Method of obtaining nanocatalytic material

FIELD: chemistry.

SUBSTANCE: invention relates to technological processes, namely to methods of realising chemical processes, in particular to the field of general and special catalysis, as well as to the creation of novel materials with special properties for the realisation of the said processes. The invention can be used for manufacturing thermochemical catalytic reactors of steam fuel conversion and chemical regeneration of heat, chemical current sources, fuel elements. In the method of a nanocatalytic material manufacturing obtaining a catalytically active layer on a metal carrier is carried out by the application of a powder composition by means of high-energy processes of the heterophase transfer with the application of two or more autonomously working devices on the metal carrier. The carrier has through holes, made by notching or by the other way of perforation. An area of the through holes of the metal carrier constitutes from 0.1 to 0.7 cm2, thickness of the catalytically active layer is from 100 to 200 mcm.

EFFECT: obtaining the nanocatalytic material, characterised by higher process efficiency, conditioned by an efficient mass-exchange in a reaction zone and the presence of through porosity, higher specific surface of the material due to the polydisperse structure and the presence of microporosity, higher strength of adhesion of the catalytic layer to the metal carrier.

4 cl, 2 tbl, 2 ex

 

The invention relates to technological processes, and in particular to methods of performing chemical processes, in particular to the field of General and specific catalysis, also to the creation of new materials with special properties for the implementation of these processes.

The invention can be used for the manufacture of catalytic thermochemical reactor steam reforming fuel and chemical heat recovery, chemical power sources, fuel cells.

Catalysis increasingly used in various fields of technology, delivering significant profit economy. This significantly stricter requirements for catalysts, including, for their effectiveness, selectivity, operating temperature and physico-mechanical characteristics. The preferred gradient-functional catalysts on metallic media.

Advantage in connection with the tightening of conditions are:

1 - metal (tape) media have compared to ceramic, a considerably higher thermal conductivity and therefore less inertia of the system as a whole;

2 - oxide media with high porosity compared with other materials and good processability when obtaining functional coatings;

3 - activators with nanoscale elements providing pain is th catalytic activity and a developed specific surface polydisperse structure.

To accomplish the above advantages of using different technological methods.

For example, is known [1] a method of manufacturing embossed porous framework of the hydrogen electrode of the chemical current source consists in preparing and rolling the mixture containing the Nickel powder and the pore-forming, sintering and subsequent removal of the pore-forming substance, wherein after sintering on the surface of the metal cause the relief of the calibration in the rolls.

Known [2] the electrode for electrochemical processes comprising a substrate of copper or other metal of high electrical conductivity in the form of a sheet with a deposited layer. A method of manufacturing an electrode for electrochemical processes includes applying a layer on a substrate of copper at elevated temperatures, with a substrate of copper or other metal with high electrical conductivity is subjected to annealing, put on her by plasma spraying a layer of Nickel and then a layer of Nickel with aluminum, the resulting layers annealed, cooled to room temperature and subjected to leaching. Next, take a plate of aluminium alloy with magnesium and applied to it a layer of copper or other metal with high electrical conductivity, then the substrate and the layer of copper or other metal with high electrical conductivity connected to each other by soldering.

Known [3] the method of manufacture of the population electrode, including the application of functionally graded layer on a metal substrate by the method of cold gas-dynamic spraying, using 3 self-contained dispenser. Functionally graded coating consisting of a copper or other electrically conductive material and a catalytically active components, and the composition of the coating varies linearly through the thickness. Deposited on a substrate layer is subjected to chemical etching.

The closest technical solution is the method [4] of manufacturing a catalytic composite coating. By functionality and the maximum number of similar essential features of this method is adopted us for the prototype.

The method of manufacturing a catalytic composite coating, including the production of a catalytically active layer by plasma spraying using two dispensers on the metal carrier. When consistently applied: - adhesive layer-coated powder composition containing, in mass%: aluminum 3-10, the aluminum hydroxide - else; - catalytically active layer by plasma spraying a powder composition containing, in mass%: aluminum 3-5, chromium oxide 2-5, tungsten 0,8-1,2, oxides of cerium, Langan, neodymium in an amount of 1.8 to 2.2, the copper oxide - 2-3, the aluminum hydroxide - rest. A layer of activator is applied innoplast method using two evaporators, containing in wt.%: the copper oxide 27-34, chromium oxide - 66-73.

The main drawbacks are:

- low efficiency of the process (catalytic activity), due to the accumulation of reaction products in the reaction zone;

insufficiently high specific surface of the material, the average pore diameter of between 20 and 50 μm, there is no microporous structure with an average pore diameter of less than 0.02 μm;

- lack of high adhesion of the catalytic layer with a metal carrier, due to the difference in coefficient of thermal expansion.

