CN106607087B - Catalyst for catalytic conversion of nitrogen-containing compounds by carbon monoxide - Google Patents
Catalyst for catalytic conversion of nitrogen-containing compounds by carbon monoxide Download PDFInfo
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Abstract
The invention relates to a catalyst for catalytic conversion of nitrogen-containing compounds by carbon monoxide under low temperature, which mainly solves the problems that the catalyst in the prior art has low activity under low temperature or poor selectivity under high temperature, and can not effectively remove the nitrogen-containing compounds. The invention better solves the problem by adopting the technical scheme that copper oxide is loaded on the SAPO-34 molecular sieve carrier and is modified by rare earth oxide and VIB and VIIB group metal oxide, and the invention can be used in the industrial production of converting nitrogen-containing compounds at low temperature.
Description
Technical Field
The invention relates to a catalyst for catalytic conversion of nitrogen-containing compounds by carbon monoxide, in particular to a catalyst for low-temperature catalytic conversion of nitrogen-containing compounds by carbon monoxide.
Background
With the rapid development of modern industries in countries around the world, atmospheric pollution has become an increasingly serious global problem. NOx is one of the recognized major pollutants of the atmosphere. In China, the developing countries mainly use coal as fuel, the energy structure mainly using coal in China cannot be changed in a long time in the future, and nitrogen oxides generated by the coal are main factors for generating acid rain, photochemical smog and related environmental damages. Acid rain can cause damage to soil productivity, crops, forests, inland lakes, buildings, and the like. In addition, NOx can induce many human diseases, which are extremely harmful to human health, especially to the growth and development of children.
US patent 6685897 discloses a catalyst for exchanging molecular sieves with alkali metal cations, which has a high specific surface area and a large pore structure, and the operating temperature of the catalyst is in the range of 150 to 450 ℃.
U.S. Pat. No. 4,989,825 proposes a process for catalytic reduction of NOx using ammonia as a reducing agent, the catalyst used being TiO2-V2O5-Mo2O3As an active component, a nitrogen oxide reduction catalyst is used at a temperature greater than 350 ℃, which is suitable for use under moderate temperature conditions.
Chinese patent CN01131952.6 discloses a catalyst for ammonia selective reduction of nitrogen oxides, which is an alumina-supported copper-manganese composite oxide catalyst, and has high activity and stability at a reaction temperature of 150-350 ℃.
Chinese patent CN87100737A discloses a catalyst for selective reduction of nitrogen oxides to nitrogen in the presence of ammonia, which comprises cobalt oxide and zeolite as main active components, and a small amount of oxide selected from vanadium and copper as a promoter. The catalyst belongs to a mixed oxide type catalyst, and can reduce the NOx content of 1600ppm by 90 percent at 350 ℃.
US patent No. 4981659 discloses a catalyst for the selective reduction of NOx to nitrogen in the presence of a hydrogen reducing agent. The catalyst uses VIII group noble metal, and the active component is formed by mixing one or more of Pt, Pd and Ir. The novel feature of the catalyst is that hydrophobic organic polymer is used as catalyst carrier. Since the organic polymer has poor heat resistance, the NOx conversion is less than 90% when the catalyst is used at a temperature exceeding 200 ℃.
The technical scheme that copper oxide is loaded on an SAPO-34 molecular sieve carrier and is used as an active component, and modification is carried out by using rare earth oxide and VIB and VIIB group metal oxide is adopted, so that the obtained catalyst is used in industrial waste gas containing carbon monoxide and nitrogen-containing compounds, the carbon monoxide can be effectively converted into nitrogen oxides and methyl nitrite in the nitrogen-containing compounds, the nitrogen-containing compounds are removed, the carbon monoxide content is reduced, and the catalyst has high activity, high selectivity and longer service life.
Disclosure of Invention
The invention aims to solve the technical problems of low activity, poor stability and high reaction temperature of the existing ammonia selective reduction nitrogen oxide catalyst, and provides a catalyst for reducing nitrogen compounds by carbon monoxide, which has the characteristics of low reaction temperature, high reaction activity and high stability when being used for catalyzing and converting nitrogen compounds.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a catalyst for the low-temperature catalytic conversion of nitrogen-containing compounds by carbon monoxide comprises the following components in percentage by weight:
a) 1-10% of copper oxide;
b) 0.1-5% of VIB and VIIB group metal oxides;
c) 0-5% of rare earth oxide;
d) 80-99% of SAPO-34 molecular sieve carrier.
