Method of automotive catalyst

FIELD: process engineering.

SUBSTANCE: invention relates to production of automotive catalysts, particularly, to their recovery. Method or recovery comprises thermal decomposition of pyrocarbon, dissolution of platinoids by the mix of hydrochloric acid and nitric acid, or 30%- hydrogen peroxide in closed cycle. Note here that dissolution process is analysed for completeness of platinoids extraction while excess nitric acid and hydrogen peroxide are removed by reducing agents. To extract platinoids, acid solution is subjected to ionic flotation extraction by cationic surfactants. Then, extract with platinoid precursors is separated from acid solution containing cerium and aluminium ions to evaporate extractant. Platinoid precursors are dissolved in water to produce micellar solution, added is hydrazine hydrate to reduce platinoids in alkaline medium to metal nanoparticles on mixing by ultrasound. Dispersion is centrifuged to drain aqueous solution and rinse centrate by alcohol to proceed with centrifugation to obtain nanopowder of platinoids. Acid solution containing ions of cerium and aluminium is neutralised by potassium hydroxide to pH=8-9. Potash soap of higher carbonic acids is added to separate cerium and aluminium soaps. The latter are dissolved in micellar aqueous solution of sodium dodecylsulphate to make the mix of cerium and aluminium hydroxides and centrifuge obtained dispersion. Precipitate of cerium and aluminium hydroxides are rinsed by water to be centrifuged again so that precipitate is separated and air dried. Then, said precipitate is calcined at 400°C to obtain nanopowders CeO2 and γ-Al2O3 and CeO2.

EFFECT: new catalysts produced with no extra treatment.

5 cl, 2 ex

 

The invention relates to the production of automotive catalysts-catalysts. In particular, regeneration of catalysts for the afterburning of exhaust gases - carbon monoxide, nitrogen oxides, hydrocarbons.

The composition of the catalyst comprises nanoparticles double or triple systems, Pt/Rh, Pd/Rh, Pt/Pd/Rh deposited on the sublayer ultrafine γ-Al2About3and of cerium dioxide CeO2with a specific surface area of about 200 m2/year / γ-Al2O3plays the role of a catalyst carrier, a SEO2reduces the coefficient of thermal expansion and creates favorable conditions for regulating the content and activity of oxygen on the catalyst surface. The composition of the catalyst, in turn, covers cellular ceramics from cordierite, 2MgO·2Al2O3·5SiO2. Honeycomb ceramic has a much smaller specific surface 0.0014 m2/g than nanoscale materials.

Known methods of removing the catalytic components of the platinum group by oxidation of gaseous reactants, oxygen, chlorine, fluorine. They are dangerous in the work, require expensive equipment, compliance increased security measures. Widely presents the methods of extraction of platinum group metals with liquid reagents, for example the Royal vodka, nitric acid, hydrogen peroxide, etc. they are All listed in the best part close to the claimed invention of the patent of the Russian Federation No. 2209843 (Publ. 10.08.2003).

Thus, the method for extracting platinum group metals from automobile catalysts, including thermal decomposition of pyrocarbon, dissolution of platinum with a mixture of hydrochloric and nitric acids or 30% hydrogen peroxide in a closed loop. Platinum after leaching precipitated by cementation aluminum powder.

The disadvantage of this method of recycling of automotive catalysts is that the recycled material cannot be used directly to create a new catalyst. Recoverable platinum nanomaterials are not, as is required to create a new catalyst. In addition, waste not retrieved ultrafine SEO2and γ-Al2About3.

The present invention is carrying out the regeneration process in such a way as to extract from the solution after leaching of platinum group metals and other valuable components (CEO2and γ-Al2About3) in the form of powders, thereby providing the technical result: the preparation of extracted materials for the new catalyst.

The technical result is achieved by the method of recycling of automotive catalysts after thermal decomposition of pyrocarbon and dissolution of platinum with a mixture of hydrochloric and nitric acids or 30% hydrogen peroxide in a closed loop, and gave the e, according to the invention, according to the scheme:

analysis of the solution on the completeness of extraction of platinum;

- recovery of excess nitric acid and hydrogen peroxide;

- selection of platinum group metals from acidic solution by the method of ion protectable using cationic surfactant;

- separation of the extract with a precursor of platinum group metals from acid solution containing ions of cerium and aluminum;

- removal of the solvent by evaporation;

- dissolution of the platinum precursor in water to form a micellar solution;

- restore to platinum nanoparticles by hydrazinehydrate in alkaline medium under stirring ultrasound;

- separation of the resulting dispersion by centrifugation, the sediment washing successively with water, ethanol and re-centrifuged for separation of nanopowder platinum;

- alkalinization of acidic solution containing ions of cerium and aluminum, potassium hydroxide until pH=8-9;

- adding to the resulting solution of potassium Soaps of higher carboxylic acids, and separating the formed soap cerium and aluminium;

- dissolving soap in micellar aqueous solution of sodium dodecyl sulfate;

- biodegradable Soaps ammonium hydroxide with formation of a mixture of cerium hydroxide and aluminium;

the Department of dispersion by centrifugation, washing the precipitate hydroxides of cerium and aluminum water surface is priori by centrifugation;

- drying the precipitate hydroxides of cerium and aluminum in the air and calcination at a temperature of 400°C with the formation of nanopowder SEO2and γ-Al2About3.

