CN111068764B - NH for tail gas of diesel vehicle 3 SCO catalyst and preparation method thereof - Google Patents
NH for tail gas of diesel vehicle 3 SCO catalyst and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
- B01J29/72—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing iron group metals, noble metals or copper
- B01J29/76—Iron group metals or copper
- B01J29/7615—Zeolite Beta
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
- F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
- F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
- F01N3/105—General auxiliary catalysts, e.g. upstream or downstream of the main catalyst
- F01N3/106—Auxiliary oxidation catalysts
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/10—After treatment, characterised by the effect to be obtained
- B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T10/00—Road transport of goods or passengers
- Y02T10/10—Internal combustion engine [ICE] based vehicles
- Y02T10/12—Improving ICE efficiencies
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Abstract
The invention discloses NH for tail gas of a diesel vehicle 3 -a process for the preparation of an SCO catalyst, comprising the steps of: dissolving Co salt and Cu salt in water to form a mixed solution; taking the dried Beta molecular sieve as a carrier; dropwise adding the mixed solution into a container containing the carrier Beta, stirring while dropwise adding, continuously stirring for 15-30min after dropwise adding, uniformly mixing, and soaking overnight. After the impregnation is finished, placing the mixture in an oven for drying to obtain a precursor of the SCO catalyst; placing the precursor in a muffle furnace, and roasting for 3-5h in an air atmosphere at 450-600 ℃ to obtain NH for diesel vehicle exhaust 3 -SCO catalyst. The catalyst prepared by the method has high low-temperature catalytic activity and N 2 The selectivity is good, the price is low, and the method has important practical and economic significance.
Description
Technical Field
The invention belongs to the field of environmental protection technology and environmental catalysis, and particularly relates to a low-temperature and N-type catalyst for tail gas of a diesel vehicle 2 NH with better selectivity 3 -a process for the preparation of SCO catalysts.
Background
In recent years, with the continuous improvement of the economic level of China, the maintenance of motor vehicle people is also continuously increasing. Statistics data of the department of transportation of China show that although the diesel vehicle of China only accounts for 17% of the total amount held by the vehicle at present, nitrogen oxides (NO X ) The emission amount is nearly seven times of the total emission amount of the automobile. NO for diesel vehicle exhaust X Selective Catalytic Reduction (SCR) treatments are typically employed, and are often sprayed into the vehicle urea to produce excess NH 3 As a reducing agent to achieve a greater NO removal rate, but NH actually taking part in the reduction reaction 3 The ratio of/NO is less than 1 (. Apprxeq.0.90-0.95), thus resulting in unreacted NH 3 Leakage phenomenon of (2). In addition, the national standard has more and more strict requirements on NOx emission limit, and more urea is added to meet the NOx emission requirement, thereby causing larger NH 3 Leakage. The national VI standard fully implemented in 2021 is applied to the NH of diesel vehicles 3 The emission limit is 10ppm, so an ASC system is added in the diesel vehicle exhaust aftertreatment system to realize the removal of excessive ammonia.
NH 3 Is a colorless gas with strong pungent smell, is extremely easy to dissolve in water, is harmful to human health, and can cause a series of environmental problems such as acid rain, photochemical smog, ozone layer damage, greenhouse effect and the like. NH (NH) 3 The SCO technology is the most promising technology for removing ammonia in tail gas of diesel vehicles, and currently, catalysts applied to catalytic oxidation of ammonia mainly comprise noble metal catalysts, transition metal catalysts, composite oxide catalysts and molecular sieve catalysts. These catalyst materials each have advantages and disadvantages, in which the noble metal catalyst has a high catalytic activity, but N 2 The selectivity is generally poor and the price of the noble metal is high; the transition metal catalyst N2 has better selectivity but needs higher ignition temperature; the catalytic performance of the composite oxide catalyst varies from material to material, and the low-temperature activity is generally required to be improved; molecular sieve based catalysts are characterized by their own structure to NH 3 Has good catalytic performance, but is easy to dealuminate at high temperature to destroy the structural stability. The exhaust temperature of the tail gas of the diesel vehicle is about 150-400 ℃, so that the NH for the tail gas of the diesel vehicle 3 The SCO catalyst must have a broad temperature window and a high N 2 Selectivity. Together with the national VI standard, the method is implemented nationwide in 2021, and part of the regions are implemented in 2019, 7 and 1, so as to find NH for tail gas of diesel vehicles 3 SCO catalysts are of great practical and economic importance.
