Method of production of the platinum catalyst used for purification of the exhaust gases of the internal combustion engines

FIELD: chemical industry; other industries; methods of production of the platinum catalysts.

SUBSTANCE: the invention is pertaining to the method of production of the platinum catalyst used for purification of the exhaust gases of the internal combustion engines. The invention presents the description of the method of manufacture of the catalyst for purification of the exhaust gases of the internal combustion engines including deposition of the aluminum oxide layer containing the catalytically active component - platinum on the inert steel carrier containing 15-23 % of chromium and 4.5-5.1 % of aluminum, with the subsequent drying and calcinations. At that before deposition of the aluminum oxide layer containing the catalytically active component - platinum the inert steel carrier is subjected to etching in the hydrochloric acid diluted with the water in the ratio of 1:1 within 25-35 seconds at the temperature of 20-25°С with the subsequent washing by the running and distilled water and the further heat treatment in the air at the temperature within the interval of 850-950°С for 10-20 hours, then it is subjected to the treatment with the ultrasound with the frequency of 18 kHz within 1-2 minutes and with the subsequent treatment of the surface of the inert steel carrier in the KOH alkaline solution with concentration of 10 % within 30-60 minutes for transformation of the oxides of the surface layer into the hydroxides. The technical result of the invention is simplification of the production process.

EFFECT: the invention ensures simplification of the production process.

3 cl

 

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

Known method of preparing catalysts [RU, patent No. 2063804, CL 0J 23/89, 37/03, 20.07.1996, BI No. 20], including the deposition of platinum on a metal carrier, where the metal carrier is a crushed chips of stainless steel, which is pre-occiderit, and then put platinum by immersing the carrier in an aqueous solution containing a soluble complex salt of platinum 4,5·10-4-6,0·10-4mol/l [Pt(NH3)4]Cl2and 0.005 mol/l potassium hydroxide at a temperature of 170-210°in a confined space within 150-180 minutes and the ratio of bulk volume of the medium to the volume of solution equal to 1:13-1:14.

The disadvantage of this method is that the granular carrier does not provide the immutability of the relative spatial position of the elements of the structure (rigidity) and has a low percentage of solid material in the reactor volume (high porosity). As well as the initial specific surface area of the primary carrier is very small and catalysts based on it have low catalytic activity.

To increase the initial specific surface area of metallic and ceramic substrates are widely practiced by applying an intermediate on the spoons or fillers.

Thus, in [RU, patent No. 2022643, CL 01J 35/04, 23/89, 53/36, 15.11.94, BI No. 21] was preparing a catalyst for the oxidative purification of exhaust gases of diesel engines of the following composition (in g / DM3volume of catalyst): platinum group metals (PGM) 0,35-2,83, the vanadium oxide is 1.0-10.0, filler 60-2000,0; where PGM platinum or palladium, or a combination thereof 1-2:1-3, or platinum, or palladium, in combination with iridium and rhodium in a ratio of 5:1, the filler is aluminum oxide or zirconium, or mordenite at a ratio of from 20-30 up to 10-80, media - cordierite ceramics or metal. In this case, all the components are on the walls through free channels of a monolithic or made in the form of the carrier material and the active components deposited on the surface of the carrier by simultaneous or sequential in any order impregnation with solutions of compounds of vanadium, or PGM, followed by drying and heat treatment in a stream of hydrogen containing gas or air. While soaking lead before or after application of the filler with intermediate stages: drying and heat treatment at successive application components when the density of the carrier 62 cells/cm2.

The disadvantages of the method are multi-stage and low-tech process.

The closest in technical essence and the achieved effect is the way that is written in [EN, patent No. 2005538, CL 01J 37/03, 23/46, 15.01.94, BI No. 1], which comprises applying a catalytically active component on an inert carrier, representing steel corrugated and rolled into a block foil containing 15-23% chromium and 4.5-5.1% of aluminum, the aluminum oxide layer from a solution of caustic soda with a concentration of 0.7 to 1.5% by direct dissolution therein of aluminum shavings, followed by drying and calcining, and further impregnation with aqueous solutions of salts of cerium, platinum and rhodium, drying and restoration in a stream of hydrogen gas.

The disadvantages of the method are multi-stage, complexity and duration of the process of preparation of the catalyst.

