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.  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  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  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  , 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'clockBlock 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'clockAfter 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 hoursRestore the active components are in hydrogen at a temperature of 400about5 o'clockThe 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.
FIELD: inorganic synthesis catalysts.
SUBSTANCE: invention provides ammonia synthesis catalyst containing ruthenium as active ingredient supported by boron nitride and/or silicon nitride. Catalyst can be promoted by one ore more metals selected from alkali, alkali-earth metal, or rare-earth metals. Ammonia synthesis process in presence of claimed catalyst is also described.
EFFECT: increased temperature resistance of catalyst under industrial ammonia synthesis conditions.
4 cl, 6 ex
FIELD: processes catalyzed by metal-phosphoro-organic ligand complexes when target product may be selectively extracted and separated from liquid product.
SUBSTANCE: Specification gives description of methods of separation of one or several products of decomposition of phosphoro-organic ligand, one or several reaction byproducts and one or several products from liquid reaction product synthesized continuously and containing one or several non-consumed reagents, catalyst in form of complex of metal-phosphoro-organic ligands, not obligatory free phosphoro-organic ligand, one or several said decomposition products of phosphoro-organic ligand, one or several said reaction byproducts, one or several said products, one or several non-polar solvents and one or several polar solvents by separation of phases where (i) is selectivity of non-polar phase for phosphoro-organic ligand relative to one or several products expressed by ratio of distribution coefficient Ef1 whose magnitudes exceeds about 2.5; (ii)is selectivity of non-polar phase for phosphoro-organic ligand relative to one or several decomposition products expressed by ratio of distribution coefficients Ef2 whose magnitude exceeds proximately 2.5; and (iii) is selectivity of non-polar phase for phosphoro-organic ligand relative to one or several reaction byproducts expressed by ratio of distribution coefficients Ef3 whose magnitude exceeds approximately 2.5 (versions). Description is also given of continuous methods of obtaining one or several products (versions) and reaction mixture containing one or several aldehyde products.
EFFECT: increased conversion of initial materials and selectivity by product; avoidance or exclusion of deactivation of catalyst.
20 cl, 2 tbl
FIELD: inorganic synthesis catalysts.
SUBSTANCE: ammonia synthesis catalyst includes, as catalytically active metal, ruthenium deposited on magnesium oxide having specific surface area at least 40 m2/g, while concentration of ruthenium ranges between 3 and 20 wt % and content of promoter between 0.2 and 0.5 mole per 1 mole ruthenium, said promoter being selected from alkali metals, alkali-earth metals, lanthanides, and mixtures thereof. Regeneration of catalytic components from catalyst comprises following steps: (i) washing-out of promoters from catalyst thereby forming promoter-depleted catalyst and obtaining solution enriched with dissolved promoter hydroxides; (ii) dissolution of magnesium oxide from promoter-depleted catalyst in acidic solvent wherein ruthenium is insoluble and thereby obtaining residual ruthenium metal in solution enriched with dissolved magnesium compound; and (iii) regeneration of residual ruthenium metal from solution enriched with dissolved magnesium compound via liquid-solids separation to form indicated solution enriched with dissolved magnesium compound and ruthenium metal.
EFFECT: increased catalyst activity.
6 cl, 6 ex
FIELD: inorganic synthesis catalysts.
SUBSTANCE: ammonia synthesis catalyst is based on ruthenium on carrier of inoxidizable pure polycrystalline graphite having specific BET surface above 10 m2/g, said graphite being characterized by diffraction pattern comprising only diffraction lines typical of crystalline graphite in absence of corresponding bands of amorphous carbon and which graphite being activated with at least one element selected from barium, cesium, and potassium and formed as pellets with minimal dimensions 2x2 mm (diameter x height). Catalyst is prepared by impregnating above-defined catalyst with aqueous potassium ruthenate solution, removing water, drying, reduction to ruthenium metal in hydrogen flow, cooling in nitrogen flow, water flushing-mediated removal of potassium, impregnation with aqueous solution of BaNO3 and/or CsOH, and/or KOH followed by removal of water and pelletizing of catalyst.