Disclosure of Invention
Aiming at the characteristics of the tail gas discharged by the diesel vehicle, the invention provides NH for the tail gas of the diesel vehicle 3 The preparation method of the SCO catalyst is a novel metal oxide supported catalyst which has high low-temperature catalytic activity and N 2 The selectivity is good, the price is low, and the method has important practical and economic significance for treating ammonia leakage of tail gas of diesel vehicles.
In order to solve the technical problems, the invention provides NH for tail gas of diesel vehicles 3 Preparation method of SCO catalyst and packageThe method comprises the following steps:
step one, putting a Beta molecular sieve into an oven, drying for 2-4 hours at 100-120 ℃, and measuring the saturated water absorption;
weighing a certain amount of copper nitrate and cobalt nitrate precursors, dissolving the copper nitrate and cobalt nitrate precursors in deionized water to form a mixed solution A, and weighing a certain amount of dried Beta molecular sieve, wherein the mass ratio Co: beta=0.01-0.1, mass ratio Cu: beta=0.01-0.2;
step three, dropwise adding the mixed solution A into a container containing Beta, stirring while dropwise adding, continuously stirring for 15-30min to form paste after dropwise adding, and standing overnight;
step four, putting the pasty catalyst precursor after standing overnight into a baking oven for drying to obtain a solid;
step five, placing the solid in a muffle furnace, and roasting for 3-5h in an air atmosphere at 450-600 ℃ to obtain NH for diesel vehicle exhaust 3 -SCO catalyst.
In the invention, the condition of the drying process in the fourth step is that the drying is carried out for 10-12 hours at 100-120 ℃.
NH for diesel vehicle tail gas prepared by the invention 3 SCO catalyst takes oxygen as oxidant at the reaction temperature of 150-400 ℃ and 500ppm NH 3 ，10％O 2 ，N 2 As balance gas, the total flow of the gas is controlled to be 300mL/min, and the catalyst dosage is 0.3mL for fixed bed reaction. After each temperature point is stable, NH in gas at the outlet of the reaction furnace is measured 3 、NO、NO 2 And N 2 The concentration of O is determined according to the formula (reactor inlet NH 3 Concentration-reactor outlet NH 3 Concentration)/(reactor inlet NH 3 Concentration). Times.100% conversion was calculated as (reactor inlet NH) 3 Concentration-reactor outlet NH 3 Concentration-reaction furnace outlet NO 2 Concentration-reaction furnace outlet N 2 O concentration)/(reactor inlet NH 3 Concentration-reactor outlet NH 3 Concentration) ×100% calculation of N 2 Selectivity.
Repeated experiments prove that the NH prepared by the invention 3 SCO catalysisThe NH of the agent is between 250 and 400 DEG C 3 The conversion rate of the catalyst can reach 89-95%; at 150-350 deg.C, its N 2 The selectivity can reach more than 77 percent. The product prepared by the invention has good low-temperature activity, especially the product in the example 5, and the low-temperature activity is obviously better than that of the similar products. The product of example 5 has an optimal N2 selectivity at 150 degrees.
In recent years, common use for NH 3 The catalysts and catalytic effects of SCO are shown in Table 1, compared with the prior art, the invention has the following beneficial effects:
(1) The invention prepares NH by common and economic inorganic salt and commercial molecular sieve 3 -an SCO catalyst;
(2) The catalyst removes NH 3 Is relatively efficient and can operate at temperatures in the range of 150-400 ℃;
(3) The catalyst N 2 The selectivity is good.
TABLE 1
Drawings
FIG. 1 is a test of SCO Activity of catalysts of examples 1-5 according to the invention NH 3 A conversion rate result graph;
FIG. 2 shows SCO activity test N for catalysts of examples 1-5 of the present invention 2 A selective outcome map;
FIG. 3 is an XRD pattern of the catalyst obtained in examples 1 to 5 of the present invention
Detailed Description
The technical solution of the present invention will be described in further detail with reference to the accompanying drawings and the specific embodiments, which are only illustrative of the present invention and are not intended to limit the present invention.
Example 1, NH for Diesel vehicle exhaust 3 -a process for the preparation of SCO catalysts comprising the steps of:
(1) The Beta molecular sieve is placed in an oven and dried for 3 hours at 120 ℃ for standby.
(2) Dissolving 0.493g of copper nitrate and 1.89g of cobalt nitrate in 4.78g of deionized water to form a mixed solution A, weighing 5g of dried Beta molecular sieve, dropwise adding the mixed solution A to the Beta molecular sieve while stirring, continuously stirring for 15min after the dropwise adding is finished, and standing overnight;
(3) Placing the pasty mixed solution after standing overnight at 120 ℃ for drying for 12 hours to obtain a precursor of the SCO catalyst;
(4) The precursor of the catalyst is placed in a muffle furnace and baked for 3 hours at 450 ℃ in air atmosphere, thus obtaining the low-temperature NH for diesel vehicle tail gas 3 -SCO catalyst.