The basis of the invention the task is to simplify technology for catalysts for EXHAUST gas of the engine.

The problem is solved due to the fact that in the method of manufacturing a catalyst for purification of exhaust gases of internal combustion engines, including the application of the aluminum oxide layer containing the catalytically active component is platinum on an inert steel media containing 15-23% chromium and 4.5-5.1% of aluminum, followed by drying and calcining, according to the invention before application of the catalytically active component is platinum inert steel media hounded in hydrochloric acid, diluted with water in ratio 1:1, for 25-35 seconds at 20-25°s, followed what Romilly flow and distilled water and further heat treated in air in the temperature range of 850-950° With 10-20 hours, then spend the sonication frequency of 18 kHz within 1-2 minutes, followed by processing the surface of an inert steel media in an alkaline solution of KOH concentration of 10% within 30-60 minutes for the conversion of the oxide surface layer hydroxides.

The application of the aluminum oxide layer containing the catalytically active component is platinum on an inert steel media carry out single by dipping in a suspension of Metagalaxy aluminum containing metal fine platinum.

In addition, the suspension Metagalaxy aluminum (boehmite)containing dispersed metal is platinum, obtained in a closed volume at the temperature of 180-210°C, with stirring in the absence of oxygen during 130-180 minutes from the suspension of amorphous aluminum hydroxide in a solution of potassium hydroxide (concentration of 0.005 mol/l) and chloride tetrammine platinum (II). Amorphous aluminum hydroxide precipitated from nitrate aluminum ammonia solution and thoroughly washed from the NO3-ions (pH 5-6) and chloride tetrammine platinum (II). Development of platinum catalysts for EXHAUST gas of internal combustion engine on the sorption inert low surface area porous media (metals) usually consists of two stages:

1. synthesis of the intermediate layer, for example, aluminum oxide,

2. the application of the catalytically act who ate atom, for example, platinum.

Typically, these stages are separated in the process of preparation of the catalysts, each of them requires its own design, time and energy. Autoclave methods allow you to combine these two steps in one operation to obtain a suspension of the oxide or hydroxide of aluminum, containing a platinum metal in a highly dispersed state.

The proposed method is as follows. Media - corrugated foil of heat-resistant stainless steel containing 15-23% chromium and 4.5-5.1% of aluminum.

The media is placed in hydrochloric acid, diluted with water in ratio 1:1, 25-35 seconds at 25°s, followed by rinsing with running and distilled water. This operation provides the necessary purity of the samples and partially loosens the surface, increasing it.

Heat treatment in air at between 800 and 950°C for 15 hours. This operation is required for the enrichment of the surface of the steel aluminium due to its diffusion from the alloy to the surface and create rich, well connected with a base layer of oxide components of steel. It was established experimentally that the temperature is below 800°is insufficient to complete the aluminum concentration at the surface and at temperatures above 900°With the number of surface aluminum sharply against the melt, further increase in temperature is impractical. Previously conducted studies have shown that heat treatment for 5 hours allows to obtain an oxide layer thickness of about 4 μm, which is insufficient for stabilization applied in subsequent stages of the dispersed metal particles. It is shown that the optimum heat treatment time is 10-20 hours, because with less than 10 hours oxidation number of aluminum on the surface is insufficient, and when more than 20 hours duration of this operation, the amount of aluminum on the surface varies only slightly compared with the duration of about 20 hours.

Ultrasonic treatment (UZ). Oxidized carrier is placed in distilled water and treated with ultrasound frequency 18 kHz within 1-2 minutes. Experimentally determined optimal time of ULTRASONIC treatment for 1-2 minutes, because less than 1 minute is not enough to clean the entire surface, and 3 minutes ULTRASONIC treatment is impractical. This stage removes scale, poorly connected to the surface of the media.

Samples after ULTRASONIC treatment are placed in 10% potassium hydroxide solution and boiled for 30-60 minutes for hydration of the surface of the oxide layer. In this operation, the oxides are converted to hydroxides. It is found experimentally that the optimum time copaceni the media in alkali is 30-60 minutes, after boiling in less than 30 minutes hydroxyl layer on the surface uneven, and after boiling for more than 60 minutes hydroxyl surface layer differs little from the surface layer obtained after boiling in a time interval of 30-60 minutes boiling in 10% potassium hydroxide solution.