EFFECT: increased activity of catalyst even when charging ruthenium in amount considerably below known amounts and increased resistance of catalyst to methane formation.
12 cl, 1 tbl
FIELD: organic synthesis catalysts.
SUBSTANCE: invention is dealing with preparation of homogenous catalyst for production of acrylic acid esters according to metathesis reaction of malates with ethylene. Two variants of preparing catalyst are developed. In particular, catalyst of general formula , wherein A1, A2 represent chlorine, L dihydroimidazole ligand, R1, R2, R3, the same or different, are substituents selected from hydrogen, alkyl, trialkylsylyl, and alkoxy; and catalyst of formula are proposed. Use of these catalysts allows number of cycles of metathesis reaction of dialkyl malates with ethylene to be increased both under moderate temperature (about 50°C) conditions when reaction is carried out without distillation of product and at temperatures about 120°C when acrylate produced is distilled out of reaction mixture. Catalytic composition is further developed allowing not only number of reaction cycles but also catalyst lifetime to be increased. Such composition contains indicated catalyst and 2-isopropoxystyrene or its derivative at molar ratio 1:(5-500), respectively.
EFFECT: increased catalyst activity and lifetime.
7 cl, 4 tbl, 28 ex
FIELD: gas treatment catalysts.
SUBSTANCE: invention concerns environmental protection area and aims at neutralizing toxic components of emission gases and, more specifically, related to a method of preparing catalyst for oxidative treatment of gases polluted by hydrocarbons and carbon monoxide. Invention provides catalyst supported by stainless steel containing 0.05-0.15 wt % ruthenium or ruthenium in the same quantity combined with platinum or palladium in quantity not exceeding 0.05 wt %. Catalyst preparation method is also described.
EFFECT: increased degree of removal of hydrocarbons, increased strength of catalyst, and reduced price of catalyst.
2 cl, 2 tbl
FIELD: gas treatment.
SUBSTANCE: invention relates to processes of removing carbon monoxide from gas mixtures containing, except hydrogen, carbon dioxide. This process is an important step for production of pure hydrogen or hydrogen-containing gas, e.g. in ammonia synthesis. Catalyst for removing carbon monoxide from hydrogen-containing gas represents permeable composite material containing combination of phases of catalytically active group VIII metal or their alloy, oxide-type carrier, and metallic copper or copper metal containing alloy, composite-forming grain size being less than 0.5 mm and permeability of composite exceeding 10-14 m2. Catalyst preparation procedure as well as processes of removing carbon monoxide from hydrogen-containing gas using it are also described.
EFFECT: increased activity and selectivity of catalyst.
20 cl, 3 dwg, 8 ex
FIELD: hydrogenation-dehydrogenation catalysts.
SUBSTANCE: invention relates to novel ruthenium catalysts, method for preparation thereof, and to employment thereof for catalytic hydrogenation of mono- and oligosaccharides in production of corresponding sugar alcohols. Ruthenium hydrogenation catalyst contains ruthenium supported by amorphous silica-based carrier, content of ruthenium being 0.2 to 7% of the weight of carrier, while carrier contains at least 90% silica and less than 10% of crystalline silicon dioxide phases. Catalyst is prepared by single or multiple treatment of carrier material with halogen-free solution of low-molecular weight ruthenium compound and subsequent drying of treated material at temperature not lower than 200°C immediately followed by reduction of dried material with hydrogen at 100 to 350°C. Herein disclosed is also a process for liquid-phase production of sugar alcohols (excepting sorbitol) via catalytic hydrogenation of corresponding mono- and oligosaccharides in presence of proposed catalysts.
EFFECT: increased activity and selectivity of catalysts.
16 cl, 4 tbl, 7 ex
FIELD: chemistry, organic, processing of hydrocarbons.
