The catalyst for reduction of nitrogen oxides by hydrocarbons in an oxidizing atmosphere and method thereof

 

(57) Abstract:

Usage: in catalytic chemistry, in particular in the catalysts for purification of any gas in an oxidizing atmosphere containing flue gases of thermal power plants, exhaust gases of cars, as well as gases from nitric acid production. The inventive catalytic oxide composition f-ly 1: MeO-ZrO2where IU CA, Sr, Ba, Y, Ce; composition MeO 2 10 mol. and the rest of ZrO2or f-crystals 2: Al2O3-SrO-ZrO2composition (in mol.): Al2O3-25,0-50,0 ZrO 2,5 - 3,8, ZrO2-47,5-71,2. The compositions of f-crystals 1 are given either by coprecipitation of the components or by mixing for f-crystals 2 and subsequent stages of forming, drying and calcination at 700 100°C. These catalysts provide a 100% degree of conversion of oxides of nitrogen at the reaction temperature recovery of hydrocarbons in an oxidizing atmosphere. 2 S. and 1 C.p. f-crystals, 1 table.

The invention relates to catalysts for efficient removal of nitrogen oxides in oxidizing conditions and the method of obtaining them, characterized by a high degree of purification, selectivity, chemical and thermal stability. The proposed catalyst is effective for cleaning of any gas with an oxidizing atmosphere, stereoty.

The nature of the catalyst and technological design process flue gas (EXHAUST gas) from the NOxdepend on the ratio of (a) oxidizing and reducing components in the EXHAUST gas, and restorative components, namely:

1. If = 1, then the most common catalytic systems used in these cases are the metals Cu, Pd, Pt, Rh deposited on porous media (Al2O3, ZrO2, zeolites) [1]. However, these catalysts do not provide efficient purification from nitrogen oxides in an oxidizing atmosphere containing a large amount of oxygen.

2. If >1 (such oxidizing mixture formed from internal combustion engines, by operation of a thermal power plant, and so on), then there are two variants of the process:

(a) For cleaning the EXHAUST gas from the NOxuse the method of selective catalytic reduction of NOxthe ammonia. For this process using the catalysts, in which the role of the active component performs deficient oxides of vanadium, tungsten, titanium [2] While there are difficulties associated with transporting, storing and regulating the supply metered quantities of ammonia.

b) For purification of EXHAUST gas from and NOxprimadaya composition Cu/zeolite [3], Cu/Al2O3, Cu/Al Si O [4] the copper content varies in the range 2-5%

The specified catalyst [3] is the closest to the proposed. The method of obtaining this catalyst is repeated impregnation of porous media (zeolite) with a solution of nitrate of copper at a temperature of 80aboutWith; and then washed with water, dried at 110aboutS, 12 h and calcined at 600aboutC, 3 hours the Catalyst may have a different shape: granules in the form of cuttings, blocks cell structure.

The main disadvantage of this catalyst is relatively low degree of purification from the NOx. The degree of conversion of NOxdepending on the reaction temperature passes through a maximum value corresponding to the temperature of 500aboutFrom [5] which makes it impossible to increase the degree of conversion by increasing the reaction temperature. In addition, it should be noted the technological complexity of the preparation of the catalyst, due to the presence of multiple impregnation.

The aim of the invention is to obtain a catalyst to achieve a high degree of purification from the NOxby restoring the last hydrocarbons in the presence of excess oxygen, the possession is the catalyst based on ZrO2containing MeO < 10 mol. where IU CA, Sr, Ba, Al, Y, Ce, representing cuttings of size 2,5x3,5 mm; and the catalyst Al-Sr-Zr-O containing 25Al2O350 mol. and SrO 2-10 mol. the rest of ZrO2representing tube dimensions: dEXT2.5 mm and dint.1 mm, 15-20 mm l or microblock in the form of a hexagon with triangular channels and a wall thickness of 1 mm, the Number of channels in the cross-section of microbiota was 24-30 pieces. The proposed catalysts are received either by the deposition of the components, or their mixture with the subsequent stages of forming, drying and calcination at appropriate temperatures.

Distinctive features of the proposed catalyst are:

1. The nature of the active component, which is based on ZrO2with the addition of MeO, where Me is Ca, Sr, Ba, Al. Y, Ce; or Al2O3-SrO-ZrO2.

2. The method of preparation of the catalyst, consisting either in the deposition of the respective components or the mixture of fresh and dried binary or ternary compositions.