The technical result of the invention is to provide a nanocatalytic material, wherein the higher efficiency of the process (catalytic activity, due to effective mass transfer in the reaction zone and the presence of through-porosity, higher specific surface of the material provided polydisperse structure, the presence of microscopic pores (up to 30% of the pores have an average diameter of less than 0.02 μm), higher strength of adhesion of the catalytic layer with metal media).

The technical result is achieved due to the fact that in the method of manufacturing a nanocatalytic material receiving catalytically active layer on the metal carrier is made by powder coating the composition using high-energy processes in heterogeneous phase transfer (for example, microplasma or cold spray) using two or more Autonomous devices operating on a metal carrier having a through hole, which is made by a method of punching or other means of punching. The area of the through-holes of the metallic carrier is from 0.1 to 0.7 cm2the thickness of the catalytically active layer is from 100 to 200 microns.

In the chemical composition of the metal carrier includes at least one metallic element, and the composition of the powder composition includes at least one oxide of a specified metal element to form on the metal carrier of the oxide film during application of the powder composition.

The powder coating compositions are produced by changing the angle of the spray from 30 to 150°.

The catalytic coating layer of the high-energy methods heterophase transfer using two or more Autonomous working devices allows you to apply powders in different temperature zones of the reaction stream and create a gradient-functional coating, providing diffusion in non-equilibrium conditions of aluminum, Nickel, aluminum compounds, transition metals and rare earth elements in the material of the metal strip.

Use a metal carrier having a through hole, the example made in the form of corrugated expanded metal mesh or perforated other way, you can create the material through the porosity, which ensures the removal of reaction products, the increase in the mass transfer in the reaction zone, the reaction rate and catalytic activity.

The powder coating compositions are produced by changing the angle of the spray from 30 to 150°, which creates optimal conditions for applying the catalytic coating in hard-to-reach places, such as nodes and edges of the perforated material.

In addition, the use of a metal carrier having a through hole, opens great prospects for designing catalytic elements having sufficient open cross-section and low dynamic resistance.

Experimental work conducted in the field of creation of catalytic materials on the metal carrier, showed that the optimum size of each hole of catalytic material on a metal carrier (for example, in bulk or planar catalytic reactors) should be at least 0.1 cm2and not more than 0.7 cm2. When using a catalytic material, the orifice area less than 0.1 cm2the accumulation of reaction products and the catalytic activity is reduced. When using Catalytica is one material with square holes more than 0.7 cm 2reduces the number of collisions of the atoms of the reactants to the active surface, and therefore the catalytic activity is reduced.

The thickness manufactured in accordance with the invention, the catalytically active layer should be at least 100-200 μm in order to ensure effective operation throughout the regulated time.

When the coating layer thickness of less than 100 μm, a decrease of time effective operation of the catalytic layer due to possible poisoning or ash from the surface of the metal strip. When the coating layer thickness of more than 200 μm is observed cracking and delamination of the material during installation and operation.

To eliminate the influence of the difference of coefficients of thermal expansion between adjacent materials in multilayer structures on the adhesion strength of the composition in General, a metal carrier having holes, made of alloy, the chemical composition of which includes an element (or elements), resulting in the oxidation to the formation of a surface oxide film of oxide (or oxides)included in the composition applied to the metal carrier of the powder composition, which has a positive effect on increasing the strength of adhesion of the catalytic layer with a metal carrier especially at the nodes and edges of the lattice is I.

As showed researches of many authors [5], for reaction in a seemingly diffusion region, when the overall rate of the process is limited by diffusion of the reactants in the burrows of catalysts, to speed up the process you want to use porous media, bi - and polydisperse structures in which large pores are transport paths then a smaller radius, where is the bulk of the active centers. In accordance with this, in the proposed method, the higher the efficiency of the process (catalytic activity and specific surface) is achieved through the creation of an advanced macro (from 0.02 to 0.10 μm) and microporous (<20 µm) structures through the use of layer-by-layer gradient-functional method of applying a nanostructured powder of oxide or intermetallic activator.

Such a set of tools to achieve a technical result allows to obtain nanocatalytic material, wherein the higher efficiency of the process (catalytic activity), due to effective mass transfer in the reaction zone and the presence of through-porosity, higher specific surface of the material provided polydisperse structure, the presence of microscopic pores (up to 30% of the pores have an average diameter of less than 0.02 μm), higher strength, he is of the catalytic layer with a metal carrier.

To create a quick payback and cost-effective production of the most relevant catalytic systems, such as thermochemical catalytic reactor steam reforming fuel and chemical heat recovery, chemical power sources, fuel cells, necessary universal ways of making nanocatalytic material for various purposes on the basis of the common principles of its construction, using high-energy processes in heterogeneous phase transfer.