SUBSTANCE: invention is related to an improved method for hydroprocessing of hydrocarbon raw stock containing sulphur- and/or nitrogen-bearing contaminants. The method comprises the first contact interaction of hydrocarbon raw stock with hydrogen in the presence of at least one first catalyst based on VIII group metals on an acidic carrier, the carrier being selected from the group of zeolites and zeolite-bearing carriers, and then the flow leaving the first catalyst directly contacts hydrogen in the presence of at least one second catalyst based on a VIII group metal on a less acidic solid carrier, said solid carrier being selected from the group of carriers based on silicon dioxide-aluminium oxide and other solid carriers that are not zeolites. Said combination of two catalyst layers allows processing of raw stock with a high content of contaminating impurities without high-level cracking that involves the use of highly acidic carriers.
EFFECT: processing of hydrocarbon raw stock with contaminating impurities without high-level cracking.
14 cl, 1 ex
SUBSTANCE: catalytic composition contains the catalyst of olefin metathesis as one component, and phenol derivatives as another component, at proportion: 1 mol equivalent of catalyst to 200-1500 mol equivalents of phenol derivatives. In another modification, the catalytic composition contains as the second component the alcohol derivates which do not contain the C-H fragments at α-position to hydroxyl function, at proportion: 1 mol equivalent of catalyst to 200-1500 mol equivalents of alcohol derivatives. Another one modification of the invention has quinine or its derivatives as the second component of the catalytic composition. Particularly, the ruthenium complex with formula can be used as a catalyst of olefin metathesis.
EFFECT: number of catalyst turnover and life-time of catalyst in metathesis reaction of dialkylmaleate with ethylene are increased.
10 cl, 12 ex, 6 tbl
FIELD: heterogeneous catalysts.
SUBSTANCE: catalyst contains porous carrier, buffer layer, interphase layer, and catalytically active layer on the surface wherein carrier has average pore size from 1 to 1000 μm and is selected from foam, felt, and combination thereof. Buffer layer is located between carrier and interphase layer and the latter between catalytically active layer and buffer layer. Catalyst preparation process comprises precipitation of buffer layer from vapor phase onto porous carrier and precipitation of interphase layer onto buffer layer. Catalytic processes involving the catalyst and relevant apparatus are also described.
EFFECT: improved heat expansion coefficients, resistance to temperature variation, and reduced side reactions such as coking.
55 cl, 4 dwg
FIELD: hydrogenation-dehydrogenation catalysts.
SUBSTANCE: palladium-containing hydrogenation catalyst, which can be used to control rate of autocatalytic hydrogenation reactions, is prepared by hydrogen-mediated reduction of bivalent palladium from starting compound into zero-valence palladium and precipitation of reduced zero-valence palladium on carbon material, wherein said starting material is tetraaqua-palladium(II) perchlorate and said carbon material is nano-cluster carbon black. Reduction of palladium from starting compound and precipitation of zero-valence palladium on carbon material are accomplished by separate portions.
EFFECT: increased catalytic activity, enabled catalyst preparation under milder conditions, and reduced preparation cost.
1 dwg, 1 tbl, 12 ex
FIELD: industrial organic synthesis catalysts.
SUBSTANCE: invention relates to environmentally friendly processes for production of isoalkanes via gas-phase skeletal isomerization of linear alkanes in presence of catalyst. Invention provides catalyst for production of hexane isomers through skeletal isomerization of n-hexane, which catalyst contains sulfurized zirconium-aluminum dioxide supplemented by platinum and has concentration of Lewis acid sites on its surface 220-250 μmole/g. Catalyst is prepared by precipitation of combined zirconium-aluminum hydroxide from zirconium and aluminum nitrates followed by deposition of sulfate and calcination in air flow before further treatment with platinum salts. Hexane isomer production process in presence of above-defined cat is also described.
EFFECT: increased catalyst activity.
5 cl, 2 tbl, 6 ex
FIELD: catalyst preparation methods.
