CN110586177A - For NOxCore-shell structure catalyst capable of efficiently and synergistically removing methylbenzene and preparation method thereof - Google Patents

For NOxCore-shell structure catalyst capable of efficiently and synergistically removing methylbenzene and preparation method thereof Download PDF

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Publication number
CN110586177A
CN110586177A CN201910936837.XA CN201910936837A CN110586177A CN 110586177 A CN110586177 A CN 110586177A CN 201910936837 A CN201910936837 A CN 201910936837A CN 110586177 A CN110586177 A CN 110586177A
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core
beta
preparation
catalyst
toluene
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张俊丰
张良芃
赵令葵
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Xiangtan University
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Xiangtan University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8621—Removing nitrogen compounds
    • B01D53/8625—Nitrogen oxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
    • B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
    • B01D2257/702—Hydrocarbons
    • B01D2257/7027—Aromatic hydrocarbons

Abstract

The invention discloses a pair of NOxA core-shell structure catalyst which can efficiently remove toluene in a synergic manner and a preparation method thereof. The catalyst comprises the following components in percentage by mass: cu: 0.5 to 4 percent of CeO2: 20-30% of Beta molecular sieve serving as a carrier. The preparation method comprises the following steps: taking Cu/Beta as a core, and adding CeO2Coating the Cu/Beta nuclear layer, drying and calcining to obtain Cu/Beta @ CeO2A core-shell catalyst. The invention adopts Cu/Beta with stronger toluene adsorption and desorption capacity as a core, and Cu can be reduced simultaneouslyLow catalyst light-off temperature; second, CeO2The strong oxygen storage capacity of the shell can prevent carbon deposition on the surface of the catalyst, so that the active components of the core layer are protected and form a special interface effect with the active components, and the catalytic activity of the catalyst at low temperature of toluene is further improved.

