unit weighs 11,99 g and contains 20 wt. % Al2O3.

To obtain the catalyst composition of example 1, the amount of salt Ce(NO3)2in the dual solution. Further according to the example 1. The unit weighs 12.2 g and contains CeO210 wt. % with respect to m is2O and

6,5 mg - RhCl34H2O for the same volume of solution. Further according to the example 1.

The catalyst weighs 12,23 g and contains:

Al2O3- 20 wt. %

CeO2to 1.9 wt. %

Pt - 0.1 wt. %

Rh - 0.02 wt. % the rest is steel HU with Cr content Of 20% , Al of 4.5% .

P R I m e R 3. Analogously to example 1, but with the aim of increasing the number of aluminum oxide, the dissolution of aluminum shavings are 1.5% NaOH solution and the number of chips is increased to 4 g, the block is kept in solution at 60-80about5 h and 15 h at room temperature, and then this cycle is repeated, then as in example 1.

After heat treatment unit with a coating of aluminum oxide weighs 13,7 g, where the coating weight of 4.1 g (Al2O3) that is 30 wt. % by weight of the entire unit. The amount of salt in solution increases 3 times. Further according to the example 1.

Block after impregnation with cerium salt, drying and calcining weighs 14.2 g and contains 10 wt. % CeO2with respect to the coating weight of Al2O3(by weight of the total block a content CeO22.9 wt. % ). A number of salts of platinum and rhodium in example 3 is:

H2PtCl 6H2O - 38,00 mg

RhCl34H2O - 7,54 mg Dissolution of salts and impregnation unit spend%

CeO22.9 wt. %

Pt - 0.1 wt. %

Rh - 0.02 wt. % the rest is steel HU (Cr content Of 20% , Al of 4.95% ).

P R I m e R 4. Analogously to example 1, but 100 ml of a 0.7% solution take 1 g of aluminum shavings. The block weighs 10.2 g, a coating of Al2O3weighs 0.6 grams, representing 5.9% of the mass of the block. The number of Ce(NO3)2for impregnating solution to take in 2 times less than in example 1.

After impregnation with a solution of Ce(NO3)2and heat treatment unit weighs 10,26 g, the number of SEO2it 10% (on all coverage of Al2O3or 0,58% (on the weight of the block). A number of salts of precious metals is:

H2PtCl66H2O - 27,1 mg

RhCl34H2O - 5.3 mg Impregnation with salts of the metals and the recovery analogously to example 1.

The catalyst weighs 10,27 g and contains:

Al2O3- 5.9 wt. %

CeO2is 0.58 wt. %

Pt - 0.1 wt. %

Rh - 0.2 wt. % the rest is steel HU (Cr content Of 20% , Al 5% ).

P R I m e R 5. Analogously to example 1, but dissolving 4 g of aluminum shavings are 1.5% NaOH solution and the cycle is repeated 3 times. Everything else, as in example 1. The unit weighs 16.7 g, the gain of Al2O3is 7.1 g (or to 42.5 wt. % to 40% ).

Caliceti contains 10 wt. % CeO2the weight of Al2O3and 4.1 wt. % by weight of the entire block.

A number of salts of precious metals will be:

H2PtCl66H2O - 46.2 mg

RhCl34H2O - 9,2 mg in the same amount of solution, hereinafter in example 1.

The catalyst weighs 17,41 g and contains:

Al2O3- 40.0 wt. %

CeO2of 4.1 wt. %

Pt - 0.1 wt. %

Rh - 0.02 wt. % the rest is steel HU with Cr content Of 20% , Al 5% .

P R I m e R 6. As in example 1, but instead of steel foil stamps HU take a steel block with a weight of 9.6 g of steel HU.

The catalyst weighs - 11.5g and contains:

Al2O3- 10.0 wt. %

CeO2to 1.0 wt. %

Pt - 0.1 wt. %

Rh - 0.02 wt. % the rest is steel HU with CR content Of 15% , Al 5% .

P R I m e R 7. As in example 1, but instead CHU take steel HU.

The catalyst weighs 11,5 g and contains:

Al2O3- 10.0 wt. %

CeO2to 1.0 wt. %

Pt - 0.1 wt. %

Rh - 0.02 wt. % the rest is steel HU.

The activity of the catalysts of examples 1 to 7 were tested in a flow-through installation in a three-part process of cleaning gas composition: CO - 0,4 about. % , NO - 0,1 about. % , C3H6- 0,076 about. % , ostalarietan increases in the number N 4 N 7 = N 6 N 1 N 2 N 3 = 5 and almost the same samples N 1, N 6, N 7, which suggests that the composition of the foil does not affect the activity of the catalyst that will allow you to apply the foil with a lower chromium content (15-20% ), which is cheaper and easier to manufacture.

The activity of samples N 3 and N 5 are almost identical, which allows to conclude that the content of aluminum oxide in the amount of 10-30 wt. % is optimal for creating an effective catalyst for purification of exhaust gases of internal combustion engines.

In the factory were made full-size samples of catalysts on metal block media claimed method and road tests have been conducted on the car GAZ-24 to ground US. The catalyst showed high efficiency of purification of exhaust gases, the required resource work and was recommended for practical use. (56) U.S. Patent N 4096095, CL 01 J 21/04, 1979.

U.S. patent N 4132673, class B 01 J 21/04, published. 1979.

The application of Germany N 2411378, class B 01 J 35/02, 1979.

U.S. patent N 4587231, class B 01 J 21/04, 1986.

The METHOD of PREPARATION of the CATALYST FOR PURIFICATION of EXHAUST GASES of INTERNAL COMBUSTION ENGINES, comprising a coating on an inert carrier layer of aluminum oxide with subsequent impregnation with aqueous solutions with the optimum corrugated and rolled into a block foil with a chromium content of 15 - 23 wt. % aluminum 4,5 - 5,1 Mac. % , applying a layer of aluminum oxide is carried out in aqueous sodium hydroxide solution with a concentration of 0.7 to 1.5% by direct dissolution of aluminum, followed by drying and calcining, and the recovery of platinum and rhodium are in a stream of hydrogen.

 

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68 cl, 21 ex, 2 dwg

FIELD: production of catalytic compositions.

SUBSTANCE: proposed method includes combining and bringing into interaction at least one component of non-precious metal of group VII and at least two components of metal of VIB group in presence of proton liquid; then composition thus obtained is separated and is dried; total amount of components of metals of group VIII and group VIB in terms of oxides is at least 50 mass-% of catalytic composition in dry mass. Molar ratio of metals of group VIB to non-precious metals of group VIII ranges from 10:1 to 1:10. Organic oxygen-containing additive is introduced before, during or after combining and bringing components into interaction; this additive contains at least one atom of carbon, one atom of hydrogen and one atom of oxygen in such amount that ratio of total amount of introduced additive to total amount of components of metals of group VIII to group VIB should be no less than 0.01. This method includes also hydraulic treatment of hydrocarbon material in presence of said catalytic composition.

EFFECT: enhanced efficiency.

29 cl, 8 ex

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