NH prepared in example 1 3 In the SCO catalyst, the mass ratio of Co: beta=0.02, mass ratio Cu: beta=0.1, the catalyst particle size is 40-60 mesh (300-450 μm), the XRD pattern of the catalyst is shown in fig. 3, the SCO activity test results are shown in fig. 1 and 2, wherein the activity test conditions are as follows: 500ppm NH 3 ，5％O 2 ，N 2 As balance gas, total flow rate 300ml/min, catalyst dosage 0.3ml, experimental facilities: denitration catalysis evaluation device.
Example 2, NH for Diesel vehicle exhaust 3 -a process for the preparation of SCO catalysts comprising the steps of:
(1) The Beta molecular sieve is placed in an oven and dried for 3 hours at 120 ℃ for standby.
(2) 0.987g of copper nitrate and 1.89g of cobalt nitrate are dissolved in 4.78g of deionized water to form a mixed solution A, 5g of dried Beta molecular sieve is additionally weighed, the mixed solution A is dropwise added to the Beta molecular sieve while stirring, stirring is continued for 15min after the dropwise addition is finished, and standing is carried out overnight;
(3) Placing the pasty mixed solution after standing overnight at 120 ℃ for drying for 12 hours to obtain a precursor of the SCO catalyst;
(4) The precursor of the catalyst is placed in a muffle furnace and baked for 3 hours at 450 ℃ in air atmosphere, thus obtaining the low-temperature NH for diesel vehicle tail gas 3 -SCO catalyst.
Example 2 NH prepared 3 In the SCO catalyst, the mass ratio of Co: beta=0.04, mass ratio Cu: beta=0.1, the catalyst particle size is 40-60 mesh (300-450 μm) and the XRD pattern of the catalyst is shown in fig. 3, and the SCO activity test results are shown in fig. 1 and 2, wherein the activity test conditions are as follows: 500ppm NH 3 ，5％O 2 ，N 2 As balance gas, total flow rate 300ml/min, catalyst dosage 0.3ml, experimental facilities: denitration catalysis evaluation device.
Example 3 NH for Diesel exhaust 3 -a process for the preparation of SCO catalysts comprising the steps of:
(1) The Beta molecular sieve is placed in an oven and dried for 3 hours at 120 ℃ for standby.
(2) 1.48g of copper nitrate and 1.89g of cobalt nitrate are dissolved in 4.78g of deionized water to form a mixed solution A, 5g of dried Beta molecular sieve is additionally weighed, the mixed solution A is dropwise added to the Beta molecular sieve while stirring, stirring is continued for 15min after the dropwise addition is finished, and standing is carried out overnight;
(3) Placing the pasty mixed solution after standing overnight at 120 ℃ for drying for 12 hours to obtain a precursor of the SCO catalyst;
(4) The precursor of the catalyst is placed in a muffle furnace and baked for 3 hours at 450 ℃ in air atmosphere, thus obtaining the low-temperature NH for diesel vehicle tail gas 3 -SCO catalyst.
Example 5 NH prepared 3 In the SCO catalyst, the mass ratio of Co: beta=0.06, mass ratio Cu: beta=0.1, the catalyst particle size is 40-60 mesh (300-450 μm), the XRD pattern of the catalyst is shown in fig. 3, the SCO activity test results are shown in fig. 1 and 2, wherein the activity test conditions are as follows: 500ppm NH 3 ，5％O 2 ，N 2 As balance gas, total flow rate 300ml/min, catalyst dosage 0.3ml, experimental facilities: denitration catalysis evaluation device.
Example 4 NH for Diesel exhaust 3 -a process for the preparation of SCO catalysts comprising the steps of:
(1) The Beta molecular sieve is placed in an oven and dried for 3 hours at 120 ℃ for standby.
(2) 1.973g of copper nitrate and 1.89g of cobalt nitrate are dissolved in 4.78g of deionized water to form a mixed solution A, 5g of dried Beta molecular sieve is additionally weighed, the mixed solution A is dropwise added to the Beta molecular sieve while stirring, stirring is continued for 15min after the dropwise addition is finished, and standing is carried out overnight;
(3) Placing the pasty mixed solution after standing overnight at 120 ℃ for drying for 12 hours to obtain a precursor of the SCO catalyst;
(4) The precursor of the catalyst is placed in a muffle furnace and baked for 3 hours at 450 ℃ in air atmosphere, thus obtaining the low-temperature NH for diesel vehicle tail gas 3 -SCO catalyst.
