Method of producing catalyst for diesel soot after-burning

FIELD: chemistry.

SUBSTANCE: invention relates to methods of producing catalysts for cleaning diesel engine emissions. Described is a method of producing a catalyst for diesel soot after-burning, involving mixing a copper extract in n-caprylic acid and a molybdenum extract in isoamyl alcohol in a ratio which ensures content of metals in the obtained mixture which corresponds to the composition CuMoO4, subsequent removal of the solvent from the obtained mixture and pyrolysis thereof on air, wherein the obtained mixture of extracts is brought to total concentration of metals of 1.5-2.0 wt % using isoamyl alcohol; the diluted mixture is deposited on a substrate made from titanium or alloy thereof, which is treated by plasma-electrolytic oxidation in an aqueous electrolyte; the solvent is removed by heating the titanium substrate with the deposited mixture of extracts to 150°C for not less than 1 hour; subsequent pyrolysis is carried out at temperature 540-550°C for not less than 1 hour.

EFFECT: simple method of producing a catalyst on a metal substrate and high efficiency thereof while simultaneously improving quality and efficiency of the obtained catalyst.

2 cl, 3 dwg, 3 ex

 

The invention relates to the production of catalysts for emission control of diesel engines and other combustion products of fossil fuels, the main toxic component of which is carbon black, and may find application in the automotive industry and energy.

Cleaning processes ("reuse") exhaust and waste gases, which are based on the oxidation accompanied by heat and are characterized by large pressure drops. Catalysts on metal media with high conductivity and mechanical strength, less prone to overheating, which can lead to decontamination and mechanical destruction catalysts, with metal media can be made in the form of a complex multi-structures.

Known for having a high activity catalyst for purification of exhaust gases of diesel engines (RF application No. 9305276, publ. 1996.04.27), which is a metal carrier of alloys containing Nickel and chromium, which by the method of chemical treatment applied active ingredients, and a method thereof, which consists in processing a metal carrier with a solution of chromic anhydride and subsequent washing, drying and calcining. The disadvantage of this method is the lack of oxide or drain the institutions sublayer on the surface of the alloys, containing Nickel and chromium, due to the high oxidation resistance of these alloys (nichrome, ferrochrome) in air (up to 1250°C), as well as to aggressive reagents, including a solution of chromium trioxide. Porous oxide sublayer on the metal carrier is required to ensure the adhesion of the active catalyst components to the media and increase the working surface of the catalyst (Scientific basis for the production of catalysts, edited by Rasulova, Novosibirsk., 1982. Technology catalysts, edited Ipomaea, 3rd ed., L., 1989. Overruled). In addition, the use of toxic chromium trioxide is undesirable because of its harmful effects on the human body.

Known (U.S. Pat. Of the Russian Federation No. 2103057, publ. 1998.01.27) way to obtain high activity and thermal stability of the catalyst for deep oxidation of CO, hydrocarbons, soot, purification of vehicle exhaust and waste gases of industrial enterprises on the metal aluminum carrier containing the oxide composite consisting of aluminum oxide, oxides of transition metals and oxides of rare earth elements, or mixtures thereof, and/or phosphorus oxide and/or silicon oxide, and/or mixtures of oxides of transition metals. The catalyst may also contain platinum metals or their mixtures. Known catalyst receive the Ute electrochemical oxidation of aluminum foil, ceramometal containing aluminum oxide, aluminum metal, the oxide of phosphorus and/or silicon oxide receive anode-spark method, oxides of rare earth and transition elements can be added together or separately by impregnation of ceramometal in solutions of nitrate salts of the corresponding composition, followed by drying and annealing at 400-600°C. Platinum metals introduced by impregnation of ceramometal in or ammonium chloride solutions of the corresponding PGE, followed by drying and annealing at 400-600°C. a Significant disadvantage of this method is the use of aluminum metal as a carrier of the active catalyst components, since the melting point of aluminum is 660°C, and the exhaust gas temperature in normal the mode of operation of the automobile engine is 500-700°C.