When regeneration of the automotive catalyst according to the above scheme proceed redox reaction of nano-powders of platinum, CEO2and γ-Al2About3with acids and hydrogen peroxide. The speed of these reactions to four orders of magnitude greater than the reaction rate of dissolution of cordierite, because the rate of heterogeneous reactions is proportional to the value of specific surface area. Therefore, the acid dissolves only the active layer of the catalyst, and cordierite is practically insoluble. To minimize the dissolution of cordierite, the solution further analyze the content of platinum finishing process in achieving its constant concentration.

All the platinum must be in solution in the form of complex ions such as [PtCl6]2-. Therefore, the excess strong oxidizing agents: nitric acid and hydrogen peroxide - restore lower aliphatic alcohols: methyl, ethyl or isopropyl. The content of ethyl alcohol to a concentration of 0.1 mole fraction strengthens the structure of water, which facilitates the subsequent formation of precursors for platinum.

For ionic protectable acid rest the R after the dissolution of the active layer of the catalyst is placed in a column, add organic solvent: toluene, a mixture of toluene with isoamyl alcohol in the ratio of 1:4 (by volume) or kerosene. Include a compressor for air supply, add a stoichiometric amount of cationic surfactant - pyridinium chloride (CPH) or cetyltrimethylammonium chloride, which form the precursor complex ions of platinum by the equation:

The precursor is carried by air bubbles in the layer of the extractant and there is gradually concentrated.

To prevent the formation of micelles of the surfactant added in the form of a solution in ethyl alcohol. The formation of micelles affects the interaction of complex ion platinum with CP. The surfactant solution in the process of photoexcitable add gradually, preventing the formation of a hazy solution.

After protectable (bleaching solution) extract is separated from the acid solution containing ions of cerium and aluminum. The organic solvent is distilled off. Thus obtained precursor is dissolved in water with the formation of the micellar solution. The critical micellization concentration (CMC) CP 6·10-4M Precursor has a lower CMC. To increase the solubility of the precursor can be added ethyl alcohol content of 0.1 M. D.

Precursor to restore the platinum nanoparticles by hydrazinehydrate in the alkaline environment of the ri stirring ultrasound by the reaction:

Get nanohybrid platinum, which corresponds to their concentration in solution.

The variance of nanohybrids platinum centrifuged, washed with ethanol, centrifuged again and poured the alcohol. The precipitate is dried. Get black nanopowder with a metallic luster.

The acidic solution containing ions of cerium and aluminum, neutralized with potassium hydroxide to pH=8-9. Add potassium soap of higher carboxylic acids. Ions of cerium and aluminum ions with carboxylic acids to form lahoratories in mild soap and water, which floats on the surface of the solution:

The resulting soap cerium and aluminum is separated, dissolved in micellar aqueous solution of sodium dodecyl sulfate and decompose the ammonium hydroxide. This forms a dispersion of a hydroxide of cerium and aluminum. The resulting dispersion is centrifuged, the resulting precipitate hydroxides of cerium and aluminum washed with water, again centrifuged, separated, air-dried, and then calcined at 400°C. Receive light nanopowder SEO2and γ-Al2About3.

Used in the technological process of extraction agents, surfactants, higher carboxylic acids and cordierite also regenerate.

The invention is illustrated by examples.