3. Other temperature range of formation of the catalyst.

A distinctive feature of the proposed catalyst for purification of EXHAUST gas from the NOxby catalytics Oginga composition for this process, which would not reduce the degree of conversion of NOxwith increasing reaction temperature, which allows to achieve 100% conversion of NOx.

The catalytic properties of the samples prepared in accordance with the foregoing compositions and method of synthesis, in the reduction reaction of NOxwas evaluated by the degree of conversion of NO to the standard mixture: 1000 ppm NO, 1300 ppm C3H8, 1 vol. ABOUT2the rest is Not at flow rate of 4000 h-1. For some catalysts was studied the influence of the oxygen content of the mixture (CO21 -10 about.) and volumetric flow rate (V 4000-32000 h-1on the activity of the samples.In addition, evaluated the degree of conversion of propane to co and CO2.

Source materials used in the synthesis of the catalyst, get:

ZrO(NO3)22H2O under MRTU 6-09-2376-65, followed by dissolving in NGO3and distilled H2About when obtaining a solution with a concentration of 100 g ZrO2/l

CAC2ABOUT4H2About under MRTU 6-09-6656-70, followed by dissolving in distilled H2About when obtaining a solution with a concentration of 100 g Cao/liter

Sr(NO3)2according to THE 5429-50 with subsequent dissolution soglasno GOST 3777-69, followed by dissolving in distilled H2About when obtaining a solution with a concentration of 100 g BaO/L.

AlOOH1,5H2About powder perezajennogo aluminum hydroxide pseudoboehmite structure with a particle size of 15 μm, produced by nitrate-ammonia technology.

P R I m e R 1. Salt solution obtained by mixing an 11.7 ml CAC2ABOUT4and 488,3 ml solution of ZrO(NO3)2, precipitated with ammonia solution at pH 9 and 70aboutWith subsequent keeping the suspension under these conditions for 2 h, after which the suspension was filtered, the precipitate washed with distilled water until no nitrate in the filtrate; the resulting paste is molded in the form of cuttings, and then dried at 110aboutS, 12 h and calcined in a stream of air for 4 h at 700aboutC. the resulting catalyst has the composition: 5 mol. CaO 95 mol. ZrO2, physico-chemical and catalytic properties of which are given in the table.

P R I m m e R 2. Similar to example 1. The difference is that the deposition serves the solution obtained by the mixture of 8.5 ml of Sr(NO3)2and 491,5 ml ZrO(NO3)2. The resulting catalyst has the composition: 2 mol. SrO, 98 mol. ZrO2, physico-chemical and catalytic properties of which are given in the table.

P R I m e R 3. UB>2and 478,8 ml ZrO(NO3)2. The resulting catalyst has the composition: 5 mol. SrO and 95 mol. ZrO2, physico-chemical and catalytic properties of which are given in the table.

P R I m e R 4. Similar to example 1. The difference is that the deposition submit a solution obtained by mixing and 42.7 ml of Sr(NO3)2and 457,3 ml ZrO(NO3)2and the calcination is carried out at 720aboutC. the resulting catalyst has the composition: 10 mol. SrO 90 mol. ZrO2, physico-chemical and catalytic properties of which are given in the table.

P R I m e R 5. Similar to example 1. The difference is that the deposition submit a solution obtained by mixing a 30.7 ml of Ba(NO3)2and 469,3 ml ZrO(NO3)2and the calcination is carried out at a temperature of 750aboutC. the resulting catalyst has the composition: 5 mol. HLW 95 mol. ZrO2, physico-chemical and catalytic properties of which are given in the table.

P R I m e R 6. Similar to example 1. The difference is that the deposition submit a solution obtained by mixing 48.6 ml Y(NO3)3and 451,4 ml SrO(NO3)2. The resulting catalyst has a composition of 10 mol. Y2O3, 90 mol. ZrO2, physico-chemical and catalytic properties which bring the PRS, the obtained mixture of 61.5 ml of Ce(NO3)3and 438,5 ml ZrO(NO3)2. The resulting catalyst has the composition: 5 mol. Ce2O3, 95 mol. ZrO2, physico-chemical and catalytic properties of which are given in the table.

P R I m e R 8. 161 g wet paste obtained according to the procedure described in example 3, containing 80.2% of N2Oh, is mixed with 80 g of dry powder transitionally composition of the same composition in the Z-shaped mixer for 15 minutes the resulting paste is molded by extrusion in the form of tubes dimensions: dEXT.7.8 mm, dint.4 mm, the Sample is dried for 20 h in air, then in a drying Cabinet at 110aboutS, 12 h, the Calcination is carried out in a muffle furnace at 700aboutWith 4 hours. The resulting catalyst has the composition: 5 mol. SrO; 95 mol. ZrO2physico-chemical and catalytic properties of which are given in the table.