Closest to the claimed is a method of obtaining copper-molybdate of catalysers of soot, in particular of copper molybdate CuMoO4, extractive-pyrolytic method, which involves the extraction of molybdenum from the hydrochloric acid solution of isoamyl alcohol extraction of copper from copper sulphate solution of n-Caprylic acid, mixing the resulting extracts in amounts of, in particular, providing a molar ratio of CuO:MoO3=50:50, pyrolysis received MESI in air at 550°C to constant weight to obtain CuMoO 4(Libohova NV, Karpovich NF, Makarevich HP, Chigrin p. g "Catalytic combustion of soot in the presence of copper-molybdate systems, obtained by different methods". Catalysis in industry, 2008, No. 6, p.35-40).

The catalytically active material obtained in a known manner, allows a reduction of the ignition temperature of the particulate carbon, however, it cannot be successfully applied for treatment of emissions from diesel engines, because the known method does not solve the task of applying the above-mentioned material on the metal surface of the particulate filters. Using the received known method of catalytically active material is limited due to the complexity of its application to the metal surface because of the formation of a uniform catalytic coating and its strong coupling with metal, you must have the oxide sublayer with a developed surface. The application of the catalytically active material on a metal surface using known methods, including pre-sputtering of the oxide substrate, characterized by low productivity, does not provide a robust and uniform catalytic coating on metal parts of complex multi-form, in particular diesel particulate filters, which reduces the efficiency of the WPI the local catalytically active material, and prevents its widespread use.

The objective of the invention is to develop a simple and highly efficient method of obtaining effective catalyst on the metal carrier, suitable for purification of diesel emissions on an industrial scale.

The technical result of the invention is to simplify the method of preparation of the catalyst on a metal substrate and increase productivity while improving the quality and effectiveness of the catalyst.

This technical result is reached by a method of producing catalyst afterburners diesel soot, comprising mixing an extract of copper in n-Caprylic acid and extract of molybdenum in isoamyl alcohol in a ratio that provides the metal content in the resulting mixture corresponding to the composition CuMoO4subsequent removal of the solvent from the resulting mixture and pyrolysis her in the air, which in contrast to the known resultant mixture of extracts bring isoamyl alcohol to the total metal concentrations of 1.5-2.0 wt.%, the diluted mixture is applied on a titanium substrate of titanium or its alloy, treated by plasma electrolytic oxidation in an aqueous electrolyte, the solvent is carried out by heating the above-mentioned substrate nameservices extracts up to 150°C for at least 1 hour, subsequent pyrolysis is carried out at a temperature of 540-550°C for at least 1 hour.

Optimal from the point of view of getting on a substrate of titanium or its alloy coating with a highly rough surface intersected by a great number of pores, is plasma-electrolytic oxidation mentioned substrate in an aqueous electrolyte containing, mol/l:

sodium silicate Na2SiO3·9H2O0,02-0,1
sodium hydroxide NaOH0,04-0,06,

in monopolar galvanostatically mode when the anode current density of 0.05 to 0.3 A/cm2within 5-30 minutes in Addition, this plasma-electrolytic treatment in an alkaline silicate electrolyte allows to form the titanium coating, which in addition to the crystalline titanium oxide is amorphous silicon oxide, is widely used in catalysis as a substrate for the deposition of the catalytically active mass.

The method is as follows.

Using extraction-pyrolytic method to form a catalytically active coating on a metal substrate treated by plasma electrolytic oxidation.

For mixing body is ical extracts using extract copper n-Caprylic acid from an aqueous solution of copper sulfate and extract molybdenum isoamyl alcohol from aqueous nitric acid saturated solutions of paramolybdate ammonium. These organic reagents are mixed in a ratio that provides metal content corresponding to the formula CuMoO4while the total concentration of metals in the resulting solution was adjusted to 1.5-2.0 wt.% by dilution used organic solvents, mainly isoamyl alcohol.