Suspension of Metagalaxy aluminum (boehmite), containing platinum, receive at room temperature, precipitating the excess ammonia concentration of 25% amorphous aluminum hydroxide from a solution of aluminium nitrate concentration of 100 g/l to pH 8-9. The precipitate is washed to pH 5-6, and then add to it the salt of platinum [Pt(NH3)4]Cl2in the amount of 10% by weight of the obtained alumoxanes cover and a solution of potassium hydroxide concentration of 0.01 mol/L. the resulting mixture was rinsed for 20-30 min in nitrogen removal from the system of molecular oxygen. The autoclave is pressurized and maintained at 190°for 150-180 minutes under stirring. According to [Manual inorganic synthesis: In 6 volumes. V.3. str. TRANS. with it. Ed. Gbauer. - M.: Mir, 1985]obtained in this way aluminum hydroxide is a boehmite AlO(OH), with restored from tetrammine platinum (II) to metallic state of highly dispersed platinum (according to analysis x-ray photoelectron spectroscopy), which after precalcino 600° With forms γ-Al2About3containing uniformly distributed finely dispersed platinum.

Applying a layer of aluminum oxide containing a metal highly dispersed platinum on a substrate carry out a single dipping pre-prepared, as described above, the substrate in a suspension of aluminum hydroxide (boehmite)containing the metal fine platinum. Method of dipping allows you to adjust the thickness of the coating.

Drying of the samples lead: at room temperature the samples allowed to stand for 1 hour, and then dried to 130°With heating rate of 10°/min and allowed to stand for 1 hour, then heated to 200°With heating rate of 10°/min. and incubated for 0.5 hour.

Samples calcined with a heating rate of 10°/min from 200 to 550°C and maintained at 200, 300, 400, 550°C for 0.5 hour.

It should be noted that the removal of oxygen from the system at the stage of obtaining the secondary suspension media containing fine metal platinum is a prerequisite for obtaining high-quality coatings, because in his presence when thermolysis along with metallic platinum are formed partially soluble platinum compounds of variable composition. Intervals of duration and temperature of the process, the concentration of potassium hydroxide in solution conditions are close to 00% exit metallic platinum from a solution of a complex compound.

Time for autoclave process consists of time of induction period (i.e. time visually observable metal in the process) and the time of separation of the metal. The temperature decrease and the concentration of potassium hydroxide in solution increases the induction period.

Thus, the method of producing catalysts for purification of exhaust gases of internal combustion engines by applying a secondary layer of aluminum oxide obtained autoclave method and containing the metal fine platinum, allows to simplify the technology of preparation of catalysts to reduce energy consumption and the execution time of the whole process up to 30 hours compared to 80 hours, and also dramatically reduce the number of wash and waste water containing harmful inorganic impurities.

1. A method of manufacturing a catalyst for purification of exhaust gases of internal combustion engines, including the application of the aluminum oxide layer containing the catalytically active component is platinum on an inert steel media containing 15-23% chromium and 4.5-5.1% of aluminum, followed by drying and calcining, characterized in that before applying the aluminum oxide layer containing the catalytically active component is platinum, inert steel media hounded in hydrochloric acid diluted with water in ratio 1:1, in ECENA 25-35 with at 20-25° With, followed by rinsing with running and distilled water and further heat treated in air in the temperature range of 850-950°in 10-20 hours, then spend the sonication frequency of 18 kHz within 1-2 min, followed by treatment of the surface of the inert steel media in an alkaline solution of KOH concentration of 10% within 30-60 minutes for the conversion of the oxide surface layer hydroxides.

2. A method of manufacturing a catalyst for purification of exhaust gases of an internal combustion engine according to claim 1, characterized in that the application of the aluminum oxide layer containing the catalytically active component is platinum on an inert steel media carry out single by dipping in a suspension of Metagalaxy aluminum containing metal fine platinum.

3. A method of manufacturing a catalyst for purification of exhaust gases of an internal combustion engine according to claim 2, characterized in that the suspension Metagalaxy aluminum boehmite containing dispersed metal is platinum, get in a confined space at a temperature of 180-210°C, with stirring in the absence of oxygen, during 130-180 min from a solution containing aluminum nitrate, ammonia (pH 5-6) and chloride tetrammine platinum (II).



 

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1 tbl, 3 ex

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