Description

For NOxCore-shell structure catalyst capable of efficiently and synergistically removing methylbenzene and preparation method thereof
Technical Field
The invention relates to tail gas purification of a diesel vehicle, in particular to NOxA core-shell structure catalyst which can efficiently remove toluene in a synergic manner and a preparation method thereof.
Background
Due to the diesel vehicleThe pollution caused by the tail gas is increasingly serious, and the purification treatment of the tail gas of the diesel vehicle is more and more important in all countries in the world. NO, especially in diesel exhaustxThe product has great destructive effect on the natural environment and human health, and can cause serious environmental problems such as photochemical smog, acid rain, greenhouse effect, ozone layer cavity effect and the like; the total amount of HC discharged is not much, but the toluene in the benzene series is discharged remarkably, so that the benzene series has great harm to human bodies, and can be indirectly used as O3And precursors of smoke, are thus harmful to the environment and are therefore typical. Selective catalytic reduction of NO with ammoniax(NH3SCR) is currently the most promising diesel vehicle exhaust NOxThe purification technology has been industrially applied in developed countries such as Europe and America, and is also used for controlling the NO of the tail gas of the diesel vehicle at present and in the future in ChinaxOne of the main technologies for discharge.
V2O5-WO3(MO3)/TiO2The series of catalysts (i.e. vanadium-based catalysts) have been successfully applied to the IV (national IV) and V (national V) stages of diesel vehicles for purifying the tail gas NOxWith the issuance of more strict emission standards in the sixth stage (national sixth), the catalyst can not meet the national sixth and higher standards on NO in the tail gas of diesel vehiclesxThe emission requirements of (2). In addition, the emission requirements of the nation six for non-methane hydrocarbons are also continuously increasing. Mainly due to the fact that vanadium-based catalysts still have some unavoidable disadvantages: the effective working window (300-400 ℃) of the catalyst can not completely cover the temperature range (200-450 ℃) of the tail gas of the diesel vehicle; vanadium-based catalyst has poor carbon deposition resistance and V2O5Has strong biological toxicity; NH at high temperature (450 ℃ C.)3Is not selectively oxidized to make NOxThe purification rate is rapidly reduced and a large amount of by-product N is produced2O, leading to the main product N2The selectivity is obviously reduced, and secondary pollution is caused to the atmosphere. In the diesel vehicle exhaust aftertreatment system, the exhaust emission of HC is high due to the low adsorption capacity of the vanadium-based catalyst, so that an oxidation catalyst needs to be additionally arranged behind an SCR (selective catalytic reduction) system, the HC removal efficiency can be improved, and the purification cost can be increased. In conclusion, the diesel oil is realizedThe automobile catalyst is economical and environment-friendly, has excellent catalytic activity, and simultaneously has the performance of catalytic oxidation of HC.
In recent years, molecular sieve catalysts have attracted extensive attention from researchers in various fields due to their natural pore structures and excellent catalytic properties. Because the normal operating temperature of the diesel vehicle is 200-450 ℃, and the temperature during cold start and idling is lower, the concentration of toluene is increased rapidly, and the driving mileage of the diesel vehicle is up to hundreds of thousands of kilometers, so that the catalyst is required to have high low-temperature activity and long service life. However, the molecular sieve catalyst is often too acidic to deposit carbon on the surface, but ammonia gas which is too weak acidic is difficult to adsorb on the surface of the catalyst. Adding CeO2Coated on Cu/Beta core layer (Cu/Beta @ CeO)2) The above problems can be effectively improved: the activity at low temperature can be improved by taking Cu/Beta as a core, and the Cu/Beta and CeO simultaneously2Shell forming interface effect provides a stable catalytic oxidation reduction cycle site, and in addition, CeO2The shell layer can also play a role in avoiding the inactivation of the active components of the nuclear layer and regulating acidity. Therefore, how to reasonably construct an oxidation-reduction catalytic system with denitration and cooperative control of toluene plays an important role in the purification of the tail gas of the diesel vehicle.
Disclosure of Invention
In order to overcome the defects of the catalyst, the invention provides a method for preparing NOxA core-shell structure catalyst which has efficient and synergistic removal with toluene and a preparation method thereof.
The technical scheme adopted by the invention is as follows:
for NOxThe catalyst with efficient synergistic removal with toluene has a core-shell structure, takes Cu/Beta as a core, and CeO2Coating the obtained product on a Cu/Beta nuclear layer to obtain Cu/Beta @ CeO2The core-shell catalyst comprises the following components in percentage by mass:
Cu：0.5％～4％，CeO2: 20-30% of a carrier Beta molecular sieve;
the Beta molecular sieve has a specific surface area of 600-650 m2(ii) a total pore volume of 0.2 to 0.5cm2(ii)/g, average pore diameter of 3 to 7nm, SiO2/Al2O3The molar ratio is 20-30.
The above pair of NOxThe preparation method of the core-shell catalyst which has high-efficiency synergistic removal with toluene comprises the following steps:
(3) preparation of Cu/Beta core layer: dissolving copper sulfate in deionized water, stirring uniformly, adding a Beta molecular sieve, stirring vigorously to prepare a mixed solution 1, adding an ammonium hydroxide solution into the mixed solution 1 to adjust the pH value to 3.0-4.0, performing suction filtration, washing with deionized water until the pH value is 7, and drying to obtain a Cu/Beta nuclear layer;
(4)Cu/Beta@CeO2preparation of core-shell catalyst: uniformly mixing ultrapure water and absolute ethyl alcohol in equal volume to prepare a mixed solution 2, grinding the Cu/Beta nuclear layer prepared in the step (1) into powder, putting the powder into the mixed solution 2 for ultrasonic dispersion to obtain a dispersion liquid 1, sequentially adding polyethylene pyrrolidone, cerium nitrate and hexamethylenetetramine into the dispersion liquid 1, uniformly stirring to prepare a mixed solution 3, carrying out condensation reflux on the mixed solution 3, centrifuging to obtain a precipitate, drying and calcining to obtain Cu/Beta @ CeO @2A core-shell catalyst.
Further, in the step (1), the dosage ratio of the copper sulfate to the molecular sieve is 0.01-0.02 mol: 8-12 g.
Further, in the step (1), the temperature of vigorous stirring is 25-30 ℃ and the time is 10-12 minutes.
Further, in the step (1), the drying temperature is 80-100 ℃ and the time is 12-24 hours.
Further, in the step (2), the Cu/Beta core layer powder: polyvinylpyrrolidone: cerium nitrate: the mass ratio of the hexamethylene tetramine is 0.1-0.5: 0.5-1.2: 0.04-0.1: 0.04 to 0.1.