A metal substrate made of titanium or its alloy, treated by the method of plasma-electrolytic oxidation with obtaining the oxide layer with a developed surface, providing strong adhesion of the catalytically active material with a metal surface. Plasma-electrolytic oxidation predominantly carried out in an aqueous electrolyte containing, mol/l: 0,02-0,1 sodium silicate Na2SiO3·9H2O and 0.04-0.06 sodium hydroxide NaOH, monopolar galvanostatically mode when the anode current density of 0.05 to 0.3 A/cm2within 5-30 minutes of the Final voltage of the formation is at this 280-300 C. the Substrate of titanium or its alloy as the anode, the cathode using a hollow coil, made for example of Nickel, through which water flows during plasma electrolytic oxidation. By mixing the electrolyte with the aid of known means to reduce it to warm up and conduct heat from xinerama metal. The temperature of the electrolyte during the process of oxidation does not exceed 30°C.

The thickness of the obtained oxide layer is from 10 to 25 μm. According to x-ray phase analysis of the specified layer contains titanium oxide in modifications rutile and anatase, while the silicon is present in the form of amorphous silica SiO2. As you can see in the images obtained using scanning electron microscope (figa - embossed surface view; b - phase representation of the surface), the surface oxide layer is rough and detects time - traces of electrical breakdowns or outputs of gas bubbles. This layer consists of crystallites with a size of 3-10 μm and has a high porosity, the pore size reaches 5-7 ám.

A substrate of titanium or its alloy coated with an oxide layer is immersed in the prepared solution containing a mixture of organic extracts of metals, in the proper ratio, and diluted to the respective total concentration of the metals with the help of used solvents, stand 30-40 minutes to seal, then if necessary, remove excess solution by shaking. The substrate coated with the composition is placed in a furnace and heated in air in two stages: at a temperature of not less than 150°C for at least one hour to remove organic solvents, ZAT is at a temperature of 540-550°C for at least one hour to decompose organic solvents and the formation of copper molybdate CuMoO 4.

The increment of the weight of the treated substrate after a single impregnation and subsequent pyrolysis is 0.01-0.03 wt.%, on the radiograph (figure 2) are the diffraction peaks of titanium, titanium oxide and copper molybdate CuMoO4triclinic structure. In the low angle region of the x-ray spectrum has a halo, characteristic of amorphous silicon oxide.

As demonstrated obtained using atomic force microscope micrograph (figure 3) surface oxidized titanium plates after extraction-pyrolytic deposition of molybdate CuMoO4the layer of molybdate evenly covers the surface, almost without changing the generated terrain. On the surface of the porous oxide layer is observed grain molybdate size up to 200 nm in diameter.

According to thermogravimetric and differential thermal analyses, obtained in the presence of the proposed method, the catalyst temperature of the combustion of soot is approximately 270°C., and the temperature corresponding to the maximum rate of combustion of soot equal to 383°C. Thus, the catalyst provides the combustion of soot within the temperature range of the exhaust gases of a diesel engine.

Examples of specific implementation of the method

The wire diameter of 0.12 cm and plate once the leader of 2.5×to 0.5×0.1 cm, made of titanium or its alloy, after chemical polishing in a mixture of concentrated acids HNO3:HF=3:1 (by volume) at 70°C was processed by the method of plasma-electrolytic oxidation. The current source served as a computer-controlled thyristor unit TER-100/N.

For the application of the catalytically active layer is oxidized samples were immersed in a solution containing the above-mentioned organic reagents in the claimed proportions and diluted up to the corresponding total metal concentrations, after which the samples were placed in a furnace and heated in air, as described above.

X-ray phase analysis of the samples coated with the catalyst layer was performed using a diffractometer DRON-7 using Cu-radiation. The surface of the samples was investigated by scanning electron spectroscopy (microscope EVO-40) and atomic force microscopy (microscope NTEGRA PRIMA).