P R I m e R 9. Analogous to example 8. The difference lies in the fact that the sample calcined at 900aboutC. the resulting catalyst has the composition: 5 mol. SrO; 95 mol. ZrO2, physico-chemical and catalytic properties of which are given in the table.

P R I m e R 10. Analogous to example 8. The difference is that mixed with 145 g of ZrO(OH)2with the second catalyst calcined in a muffle furnace at 1000aboutC, 4 h the resulting catalyst has the composition: 75 mol. Al2O3; 25 mol. ZrO2. Physico-chemical and catalytic properties of which are given in the table.

P R I m e R 11. Analogous to example 8. The difference is that the mix is 37.2 g of powder perezajennogo aluminum hydroxide with 66,9 g of dry powder transitionally composition obtained according to example 3, and to 123.5 g wet transitionally compositions containing 83,8% N2About; the resulting paste is molded in the form of microblocks, air-dried for 20 h, then in a drying Cabinet at 110aboutS, 12 h, the Calcination is carried out in a muffle furnace at 900aboutC. the resulting catalyst has the composition: 25 mol. Al2O3; of 3.8 mol. SrO; 71,2 mol. ZrO2, physico-chemical and catalytic properties of which are given in the table.

P R I m e R 12. Analogous to example 11. The difference is that mix 77,8 g perezajennogo aluminum hydroxide with 37 g of dry powder transitionally composition and 144,4 g wet transitionally compositions containing 83,8% N2O. the resulting catalyst has the composition: 50 mol. Al2O3; 2,5 mol. SrO and 47.5 mol. ZrO2, physico-chemical and catalytic properties of which are given in eacli recovery NO by hydrocarbons in an oxidizing atmosphere. It should be noted that in the prototype as a reducing agent was used more reactive hydrocarbon is propylene, and offer more sustainable propane. According to [5] the same degree of conversion of NOxunder comparable reaction conditions in the case of propylene is achieved at temperatures in the 100aboutC lower than when using propane. But even with this in mind, the table shows that tranzitionale catalysts under comparable reaction conditions on the activity are not inferior to the prototype. The proposed activity of the catalysts increases significantly, reaching 100% degree of conversion of NO, by changing reaction conditions:

1. The higher oxygen content in the original reaction mixture (table). This makes possible the application of the proposed catalysts for neutralization of mixtures with a high content of oxygen.

2. Increasing the reaction temperature. If we take into account that the catalysts obtained according to the prototype [3] raising the reaction temperature is accompanied by a reduction in the degree of conversion of NO, the proposed catalysts are more efficient and heat-resistant. This predlagajemaja catalysts (table).

Introduction to composition MeO-ZrO2where Me is Ca, Sr, Ba, Y, Ce, Al2O3in the amount of 25-50 mol. reduces the efficiency of the catalysts, however, it is higher than on the prototype, at higher temperatures the reaction (table). In addition, it allows to obtain catalysts in the form of tubes, microblocks that, in turn, contributes to a more rational design process of purification of the EXHAUST gas and reduces the loading of the catalyst. The latter is confirmed by the fact that when using the catalyst in the form of microbiota weighed samples were approximately 2.5 times less than when using cuttings, obtained by deposition (see table).

1. The catalyst for reduction of nitrogen oxides by hydrocarbons in an oxidizing atmosphere, characterized in that it is a composition MeO ZrO2where Me is Ca, Sr, Ba, Y, Ce, composition mol.

MeO 2 10

ZrO2Else

or composition of Al2O3SrO ZrO2composition, mol.

Al2O325,0 50,0

SrO 2,5 3,8

ZrO247,5 71,2

2. The method of producing catalyst for reduction of nitrogen oxides by hydrocarbons in an oxidizing atmosphere, characterized in that the components of the composition MeO ZrO2where Me is Ca, Sr, Ba, Y, Ce, taken in the ratio of 2 to 10 mol. in the or ammonia with subsequent stages of formation, drying and calcination at 700 - 750oC.

3. The method of producing catalyst for reduction of nitrogen oxides by hydrocarbons in an oxidizing atmosphere, characterized in that mix 25 to 50 mol. in terms of Al2O3perezajennogo aluminum hydroxide and 50 to 75 mol. on calcined strontium-zirconium composition SrO ZrO2obtained by coprecipitation from solutions of salts with an aqueous solution of ammonia, followed by the stages of forming, drying and calcination at 700 - 1000oC.

 

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