Example 4 NH prepared 3 In the SCO catalyst, the mass ratio of Co: beta=0.08, mass ratio Cu: beta=0.1, the catalyst particle size is 40-60 mesh (300-450 μm), the XRD pattern of the catalyst is shown in fig. 3, the SCO activity test results are shown in fig. 1 and 2, wherein the activity test conditions are as follows: 500ppm NH 3 ，5％O 2 ，N 2 As balance gas, total flow rate 300ml/min, catalyst dosage 0.3ml, experimental facilities: denitration catalysis evaluation device.
Example 5 NH for Diesel exhaust 3 -a process for the preparation of SCO catalysts comprising the steps of:
(1) The Beta molecular sieve is placed in an oven and dried for 3 hours at 120 ℃ for standby.
(2) 2.467g of copper nitrate and 1.89g of cobalt nitrate are dissolved in 4.78g of deionized water to form a mixed solution A, 5g of dried Beta molecular sieve is additionally weighed, the mixed solution A is dropwise added to the Beta molecular sieve while stirring, stirring is continued for 15min after the dropwise addition is finished, and standing is carried out overnight;
(3) Placing the pasty mixed solution after standing overnight at 120 ℃ for drying for 12 hours to obtain a precursor of the SCO catalyst;
(4) The precursor of the catalyst is placed in a muffle furnace and baked for 3 hours at 450 ℃ in air atmosphere, thus obtaining the low-temperature NH for diesel vehicle tail gas 3 -SCO catalyst.
Example 5 NH prepared 3 In the SCO catalyst, the mass ratio of Co: beta=0.1, mass ratio Cu: beta=0.1, the catalyst particle size is 40-60 mesh (300-450 μm), the XRD pattern of the catalyst is shown in fig. 3, the SCO activity test results are shown in fig. 1 and 2, wherein the activity test conditions are as follows: 500ppm NH 3 ，5％O 2 ，N 2 As balance gas, total flow rate 300ml/min, catalyst dosage 0.3ml, experimental facilities: denitration catalysis evaluation device.
As can be seen from FIG. 2, the catalyst of the present invention has a high low temperature N2 selectivity, especially a low temperature N2 selectivity of 150 degrees, which can be as high as 95, which is hardly achieved by the various preparation methods of the prior art.
In summary, as shown in FIGS. 1, 2 and 3, NH was produced from the catalysts obtained in examples 1 to 5 of the present invention 3 Conversion and N 2 The selective result graph can show that NH for diesel vehicle exhaust prepared by the preparation method of the invention 3 SCO catalyst with excellent low temperature catalytic performance and high cost performance. Stirring and standing time, distilled water washing times, small influence of drying and roasting temperature time on activity, and high NH removal of Co-Cu/Beta catalyst in the range of 150-400 ℃ and especially in the range of 250-400 DEG C 3 And N 2 Good selectivity, that is, NH can be realized in a certain temperature 3 Can be widely applied to the treatment of ammonia leakage of tail gas of diesel vehicles.
Claims (3)
1. NH for tail gas of diesel vehicle 3 -a process for the preparation of an SCO catalyst, characterized in that it comprises the steps of:
step one, putting the Beta molecular sieve into an oven, and drying for 2-4 hours at 100-120 ℃;
step two, weighing 2.467 parts of copper nitrate and 1.89 parts of cobalt nitrate precursor, dissolving the copper nitrate and the cobalt nitrate precursor in deionized water to form a mixed solution A, and weighing 5 parts of dried Beta molecular sieve;
step three, dropwise adding the mixed solution A into a container containing Beta, stirring while dropwise adding, continuously stirring for 15-30min to form paste after dropwise adding, and standing overnight;
step four, putting the pasty catalyst precursor after standing overnight into a baking oven for drying to obtain a solid;
step five, placing the solid in a muffle furnace, and roasting for 3-5h in an air atmosphere at 450-600 ℃ to obtain NH for diesel vehicle exhaust 3 -SCO catalyst.
2. NH for diesel vehicle exhaust according to claim 1 3 -a process for the preparation of SCO catalysts, characterized in that: the drying process in the fourth step is carried out at 100-120 ℃ for 10-12h.
3. NH for diesel vehicle exhaust according to claim 1 3 Use of a SCO catalyst, characterized in that it comprises NH prepared by the preparation method according to claim 1 3 Oxidation of SCO catalyst, fixed bed reaction at 150-400 deg.c to obtain NH 3 Oxidation to N 2 And H 2 O。
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