To study the catalytic properties of the samples of the latter were placed on a metal grid and covered with soot in the flame of the burner with the combustion of diesel fuel (GOST 305-82) to increase the mass of the sample is not less than 0.2-0.4 wt.%. The process of burning soot considered in the dynamic mode kiln derivatograph in the air flowing medium (50 ml/min) at a heating rate of 5 deg/min Tempera is ur ignition of soot in the presence of CuMoO 4with an accuracy of ±2°C was evaluated by a temperature maximum differential thermo analytical curves.

Example 1

Wire made of technical titanium W 1-0, was treated in an electrolyte containing, mol/l:

sodium silicate Na2SiO3·9H2O0,02
sodium hydroxide NaOH0,04,

when the anode current density of 0.05 A/cm2within 20 minutes

The thickness of the formed oxide layer 12 microns.

The treated substrate was immersed in a solution containing the extract of copper in n-Caprylic acid and extract of molybdenum in isoamyl alcohol, diluted isoamyl alcohol to the total metal concentrations of 2 wt.% (Cu - to 0.80 wt.%, Mo - 1.20 wt.%) and containing, ml:

extract copper (Cu content 0,325 mol/l)34
extract molybdenum (Mo containing 1.10 mol/l)10
isoamyl alcohol55,

it was kept in the solution for 30 minutes, shaking the excess solution then was heated in a muffle furnace SNOL at 150°C in air for 70 min, increased is the temperature up to 540°C and kept at the attained temperature for 60 minutes

The temperature of the combustion of soot is approximately 270°C., the temperature of the maximum rate of combustion of soot - 383°C.

Example 2

The plate made of titanium alloy AT-0 (wt.%: Ti 95,4-99,6, Al of 0.2-1.4, Mn 0,2-1,3, Zr 0.3) were treated in the electrolyte containing, mol/l:

sodium silicate Na2SiO3·9H2O0,1
sodium hydroxide NaOH0,06,

when the anode current density of 0.3 A/cm2within 5 minutes

The thickness of the formed oxide layer 10 microns.

The thus treated substrate was immersed in a solution containing the extract of copper in n-Caprylic acid and extract of molybdenum in isoamyl alcohol, diluted isoamyl alcohol to the total metal concentrations of 2 wt.% (Cu - to 0.80 wt.%, Mo - 1.20 wt.%) and containing, ml:

extract copper (Cu content 0,325 mol/l)34
extract molybdenum (the content of Mo 1.10 mol/l)10
isoamyl alcohol55

it was kept in the solution for 40 min, heated at 150°C for 60 min, increasing the temperature up to 540°C and is wide at the attained temperature for 70 minutes

Results similar to those obtained in example 1.

Example 3

The plate made of titanium alloy PTM (wt.%: Ti to 96.2, Al 1.8 to 2.5, Zr 2-3, Fe and 0.25) were treated in the electrolyte containing, mol/l:

sodium silicate Na2SiO3·9H2O0,1
sodium hydroxide NaOH0,06

when the anode current density of 0.3 A/cm2and within 30 minutes

The thickness of the formed oxide layer 25 microns.

The thus treated plate was immersed in a solution containing the extract of copper in n-Caprylic acid and extract of molybdenum in isoamyl alcohol, diluted isoamyl alcohol to the total metal concentrations of 1.5 wt.% (Cu - 0,597 wt.%, Mo - of 0.903 wt.%) and containing, ml:

extract copper (Cu content 0,325 mol/l)34
extract molybdenum (Mo containing 1.10 mol/l)10
isoamyl alcohol88,

it was kept in the solution for 40 min, heated at 150°C for 60 min, increasing the temperature to 550°C and kept at the attained temperature for 60 minutes

Financial p the tats similar to those obtained in example 1.