In the technical scheme, the content of the copper oxide is preferably 2-8%, the content of the VIB and VIIB group metal oxides is preferably 0.5-3%, and the content of the rare earth oxides is preferably 0.2-3%, based on the weight percentage of the catalyst.
In the above technical scheme, preferably, the SAPO-34 molecular sieve support has a Si/Al molar ratio of SiO2/Al2O3The preferable range is 0.1-1, the preferable scheme of the VIB and VIIB metal oxide is at least one selected from Cr, Mo, W, Mn and Re, and the preferable scheme of the rare earth oxide is at least one selected from La, Ce, Pr and Nd.
In the above embodiment, the weight ratio of the metal oxide of group VIB of the periodic Table to the metal oxide of group VIIB of the periodic Table is preferably (1:3) to (3: 1).
In the above technical solution, the nitrogen-containing compound includes nitrogen oxide and methyl nitrite.
The catalyst is used as follows: a method for catalytic conversion of nitrogen-containing compounds by carbon monoxide is carried out at a reaction temperature of 200-350 ℃ and a gas space velocity of 500-5000 h-1And under the reaction condition that the pressure is 0-2 MPa, the mixture of the carbon monoxide and the nitrogen-containing compound is contacted with the catalyst to remove the nitrogen-containing compound in the mixture.
In the technical scheme, the preferable reaction temperature range is 250-300 ℃.
In the technical scheme, the preferable reaction pressure range is 0.01-1 MPa.
In the technical scheme, the preferable air speed range is 600-4000 h-1。
The preparation method of the catalyst is an isometric impregnation method, namely loading the required active component and modifier on the surface of the SAPO-34 molecular sieve carrier by adopting an isometric impregnation method, and drying and roasting to obtain the finished product of the catalyst.
Currently, NH is generally used for catalytic removal of nitrogen oxides3Selective catalytic reduction (NH)3SCR), which, although industrially applied, still has a number of drawbacks: (1) NH (NH)3The gas is a toxic corrosive gas, is troublesome to store and transport, has high requirements on pipeline equipment and is expensive to manufacture; (2) in this process, NH3The addition amount needs to be controlled, so that leakage is easy or reaction is incomplete, and secondary pollution is caused; (3) the working temperature range is narrow and is not easy to control. Therefore, a replaceable NH is sought3The reducing agent has great significance. CO is adopted as a reducing agent, and NH is solved3The method has the advantages that the method is a reaction system in which two nitrogen-containing compounds and carbon monoxide exist simultaneously, the trouble of adding a reducing agent is eliminated, partial carbon monoxide is consumed while the nitrogen-containing compounds are converted, and the environment protection effect is enhanced.
The catalyst for catalytic conversion of nitrogen-containing compounds by carbon monoxide effectively overcomes the defects of poor catalyst stability and low conversion rate of nitrogen-containing compounds in the prior art, and the conversion rate of the nitrogen-containing compounds can reach 100% by optimizing reaction conditions, so that a better technical effect is achieved.
The invention is further illustrated by the following examples.
Detailed Description
[ example 1 ]
Selecting SiO2/Al2O3SAPO-34 molecular sieve with the molar ratio of 0.1 is taken as a carrier, and the water absorption of the carrier is firstly measured. Preparing a mixed solution containing 3 percent of copper oxide, 8 percent of chromium oxide and 0.5 percent of lanthanum oxide according to the water absorption rate and the planned load capacity of the carrier, soaking for 5 hours by adopting an isometric impregnation method, drying in a 120 ℃ oven, and roasting for 10 hours in a 580 ℃ muffle furnace to obtain the catalyst 3 percent of Cu8 percent of Cr0.5 percent of La/SAPO-34 for converting the carbon monoxide into the nitrogen-containing compound at the low temperature.