Example 1. Trabot the config catalyst with a car "Mercedes-Benz" weight 1.3 kg according to chemical analysis contains 0.12% Pt, 0.009% Rh and 10% of pyrocarbon. Removal of pyrocarbon the spent catalyst was pre-calcined in a muffle furnace at 600°C for 1 hour. Cool and handle the rest in a known manner with a mixture of hydrochloric and nitric acid and 30% hydrogen peroxide within 1-2 hours, until the contents in the solution Pt does not reach a constant value. The solution is cooled and filtered. Half of the solution 1.25 l leave to example 2. In the other half the volume of 1.25 l gradually poured ethanol to recover the excess of nitric acid and hydrogen peroxide. The resulting solution was poured into photoextract.com. Add in 50 ml of toluene with isoamyl alcohol in the ratio of 1:4 (by volume). Separately prepare a solution of pyridinium chloride (CPH) in 5 ml of ethanol in an amount necessary for the formation of a Pt precursor according to equation (1). Poured 1 ml CP in the flotation machine and start the flotation process, gradually adding the remaining 4 ml of surfactant solution. After ion protectable extract is separated from the solution containing ions of cerium and aluminum, and distilled toluene and ISO-amyl alcohol. The remaining platinum precursor is dissolved in water, add hydrazinehydrate and potassium hydroxide in accordance with equation (2) and recover the platinum with stirring, ultrasonic generator with a frequency of 22 kHz. The resulting dispersion p is adenoidal centrifuged, the precipitate is washed with 5 ml of ethanol, centrifuged again, pour the alcohol and dry nanopowder platinum on the air. Get black with metallic nanopowder containing 95% Pt and 94% Rh content in the catalyst. According to transmission electron microscope, the size of the nanoparticles of 5-10 nm.

The acidic solution containing ions of cerium and aluminum, neutralized with potassium hydroxide to pH=8-9. Poured a 50% alcohol solution of potassium soap of oleic acid in accordance with equation (3) until such time as adding an alcoholic solution of potassium soap will not receive the precipitate aluminum soap. Received soap bubble to the surface of the solution. The solution is drained. The resulting soap is dissolved in 0.5 l of 0.01 M micellar solution of sodium dodecyl sulfate. To the resulting clear solution was added gradually concentrated ammonia solution to obtain hydroxides of cerium and aluminum as long as the sample does not show the dissolution of the precipitate by adding ammonium hydroxide. The resulting dispersion is centrifuged. The precipitate cerium hydroxide and aluminum was washed with distilled water and again centrifuged. Centrate is separated, dried in air and calcined at 400°C. Obtain 16.2 g of γ-Al2About3with a specific surface area of 185 m2/year

Example 2. The regeneration process of the car is strong catalyst performed analogously to example 1. In the remaining volume of the acidic solution of 1.25 l, dissolve 15 g CEO2. As the reductant take isopropyl alcohol as the organic solvent take kerosene, instead CPH cetyltrimethylammonium chloride and stirred by ultrasound 44 kHz. Get black with metallic nanopowder with a particle size of 4-12 nm, which contains 93% Pt and 92% Rh content in the catalyst, 14 g of γ-Al2About3and 13 g CEO2with a specific surface area of 173 m2/year

Thus, the proposed method of recycling of automotive catalysts allows to obtain regenerated nanomaterials, suitable for the manufacture of new automotive catalysts, or for use in other catalytic processes. Simultaneously regenerated and cordierite, because in the process of dissolution of the catalyst it is completely purified from other components. Extractants, alcohols, surfactants, higher carboxylic acids, sodium dodecyl sulphate also easily regenerated.

1. The method of recycling of automotive catalysts, including thermal decomposition of pyrocarbon, dissolution of platinum with a mixture of hydrochloric and nitric acids or 30% hydrogen peroxide in a closed loop, characterized in that the process of dissolution analyze the completeness of extraction of platinum group metals, and excess nitric acid and peroxide of bodoro is and remove the reducing agent, for selection of platinum acid solution is subjected to ion protectable cationic surfactant, then extract with platinum precursors are separated from the acid solution containing ions of cerium and aluminum, the solvent is evaporated, the precursor of platinum dissolved in water with the formation of the micellar solution, add hydrazinehydrate and restore the platinum in alkaline medium to nanoparticles of metals under stirring and ultrasonic dispersion is centrifuged, the aqueous solution is drained, the centrate is washed with ethanol and again centrifuged and get the nanopowder platinum; acid solution containing ions of cerium and aluminum, neutralized with potassium hydroxide to a pH of 8-9, add potassium soap of higher carboxylic acids, separating the resulting soap cerium and aluminum, dissolved them in micellar aqueous solution of sodium dodecyl sulfate, and then decompose the ammonium hydroxide with formation of a mixture of cerium hydroxide and aluminum, the resulting dispersion is centrifuged, the resulting precipitate hydroxides of cerium and aluminum washed with water and again centrifuged, the precipitate was separated, air-dried, and then calcined at 400°C, receive the nanopowder SEO2and γ-Al2O3.

2. The method according to claim 1, characterized in that as reductants use of aliphatic alcohols: methyl, ethyl or isopropyl the output.

3. The method according to claim 1, characterized in that as extractants used toluene, kerosene, a mixture of toluene with isoamyl alcohol.

4. The method according to claim 1, characterized in that the cationic surfactant is used, pyridinium chloride, cetyltrimethylammonium chloride.

5. The method according to claim 1, characterized in that for mixing use ultrasound with a frequency of 22 and 44 kHz.



 

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