1. The method of producing catalyst afterburners diesel soot, comprising mixing an extract of copper in n-Caprylic acid and extract of molybdenum in isoamyl alcohol in a ratio that provides the metal content in the resulting mixture corresponding to the composition of Simoo4subsequent removal of the solvent from the resulting mixture and pyrolysis in air, characterized in that the mixture of extracts bring isoamyl alcohol to the total metal concentrations of 1.5-2.0 wt.%, the diluted mixture is applied on a substrate of titanium or its alloy, treated by plasma electrolytic oxidation in an aqueous electrolyte, the solvent is carried out by heating a titanium substrate coated with a mixture of extracts of up to 150°C for at least 1 h, the subsequent pyrolysis is carried out at a temperature of 540-550°C for at least 1 hour

2. The method according to claim 1, characterized in that the plasma-electrolytic oxidation of a substrate of titanium or its alloy is carried out in an aqueous electrolyte containing, mol/l:

sodium silicate Na2SiO3·9H2O0,02-0,1
sodium hydroxide NaOH0,04-0,06,

in monopolar galvanostatically mode when protestantes current of 0.05 to 0.3 A/cm 2within 5-30 minutes



 

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2 ex, 1 tbl

FIELD: chemistry.

SUBSTANCE: present invention relates to catalysts, methods of preparing catalysts and methods of producing alkenyl alkanoates. A method is described for preparing a catalyst suitable for use in production of alkenyl alkanoates, involving: deposition of a first carrier material and binding agent on a second carrier material to obtain layered carrier material in form of particles with an inner and an outer layer, where catalyst components in form of palladium, gold or combinations thereof are contained in the outer layer of the layered carrier material. A catalyst is also described for producing alkenyl alkanoates, which contains: layered carrier material in form of particles with at least an outer layer containing a first carrier material and binding agent, and an inner layer containing a second carrier material, where the outer layer contains at least palladium combined with gold which is in contact with it to obtain the catalyst, where the inner layer essentially does not contain palladium and gold. A method is described for producing alkenyl alkanoates, involving: bringing raw material containing alkene, alkanoic acid and oxidising agent into contact with a catalyst prepared using the method described above.

EFFECT: improved production of alkenyl alkanoates, reduced amount of by-products and increased efficiency of production.

44 cl, 6 tbl, 15 ex

FIELD: chemistry.

SUBSTANCE: invention relates to methods of preparing a catalyst, for example for oxidising ammonia and hydrocarbon-containing gases and can be used primarily in production of nitric acid. The method of preparing catalyst involves initial heat treatment of an inert carrier in a current of air or oxygen, depositing an intermediate coating from aluminium oxide or one or more platinum group metals onto the surface of the said carrier, and drying, wherein the intermediate coating of aluminium oxide is deposited from a gel, obtained by combining initial components in water in the following ratio, wt %: aluminium nitrate nonahydrate - 3-10; aqueous ammonia (25% concetration) - 1.7-5.5; ionogenic surfactant 0.25-1.0; water - the rest up to 100.

EFFECT: preparation of a catalyst with longer service life, which increases efficiency of production and reduces its cost, improves regeneration and recycling of the catalyst.

2 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a layered composite, method of making and method of converting hydrocarbons using said composite. A layered composite is described for catalytic production of alkenyl alkanoates, containing an inner core and an outer layer, which contains heat-resistant inorganic oxide, a fibrous component, inorganic binder and palladium, gold or their mixture as the catalytic component, dispersed in the outer layer. A method is described for production of alkenyl alkanoates, involving bringing a mixture of alkene, alkanecarboxylic acid and oxygen-containing gas into contact with the catalyst described above. A method is also described for making a catalyst for production of alkenylalkanoate, involving coating an inner core with a suspension, containing an outer heat-resistant inorganic oxide, fibrous component, inorganic binder precursor, organic binder and solvent, so as to obtain a core with an outer coating layer, and baking at temperature below 200°C for a period of time sufficient for binding the outer layer to the inner core, so as to obtain a layered composite, which contains a catalytic component containing palladium, rhodium, gold or their combination.

EFFECT: obtaining high-strength catalyst.

28 cl, 5 ex

FIELD: chemistry.