[ example 2 ]
Selecting SiO2/Al2O3SAPO-34 molecular sieve with the molar ratio of 0.2 is taken as a carrier, and the water absorption of the carrier is firstly measured. According to the measured water absorption rate and the planned load capacity of the carrier, preparing a mixed solution containing 1% of copper oxide, 2% of molybdenum oxide and 5% of cerium oxide, soaking for 5 hours by adopting an isometric immersion method, drying in a 120 ℃ oven, and roasting in a 580 ℃ muffle furnace for 10 hours to obtain the catalyst 1% of Cu 2% of Mo 5% of Ce/SAPO-34 for converting the carbon monoxide into the nitrogen-containing compound at the low temperature.
[ example 3 ]
Selecting SiO2/Al2O3SAPO-34 molecular sieve with a molar ratio of 0.4 is taken as a carrier, and the water absorption of the carrier is firstly measured. According to the measured water absorption rate and the planned load capacity of the carrier, preparing a mixed solution containing 8% of copper oxide, 5% of molybdenum oxide and 1% of praseodymium oxide, soaking for 5 hours by adopting an isometric immersion method, drying in a 120 ℃ oven, and roasting in a 580 ℃ muffle furnace for 10 hours to obtain the catalyst 8% of Cu 5% of Mo 1% of Pr/SAPO-34 for converting the carbon monoxide into the nitrogen-containing compound at the low temperature.
[ example 4 ]
Selecting SiO2/Al2O3SAPO-34 molecular sieve with the molar ratio of 0.6 is taken as a carrier, and the water absorption of the carrier is firstly measured. According to the measured water absorption rate and the planned load capacity of the carrier, preparing a mixed solution containing 10% of copper oxide, 3% of tungsten oxide and 2% of neodymium oxide, soaking for 5 hours by adopting an isometric immersion method, drying in a 120 ℃ oven, and roasting in a 580 ℃ muffle furnace for 10 hours to obtain the catalyst for converting carbon monoxide into nitrogen-containing compounds at low temperature, namely 10% Cu 3% W2% Nd/SAPO-34.
[ example 5 ]
Selecting SiO2/Al2O3SAPO-34 molecular sieve with the molar ratio of 0.8 is taken as a carrier, and the water absorption of the carrier is firstly measured. Preparing a mixed solution containing 5 percent of copper oxide, 0.1 percent of manganese oxide and 2 percent of cerium oxide according to the measured water absorption rate and the planned load capacity of the carrier, soaking for 5 hours by adopting an equal-volume soaking method, drying in a 120-DEG C oven, and roasting for 10 hours in a 580-DEG C muffle furnace to obtain the catalyst for converting carbon monoxide into nitrogen-containing compounds at low temperature, namely 5 percent of Cu0.1％Mn2％Ce/SAPO-34。
[ example 6 ]
Selecting SiO2/Al2O3SAPO-34 molecular sieve with the molar ratio of 1 is taken as a carrier, and the water absorption of the carrier is firstly measured. According to the measured water absorption rate and the planned load capacity of the carrier, preparing a mixed solution containing 2% of copper oxide, 2% of chromium oxide and 1% of lanthanum oxide, soaking for 5 hours by adopting an equal-volume impregnation method, drying in a 120 ℃ oven, and roasting in a 580 ℃ muffle furnace for 10 hours to obtain the catalyst for converting carbon monoxide into nitrogen-containing compounds at low temperature, namely 2% Cu 2% Cr 1% La/SAPO-34.
[ example 7 ]
Selecting SiO2/Al2O3SAPO-34 molecular sieve with the molar ratio of 0.3 is taken as a carrier, and the water absorption of the carrier is firstly measured. According to the measured water absorption rate and the planned load capacity of the carrier, preparing a mixed solution containing 6% of copper oxide, 4% of rhenium oxide and 2% of praseodymium oxide, soaking for 5 hours by adopting an isometric immersion method, drying in a 120 ℃ oven, and roasting in a 580 ℃ muffle furnace for 10 hours to obtain the catalyst for converting carbon monoxide into nitrogen-containing compounds at low temperature, namely 6% Cu 4% Re 2% Pr/SAPO-34.