Further, in the step (2), the temperature of condensation reflux is 50-80 ℃ and the time is 1-5 hours.
Further, in the step (2), the drying temperature is 50-100 ℃, and the drying time is 10-24 hours.
Further, in the step (2), the calcination is carried out in an inert environment at the temperature of 400-600 ℃ for 2-5 hours.
Compared with the traditional SCR catalyst, the invention has the beneficial effects that:
1. the catalyst takes Cu as an active component and is loaded on a Beta molecular sieve as a nuclear layer, so that the catalyst has stronger toluene adsorption and desorption capacity, and the Cu can also reduce the ignition temperature of the catalyst, namely, the activity of the catalyst at low temperature is improved;
2、CeO2the shell layer and the Cu/Beta core layer can form a unique core-shell interface to have a synergistic effect, the core-shell interface effect can provide a stable catalytic oxidation reduction circulation place, and CeO is used2The strong oxygen storage capacity of the shell layer can prevent carbon deposition on the surface of the catalyst, avoid the inactivation of active components of the core layer and effectively regulate acidity, thereby realizing NO controlxAnd efficient synergistic removal of toluene.
Drawings
FIG. 1 shows Beta @ CeO2、1.5％Cu/Beta、Cu-Ce/Beta、1.5％Cu/Beta@CeO2The denitration efficiency in the cooperative removal efficiency.
FIG. 2 shows Beta @ CeO2、1.5％Cu/Beta、Cu-Ce/Beta、1.5％Cu/Beta@CeO2The efficiency of the conversion of toluene in the removal efficiency.
Detailed Description
The present invention will be described in detail with reference to specific embodiments. The invention may be practiced without limitation to the scope of the embodiments.
Example 1
For NOxCu/Beta @ CeO with efficient synergistic removal effect on toluene2The core-shell catalyst is prepared from Cu/Beta as core layer and CeO as shell layer2Composition is carried out; beta, Cu, CeO2The mass percentages are respectively as follows: 76%, 1%, 23%;
the precursor of the Cu is copper sulfate; CeO (CeO)2The precursor of (2) is cerium nitrate.
The preparation method of the core-shell catalyst comprises the following steps:
(1) preparation of Cu/Beta core layer: dissolving 0.3g of copper sulfate in deionized water, stirring uniformly, then violently stirring a Beta molecular sieve for 10 minutes at 25 ℃ to prepare a mixed solution 1, adding an ammonium hydroxide solution into the mixed solution 1 to adjust the pH value to 3.0-4.0, performing suction filtration, washing with deionized water until the pH value is 7, and drying for 24 hours at 100 ℃ to obtain a Cu/Beta nuclear layer;
(2)Cu/Beta@CeO2preparation of core-shell catalyst: uniformly mixing ultrapure water and absolute ethyl alcohol in the same volume to prepare a mixed solution 2, grinding the Cu/Beta nuclear layer prepared in the step (1) into powder, putting the powder into the mixed solution 2 for ultrasonic dispersion (ultrasonic frequency is 60KHz) to obtain a dispersion liquid 1, sequentially adding 1g of polyvinylpyrrolidone, 0.08g of cerium nitrate and 0.06g of hexamethylenetetramine into the dispersion liquid 1, uniformly stirring to prepare a mixed solution 3, condensing and refluxing the mixed solution 3 at 60 ℃ for 2 hours, obtaining a precipitate through centrifugation, drying the precipitate at 60 ℃ for 24 hours, and calcining at 500 ℃ for 3 hours in an inert environment to obtain Cu/Beta CeO @2The core-shell catalyst comprises 1% of Cu by mass and can also be recorded as 1% of Cu/Beta @ CeO2。
Example 2
Preparation of the catalyst of the invention: the preparation conditions and preparation procedure were the same as in example 1, except that copper sulfate was used in an amount of 0.45g so that the Cu content was 1.5% by mass, and the catalyst was represented by the following formula, 1.5% Cu/Beta @ CeO2。
Example 3
Preparation of the catalyst of the invention: the preparation conditions and procedure were the same as in example 1, except that copper sulfate was used in an amount of 0.6g so that the Cu content was 2% by mass, and the catalyst was represented by the following formula, 2% Cu/Beta @ CeO2。
Example 4
Preparation of the catalyst of the invention: the preparation conditions and preparation procedure were the same as in example 1, except that copper sulfate was used in an amount of 0.75g so that the Cu content was 2.5% by mass, and the catalyst was represented by the following formula, 2.5% Cu/Beta @ CeO2。
Comparative example 1
Cu-free Beta @ CeO2Core-shell catalystThe preparation of (1): the preparation conditions and procedure were the same as in example 1, except that the Cu content by mass was 0, and the catalyst was represented by the following formula, Beta @ CeO2。
Comparative example 2
Not subjected to CeO2Preparation of 1.5% Cu/Beta catalyst coated with shell: namely, the procedure of example 2 was followed in step (1).
Comparative example 3
The preparation of the Cu-Ce/Beta catalyst (non-shell-core structure) was carried out according to the preparation method in the published invention CN 102716736A: wherein the mass percentage of Cu is 1.5 percent, and CeO2The mass percent of the catalyst is 23 percent, and the catalyst can be represented by the following formula, Cu-Ce/Beta.
Example 5
The catalyst disclosed by the invention is used for denitration and cooperative control of toluene activity test.
Inventive example 2 (1.5% Cu/Beta @ CeO), respectively2) Comparative examples 1, 2 and 3 denitration co-control toluene activity tests were performed in a fixed bed reactor. Loading the catalyst into a catalytic reactor with a catalyst loading of 0.25 g; the simulated smoke is introduced into the flue gas and comprises the following components: 5% vol.O2，500ppmNO，500ppmNH3100ppm toluene, balance gas N2(ii) a At the airspeed of 60000h-1And testing the toluene conversion performance of the catalyst at the reaction temperature of 100-400 ℃.
The results are shown in fig. 1 and fig. 2, it can be seen from comparative example 1 and example 2 that the addition of Cu can significantly improve the low-temperature catalytic activity of the catalyst, and the denitration efficiency and the toluene conversion efficiency at 300 ℃ reach 95% and 92% respectively; from comparative example 2 and example 2, CeO can be seen2The coating is favorable for improving the conversion efficiency of the toluene, and the conversion efficiency of the toluene reaches 95 percent at 350 ℃, which indicates that CeO2The shell can well protect the active components on the carrier and form an interface effect with the active components so as to improve the catalytic activity; as can be seen from comparative example 3 and example 2, the core-shell structure and the non-core-shell structure (comparative example 3) of the present invention have an important influence on the catalyst activity, the denitration efficiency and the toluene conversion efficiency of comparative example 3 at 300 ℃ are 83% and 81%, respectively, and the denitration efficiency and the toluene conversion efficiency of example 2 at 300 ℃ are 83% and 81%, respectivelyThe nitrate efficiency and the toluene conversion efficiency are respectively 97% and 95%, so the core-shell structure has very important effect on the improvement of the catalyst performance.