SUBSTANCE: invention relates to methods for preparing carbon monoxide-conversion catalysts used in production of hydrogen, nitrogen-hydrogen mixture, and other hydrogen-containing gases. According to first option, active catalyst component, i.e. iron compound, is precipitated from solution with precipitation reagent, whereupon precipitate is separated from mother liquor and washed to form catalyst mass, which is molded and subjected to heat treatment, re-washed, mixed with chromic anhydride and subjected to final heat treatment: at 280-420°C after molding or at 50-200°C before molding of catalyst mass. According to second option, iron compound is first mixed with promoting additives and cations of promoting additives are precipitated jointly with iron cations, resulting precipitate is separated from mother liquor, washed and subjected to heat treatment, re-washed, mixed with chromic anhydride and subjected to final heat treatment: at 280-420°C after molding or at 50-200°C before molding of catalyst mass. As iron compound in the first and second options, ferrous and ferric sulfates and, as precipitation reagent, carbonate salts or corresponding hydroxides are utilized. Promoting additives are selected from Cu, Mn, and Al or, in the second option, their mixture.
EFFECT: reduced content of sulfur in finished catalyst at the same catalyst activity.
3 cl, 1 tbl, 12 ex
FIELD: catalyst preparation methods.
SUBSTANCE: invention, in particular, relates to catalyst based on synthetic mesoporous crystalline materials and provides hydrocarbon conversion catalyst composed of: group VIII metal/SO4 2-/ZrO2-EOx, where E represents element of the group III or IV of Mendeleev's periodic table, x = 1.5 or 2, content of SO4 2- is 0.1 to 10% by weight, ZrO2/EOx molar ratio is 1:(0.1-1.0), which has porous crystalline structure with specific surface 300-800 m2/g and summary pore volume 0.3-0.8 cm3/g. Preparation method comprises precipitation of zirconium compounds, in particular zirconium hydroxide or zirconyl, under hydrothermal conditions in presence of surfactant to form mesoporous phase, which is stabilized with stabilizing agents: group III and IV elements. When stabilization is achieved, if necessary, acidity is adjusted and group VIII metal is added.
EFFECT: increased specific surface area and heat resistance at simplified technology.
9 cl, 2 dwg, 2 tbl, 6 ex
FIELD: chemical industry; methods of production of zirconium oxides
SUBSTANCE: the invention is pertaining to the field of chemical industry, in particular, to the methods of obtaining of zirconium oxide for production of the catalytic agents used, for example, in the reactions of the organic synthesis. The invention presents the method of obtaining of zirconium oxide for production of the catalytic agents, which includes the operations of dissolution of the zirconium salt in water, treatment of the solution with the alkaline reactant, settling of the metals hydroxides, filtration, separation of the mother-liquor from the settlings, the settlings water flushing, its drying, calcination and granulation and-or granulation by molding. At that dissolution of the source zirconium chloride and-or zirconium oxychloride is conducted in the sodium chloride solution with concentration of 200-250 g/dc3 till reaching of the concentration of zirconium of 20-120 g/dc3. Settling of zirconium oxyhydrate is conducted by the adding the initial chloride solution in the solution of the sodium hydroxide with concentration of 20-80 g/dm3 up to reaching the suspension pH equilibrium value - 5-8. Then the suspension is filtered up to the zirconium oxyhydrate pasta residual humidity of 40-80 %. The mother chloride solution is separated from the settlings of zirconium oxyhydrate and again use it for dissolution of the next batch of zirconium chloride and-or zirconium oxychloride. The settlings of zirconium oxyhydrate are subjected to drying at 80-100°C within 2-6 hours, then the dry settlings are suspended in the water at the ratio of liquid to solid L:S = (5-10 :1, the suspension is filtered, the sediment on the filter is flushed by water, the chlorides are wash off up to the residual concentration of ions of chlorine in the flush waters of 0.1-0.5 g/dm3, divided into 2 parts, one of which in amount of 60-80 % is subjected to drying and calcinations at the temperatures of 300-600°C, and other part in amount of 20-40 % is mixed with the calcined part of the settlings and subjected to granulation by extrusion at simultaneous heating and dehydration of the damp mixture of zirconium oxide and zirconium oxyhydrate with production of the target product. The technical result of the invention is improvement of quality of the produced zirconium oxide for production of the catalytic agents due to provision of the opportunity to use ZrO2 for the subsequent production of the various catalytic agents of the wide range of application and thereby improving the consumer properties of the produced production.