[ example 8 ]
Selecting SiO2/Al2O3SAPO-34 molecular sieve with the molar ratio of 0.5 is taken as a carrier, and the water absorption of the carrier is firstly measured. According to the measured water absorption rate and the planned load capacity of the carrier, preparing a mixed solution containing 5% of copper oxide, 3% of manganese oxide and 0.5% of cerium oxide, soaking for 5 hours by adopting an isometric immersion method, drying in a 120 ℃ oven, and roasting in a 580 ℃ muffle furnace for 10 hours to obtain the catalyst for converting carbon monoxide into nitrogen-containing compounds at low temperature, namely 5% Cu 3% Mn0.5% Ce/SAPO-34.
[ example 9 ]
Selecting SiO2/Al2O3SAPO-34 molecular sieve with the molar ratio of 0.1 is taken as a carrier, and the water absorption of the carrier is firstly measured. According to the water absorption rate and the planned loading capacity of the carrier, a mixed solution containing 3 percent of copper oxide, 8 percent of chromium oxide and 0.5 percent of lanthanum oxide is prepared, immersed for 5 hours by an isometric immersion method, and then the mixed solution is immersed at 120 DEG CDrying in an oven, and roasting in a muffle furnace at 580 ℃ for 10 hours to obtain the catalyst 3% Cu 2% Cr 6% Re0.5% La/SAPO-34 for low-temperature conversion of the nitrogen-containing compounds by the carbon monoxide.
[ example 10 ]
Selecting SiO2/Al2O3SAPO-34 molecular sieve with the molar ratio of 0.1 is taken as a carrier, and the water absorption of the carrier is firstly measured. According to the water absorption rate of the carrier and the planned load capacity, preparing a mixed solution containing 3% of copper oxide, 8% of chromium oxide and 0.5% of lanthanum oxide, soaking for 5 hours by adopting an equal-volume impregnation method, drying in a 120 ℃ oven, and roasting for 10 hours in a 580 ℃ muffle furnace to obtain the catalyst for converting carbon monoxide into nitrogen-containing compounds at low temperature, namely 3% Cu 6% Cr 2% Re0.5% La/SAPO-34.
[ example 11 ]
The catalysts prepared in examples 1-10 were used to examine the reaction performance of the low-temperature catalytic conversion of nitrogen-containing compounds by carbon monoxide in a conventional micro fixed bed reaction device. The catalyst loading is 1.05 g, and the gas space velocity is 2400h-1The reaction temperature is 200-350 ℃, and the reaction results are shown in Table 1.
TABLE 1
[ COMPARATIVE EXAMPLE 1 ]
Selecting Al2O3As the carrier, the water absorption of the carrier was measured. Preparing a mixed solution containing 3 percent of copper oxide, 8 percent of chromium oxide and 0.5 percent of lanthanum oxide according to the water absorption rate and the planned load capacity of the carrier, soaking for 5 hours by adopting an isometric immersion method, drying in a 120 ℃ oven, and roasting for 10 hours in a 580 ℃ muffle furnace to obtain the catalyst for converting carbon monoxide into nitrogen-containing compounds at low temperature, namely 3 percent of Cu8 percent of Cr0.5 percent of La/Al2O3。
The catalyst performance was evaluated under the reaction conditions of example [ 11 ], and the results are shown in Table 1.
[ COMPARATIVE EXAMPLE 2 ]
Selecting SiO2/Al2O3Molar ratio ofSAPO-34 molecular sieve with the weight of 0.1 is taken as a carrier, and the water absorption of the carrier is firstly measured. Preparing a mixed solution containing 3 percent of copper oxide and 0.5 percent of lanthanum oxide according to the water absorption rate and the planned load capacity of the carrier, soaking for 5 hours by adopting an isometric impregnation method, drying in a 120 ℃ oven, and roasting in a 580 ℃ muffle furnace for 10 hours to obtain the catalyst of 3 percent of Cu0.5 percent of La/SAPO-34 for converting carbon monoxide into nitrogen-containing compounds at low temperature.
The catalyst performance was evaluated under the reaction conditions of example [ 11 ], and the results are shown in Table 1.