The proposed method is tested on the specialized area of FSUE "CRISM "Prometey" using plasma and cold spray.

Example 1. In laboratory conditions on the installation of microplasma spraying PNP-2/2270 and the robot Kawasaki FS003 catalytic coating applied using three dispensers containing aluminum, Nickel, aluminum hydroxide, oxides of rare-earth metals, nanostructured activator, on the metal carrier of the alloy HU (no party - 1,3) and HU (no party - 2,4), made in the form of corrugated expanded metal meshes with rhombic holes of various sizes.

Example 2. In laboratory conditions on the installation of cold gas-dynamic spraying "Dime-403" and the robot Kawasaki FS003 catalytic coating applied using tre the dispensers, containing corundum, copper powder and powders of intermetallic compounds, the metal carrier of copper marks M1, made in the form of a perforated tape with round holes of different diameters.

To reduce the influence of the difference of coefficients of thermal expansion on the adhesion strength between adjacent materials in the resulting multilayer structures as a metal carrier were used alloys HU, HU if microplasmin sputtering, and a copper foil mark M1 in the case of cold gas-dynamic spraying. When microplasma spraying powder composition on the metal strip from alloys HU, HU the formation of aluminum oxide in the surface layer of the device. When the cold gas-dynamic spraying a powder composition on the perforated copper foil mark M1 is formed of copper oxide in the surface layer of the device, which has a similar effect.

Physico-chemical properties of the resulting aikaterina material was determined in the following ways:

- specific surface area measured by the BET method by thermal desorption of nitrogen, using samples of size 30×90 mm,

- the adhesion strength was determined by bending the foil with pappelendam layer on the core diameter of 5 mm and study under a microscope for the presence of cracks and the Opera the response as well as using the pin method on the installation testing the gap "Instron 1000",

catalytic activity of samples obtained microplasma spray was performed in a quartz flow reactor in the reaction of catalytic oxidation of carbon monoxide with oxygen in the temperature range from 200 to 500°C in a quartz flow reactor at a flow rate of the reaction mixture of 0.5 DM3/min,

catalytic activity of the samples obtained by cold gas-dynamic spray method was evaluated by voltampere characteristic.

The results are given in tables 1 and 2.

As follows from tables 1 and 2 obtained nanocatalytic materials has a higher catalytic activity, due to effective mass transfer in the reaction zone and the presence of through-porosity, the higher the specific surface of the material provided polydisperse structure, the presence of microscopic pores (up to 30% of the pores have an average diameter of less than 0.02 μm).

The sources of information

1. EN 2127475 C1 IPC NM 4/88, 22F 3/18 "Method of manufacturing embossed porous framework of the hydrogen electrode of the chemical current source", Galkin centuries, Kuliga B. N., Lianozov S. D., shchekoldin S. I., application 97113581/09 from 06.08.1997, publ. 10.03.1999,

2. EN 2110619 C1 IPC SW 11/04 "Electrode for electrochemical processes and the way gender is ing". Closed joint stock company "Techno-TM"application 96117482/25 from 09.09.1996, publ. 10.05.1998,

3. EN 2402839 C1, MKI SW 11/04 "Method of manufacturing electrode" Yakovleva N. In., Tarakanova T. A., Farmakovsky B. C., Ulin, I. C., Sholkin S. E.; Yurkov, M. A.

4. EN 2417841, MKI 01J 23, 01J 23/64, 01J 37/34 "Method of manufacturing a catalytic composite coatings", Vinogradova T. S., Tarakanova T. A., Farmakovsky B. C., Ulin, I. C., Sholkin S. E., M. Yurkov, A., application for invention No. 2009138705 (054808) from 19.10.09,

5. N. M.Popov. The catalysts for purification of gas emissions from industrial productions. M.: Chemistry, 1991.

Table 1
The test results of samples pinakamalaki materials obtained from the known and the proposed method (method microplasma spraying)
MethodSpraying methodNo.Thickness, micronsSquare holes
cm2
The specific surface
m2/g
Porosity (average pore size)Catalytic activity, % Adhesion strength, kg/mm2
mcm%
OfferMicroplasma spraying11000,138,00,02-0,1073,0of 87.00,75
<0,0227,0
21000,741,30,02-0,1079,091,00,73
<0,0221,0
32000,145,00,02-0,1072,095,00,76
<0,0228,0
4 2000,740,60,02-0,1075,093,00,75
<0,0225,0
Known-100-28-36Not MEAs.Not MEAs.80,0-85,00,57

Table 2
The results of the test samples nanocatalytic materials obtained known and the proposed method (using cold spray)
MethodSpraying methodNo.Thickness, micronsSquare holes
cm2
The specific surface m2/gPorosity (average pore size) Voltage-current characteristic at 0.3-0.4 V, mA/cmAdhesion strength, kg/mm2
mcm%
OfferCold gas-dynamic spraying51000,115,00,02-0,1078,037,00,65
<0,0222,0
61000,718,00,02-0,1080,040,00,63
<0,0220,0
72000,119,00,02-0,1077,039,00,60
23,0
82000,7of 17.00,02-0,1081,036,00,62
<0,0219,0
Known-100-13,0Not MEAs.Not MEAs.30,0-35,00,57
Note: the table shows the average value of three samples per pixel.