EFFECT: the invention ensures improvement of the quality of the produced zirconium oxide for production of the catalytic agents with improved consumer properties.
FIELD: catalyst preparation methods.
SUBSTANCE: invention provides Fischer-Tropsch catalyst, which consists essentially of cobalt oxide deposited on inert carrier essentially composed of alumina, said cobalt oxide being consisted essentially of crystals with average particle size between 20 and 80 Å. Catalyst preparation procedure comprises following stages: (i) preparing alumina-supported intermediate compound having general formula I: [Co2+ 1-xAl+3 x(OH)2]x+[An- x/n]·mH2O (I), wherein x ranges from 0.2 to 0.4, preferably from 0.25 to 0.35; A represents anion; x/n number of anions required to neutralize positive charge; and m ranges from 0 to 6 and preferably is equal to 4; (ii) calcining intermediate compound I to form crystalline cobalt oxide. Invention also described a Fischer-Tropsch process for production of paraffin hydrocarbons in presence of above-defined catalyst.
EFFECT: optimized catalyst composition.
16 cl, 12 tbl, 2 ex
FIELD: chemical industry; materials and the methods for the catalyst carrier manufacture.
SUBSTANCE: the invention is pertaining to the new mixed oxides produced from ceric oxide and zirconium oxide, which can used as the catalyzers or the catalyzers carriers for purification of the combustion engine exhaust gases. The mixed oxide possesses the polyphase cubical form of the crystallization and oxygenous capacity of at least 260/ micromoles of O2 /g of the sample and the speed of the oxygen extraction of more than 1.0 mg-O2/m2-minute, which are measured after combustion within 4 hours at the temperature of 1000°C. The invention also presents the substrate with the cover containing the indicated mixed oxide. The method of production of the polycrystallic particles of the indicated mixed ceric-zirconium oxide includes the following stages: i) production of the solution of the mixed salt which are containing, at least, one salt of cerium and, at least, one salt of zirconium in the concentration, sufficient for formation of the polycrystallic particles of the corresponding dry product on the basis of the mixed oxide. At that the indicated particles have the cerium-oxide component and zirconium-oxide component, in which these components are distributed inside the subcrystalline structure of the particles in such a manner, that each crystallite in the particle consists of a set of the adjacent one to another domains, in which the atomic ratios of Ce:Zr which are inherited by the adjacent to each other domains, are characterized by the degree of the non-uniformity with respect to each other and determined by means of the method of the X-ray dissipation the small angles and expressed by the normalized intensity of the dissipation I(Q) within the limits from approximately 47 up to approximately 119 at vector of dissipation Q, equal to 0.10 A-1; ii) treatment of the solution of the mixed salt produced in compliance with the stage (i),with the help of the base with formation of sediment; iii) treatment of the sediment produced in compliance with the stage (ii),using the oxidative agent in amount, sufficient for oxidizing Ce+3 up to Ce+4; iv) washing and drying of the residue produced in compliance with the stage (iii); and v) calcination of the dry sediment produced in compliance with the stage (iv),as the result there are produced polycrystallic particles of the oxide of ceric and zirconium in the form of the mixed oxide with the above indicated characteristics. The technical result is the produced mixed oxide possesses both the high oxygenous capacitance, and the heightened speed of the oxygen return in the conditions of the high temperatures.
EFFECT: the invention ensures production of the mixed oxide manufactured from ceric oxide and zirconium oxide and possessing the high oxygenous capacitance and the heightened speed of the oxygen return in the conditions of the high temperatures.
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