[ COMPARATIVE EXAMPLE 3 ]
Selecting SiO2/Al2O3SAPO-34 molecular sieve with the molar ratio of 0.1 is taken as a carrier, and the water absorption of the carrier is firstly measured. Preparing a mixed solution containing 3 percent of copper oxide and 8 percent of chromium oxide according to the water absorption rate of the carrier and the planned load capacity, soaking for 5 hours by adopting an isometric impregnation method, drying in a 120 ℃ oven, and roasting in a 580 ℃ muffle furnace for 10 hours to obtain the catalyst 3 percent of Cu8 percent of Cr/SAPO-34 for converting the carbon monoxide into the nitrogen-containing compound at the low temperature.
The catalyst performance was evaluated under the reaction conditions of example [ 11 ], and the results are shown in Table 1.
[ examples 12 to 15 ]
The catalyst prepared in example 1 was used, and the reaction conditions and the evaluation results are shown in Table 2.
TABLE 2
Claims (7)
1. A method for catalytically converting nitrogen-containing compounds by using carbon monoxide is characterized in that a catalyst used in the method is composed of the following components in percentage by weight:
a) 1-10% of copper oxide;
b) 0.1-5% of at least one metal oxide selected from group VI B or VII B of the periodic table of elements;
c) 0.2-3% of rare earth metal oxide;
d) 85-92.9% of SAPO-34 molecular sieve carrier, the silicon-aluminum molar ratio SiO of the molecular sieve carrier2/Al2O30.1 to 1.
2. The method for catalytic conversion of nitrogen-containing compounds by carbon monoxide as claimed in claim 1, wherein the content of copper oxide is 2-8% by weight of the catalyst.
3. The method for catalytic conversion of nitrogen-containing compounds by carbon monoxide according to claim 1, wherein the content of at least one selected from the group consisting of group VI B and group VII B metal oxides in the periodic table is 0.5 to 3% by weight based on the weight of the catalyst.
4. The process for the catalytic conversion of nitrogen-containing compounds with carbon monoxide according to claim 1, characterized in that at least one metal of the metal oxides of groups VI B or VII B of the periodic Table of the elements is selected from Cr, Mo, W, Mn or Re.
5. The process for the catalytic conversion of nitrogen-containing compounds with carbon monoxide as claimed in claim 1, wherein the metal of the rare earth metal oxide is at least one selected from the group consisting of La, Ce, Pr and Nd.
6. The process for the catalytic conversion of nitrogen-containing compounds of carbon monoxide according to claim 1, wherein the nitrogen-containing compounds comprise nitrogen oxides and methyl nitrite.
7. The method for catalytically converting nitrogen-containing compounds with carbon monoxide as claimed in any of claims 1 to 6, wherein the reaction temperature is 200 to 350 ℃ and the gas space velocity is 500 to 5000h-1And removing the nitrogen-containing compounds under the reaction condition with the pressure of 0-2 MPa.
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| CN109095493B (en) * | 2018-08-30 | 2020-10-27 | 南京大学 | Two-dimensional ultrathin CuO @ SAPO-34 molecular sieve sheet material and preparation method and application thereof |
| CN109482227B (en) * | 2018-08-30 | 2021-09-28 | 南京大学 | Two-dimensional ultrathin Mo/CuO @ SAPO-34 molecular sieve catalytic material, and preparation method and application thereof |
| CN110227540B (en) * | 2019-05-10 | 2020-09-08 | 四川大学 | AFI-CHA mixed crystal molecular sieve and NH using same as carrier3-SCR catalysts and process for their preparation |
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| CN102614910B (en) * | 2012-03-16 | 2014-01-01 | 北京工业大学 | Ammonia-selective preparation method of SAPO-34 supported Cu-Fe catalyst for catalytically removing NOx |
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| CN1129146A (en) * | 1995-02-17 | 1996-08-21 | 段忠善 | Catalyst for purifying waste industrial gas and exhausted gas of automobile |
| CN1245444A (en) * | 1996-12-19 | 2000-02-23 | Basf公司 | Method for reduction of nitrogen oxides |
| CN104107700A (en) * | 2013-04-16 | 2014-10-22 | 中国科学院兰州化学物理研究所 | Industrial organic exhaust gas combustion catalyst and preparation method thereof |
| CN103394369A (en) * | 2013-08-07 | 2013-11-20 | 太原理工大学 | Non-noble metal molecular sieve catalyst for low concentration gas combustion and preparation method thereof |
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