1. A method of manufacturing a nanocatalytic material, comprising applying the powder composition on the metal media using high-energy processes in heterogeneous phase transfer using two or more Autonomous devices operating with the formation of the catalytically active layer, characterized in that the powder coating composition is produced on a metal carrier having a through hole with a square hole from 0.1 to 0.7 cm2, on the formation of catalytically active layer thickness from 100 to 200 microns.

2. A method of manufacturing a nanocatalytic material under item 1, characterized in that the through holes of the metal carrier is made by the method of notching or otherwise perforating.

3. The method according to p. 1, characterized in that the chemical composition of the metal carrier includes at least one metallic element, and the composition of the powder composition includes at least one oxide of a specified metal element for the formation on the metal carrier of the oxide film.

4. The method according to p. 1, characterized in that the powder coating composition is produced by changing the angle of the spray from 30 to 150°.



 

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FIELD: chemistry.

SUBSTANCE: invention relates to field of catalysis. Described is method of manufacturing geometrical moulded products from catalyst K, in which active mass represents multi-element oxide, which contains Mo element, Bi and/or V elements, as well as one or several elements from series Co, Ni, Fe, Cu and alkali metals, in which highly dispersed mixture is obtained by means of sources of different elements, said mixture is coarsened to powder by pressing, and moulded product V is formed from said coarser powder by agglomeration; said products are divided into undamaged moulded products V+ and damaged moulded products V-, undamaged moulded products V+ are made into moulded products from catalyst K, and damaged moulded products V- are crushed and returned into production of highly dispersed mixture.

EFFECT: reduction of material loss in the process of catalyst production, improvement of working characteristics of catalyst.

5 tbl, 1 ex

FIELD: chemistry.

SUBSTANCE: inventions can be used in field of environment protection. Method of catalyst obtaining includes introduction of base metal in form of ammonium hydroxide or ammonia complex, or in form of organic amine complex, or in form of hydroxide compound into active in redox reactions cubic fluorite CeZrOx material under basic conditions. Catalyst of oxidation includes primary catalytic active metal from group of noble metals, applied on carrier, as well as secondary catalytic active component, which is obtained by ionic exchange between surface of cubic fluorite CeZrOx material and base metal solution and optionally zeolite. Obtained catalysts are used in catalytic device, placing one of them on substrate, around which case is located. Obtained catalysts are also used in method of processing of exhaust gases, passing exhaust gases above them.

EFFECT: inventions make it possible to obtain catalysts for Diesel engines, possessing resistance to hydrothermal treatment and to action of poisons under conditions of system of emission of exhaust gases of Diesel engine, as well as to achieve high degree of conversion of pollutants at lower temperatures.

26 cl, 20 dwg, 4 ex

FIELD: chemistry.

SUBSTANCE: invention relates to methods (versions) of oxidation of carbon monoxide (CO) and volatile organic compounds (VOC), as well as to a catalytic composition for the said processes. The methods include a stage of bringing tail gases of a method of obtaining purified terephthalic acid, containing water vapours and the said CO and VOC, in contact with a catalyst composition, containing a promoter based on a non-noble metal and a catalyst based on a non-noble metal, applied on an oxide carrier, which includes one or several materials, selected from aluminium oxide, silicon dioxide, zirconium dioxide, cerium dioxide and titanium dioxide. The said catalyst composition in fact does not contain platinum group metals, and the said VOC include one or several compounds, selected from methylacetate, methane, methylbromide, benzene, methanol, methylethylketone, butane and butene. The catalyst based on a non-noble metal is selected from the group, consisting of copper (Cu), iron (Fe), cobalt (Co), nickel (Ni) and chrome (Cr), and at least one promoter of the catalyst based on a non-noble metal is selected from the group, consisting of neodymium (Nd), barium (ba), cerium (Ce), lanthanum (La), praseodymium (Pr), magnesium (Mg), calcium (Ca), manganese (Mn), zinc (Zn), niobium (Nb), zirconium (Zr), molybdenum (Mo), tin (Sn), tantalum (Ta) and strontium (Sr).

EFFECT: elaboration of the alternative catalysts, demonstrating high activity and long-lasting quality.

13 cl, 11 dwg, 14 ex

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