SUBSTANCE: invention concerns neutralisation catalysts for exhaust gas (EG) of internal combustion engines (ICE) and industrial effluent gas. Catalyst is obtained due to: 1) adding orthophosphoric acid to coating suspension to obtain alumophosphate, a binding substance, the total composition of which serves for coating reinforcement and thermal stabilisation of porous coating structure; 2) energy heterogeneity increase by adding zyrconyl dihydrophosphate to coating suspension, so that the total composition serves to enhance heat resistance of both modified aluminium oxide and catalytic contacts, i.e. of the whole catalyst. Invention claims method of catalyst preparation, involving preliminary processing of inert Al-containing foil block carrier by baking at 850-920°C in air flow for 12-15 hours, followed by carrier application onto intermediary modified aluminium oxide coating surface from suspension at room temperature, thermal processing of block with intermediary coating in air flow and further applying one or more active catalytic metals of platinum group. Intermediary coating is applied from suspension containing additionally orthophosphoric acid and zyrconyl dihydrophosphate at the following component ratio, wt %: aluminium hydroxide (pseudobemite) - 22-32, aluminium nitrite - 2-4, cerium nitrite - 2-5, orthophosphoric acid - 1-2, zyrconyl dihydrophosphate - 1-3, water - up to 100; thermal processing of block with intermediary coating is performed at 620-650°C with maturing for 1.8-2 hours. Invention also claims catalyst including metal block carrier, intermediary coating of modified aluminium oxide and active phase of noble metals of platinum group applied onto porous surface of intermediary coating. Catalyst includes 7-14 wt % of modified Al2O3 with specific surface area of 120-130 m2/g, which includes additionally aluminium phosphate and zyrconyl phosphate at the following weight ratio of coating components (%): aluminium oxide (89.7-71.4), cerium oxide - (3.5-9.7), aluminium phosphate - (3.6-8.1), zyrconyl dihydrophosphate - (3.2-10.9).

EFFECT: significant enhancement of mechanical and heat resistance of catalytic coating at high efficiency in waste gas treatment process, prolonged lifetime.

2 cl, 2 tbl, 26 ex

FIELD: gas treatment catalysts.

SUBSTANCE: invention relates to a method for preparing catalyst and to catalyst supported by block ceramic and metallic carrier having honeycomb structure for treating internal combustion engine exhaust gases. Preparation of catalyst comprises preliminary calcination of inert honeycomb block carrier followed by simultaneously depositing at 550-800°C, on its surface, intermediate coating of modified alumina and active phase consisting of one or several platinum group metals from water-alcohol suspension including aluminum hydroxide (boehmite, AlOOH), cerium nitrate, and one or several inorganic salts of platinum group metals. Coated material is then dried and subjected to heat treatment and reduction. According to invention, aforesaid suspension contains boehmite and cerium nitrate at 1:2 ratio and further contains reducing disaccharide so that suspension has following composition, wt %: AlOOH 18-20, Ce(NO3)3·6H2O 36-40, one or several platinum group metal salts (e.g., H2PtCl6, PdCl3, or RhCl3 calculated as metals) 1.5-1.8, reducing disaccharide 5-6, and water/alcohol (between 5:1 and 10:1) the rest. Thus obtained catalyst for treating internal combustion engine exhaust gases is characterized by: specific surface area of coating 80-100 m2/g, Al2O3 content 2.5-6.5%, CeO2 content 2.5-6.5%, active phase (calculated for platinum group metals) 0.2-0.4%, and block carrier to 100%.

EFFECT: simplified technology due to reduced number of technological stages and shortened process time, and enabled preparation of high-activity catalyst.

6 cl, 1 tbl, 8 ex

FIELD: chemistry.

SUBSTANCE: catalyst further contains chromium oxide in amount of 5.0-20.0 wt % of the total amount of catalyst. Ethanol with water content of up to 15 wt % is used in the process. Use of the method enables to increase ethanol conversion to 58%, ethyl acetate selectivity to 95%, and use ethanol with water concentration of up to 15 wt %.

EFFECT: method does not require feeding an additional amount of hydrogen into the process.

2 cl, 10 ex, 1 tbl

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