Claims (9)

1. For NOxThe catalyst with a core-shell structure and high-efficiency synergistic removal with toluene is characterized in that Cu/Beta is taken as a core, and CeO is taken as a core2Coating the obtained product on a Cu/Beta nuclear layer to obtain Cu/Beta @ CeO2The core-shell catalyst specifically comprises the following components in percentage by mass:
Cu：0.5％～4％，CeO2: 20-30% of a carrier Beta molecular sieve;
the Beta molecular sieve has a specific surface area of 600-650 m2(ii) a total pore volume of 0.2 to 0.5cm2(ii) SiO, with an average pore diameter of 3 to 7nm2/Al2O3The molar ratio is 20-30.
2. Para NO according to claim 1xThe preparation method of the core-shell catalyst which has efficient and synergistic removal with toluene is characterized by comprising the following steps:
(1) preparation of Cu/Beta core layer: dissolving copper sulfate in deionized water, stirring uniformly, adding a Beta molecular sieve, stirring vigorously to prepare a mixed solution 1, adding an ammonium hydroxide solution into the mixed solution 1 to adjust the pH value to 3.0-4.0, performing suction filtration, washing with deionized water until the pH value is 7, and drying to obtain a Cu/Beta nuclear layer;
(2)Cu/Beta@CeO2preparation of core-shell catalyst: uniformly mixing ultrapure water and absolute ethyl alcohol in equal volume to prepare a mixed solution 2, grinding the Cu/Beta nuclear layer prepared in the step (1) into powder, putting the powder into the mixed solution 2 for ultrasonic dispersion to obtain a dispersion liquid 1, sequentially adding polyethylene pyrrolidone, cerium nitrate and hexamethylenetetramine into the dispersion liquid 1, uniformly stirring to prepare a mixed solution 3, carrying out condensation reflux on the mixed solution 3, centrifuging to obtain a precipitate, drying and calcining to obtain Cu/Beta @ CeO @2A core-shell catalyst.
3. Para NO according to claim 2xThe preparation method of the core-shell catalyst with efficient and synergistic removal of toluene is characterized in that in the step (1), the dosage ratio of copper sulfate to the molecular sieve is 0.01-0.02 mol: 8-12 g.
4. Para NO according to claim 2xThe preparation method of the core-shell catalyst with efficient and synergistic removal of toluene is characterized in that in the step (1), the temperature of vigorous stirring is 25-30 ℃, and the time is 10-12 minutes.
5. Para NO according to claim 2xThe preparation method of the core-shell catalyst with efficient and synergistic removal of toluene is characterized in that in the step (1), the drying temperature is 80-100 ℃, and the time is 12-24 hours.
6. Para NO according to claim 2xThe preparation method of the core-shell catalyst with efficient and synergistic removal of toluene is characterized in that in the step (2), Cu/Beta core layer powder: polyvinylpyrrolidone: cerium nitrate: the mass ratio of the hexamethylene tetramine is 0.1-0.5: 0.5-1.2: 0.04-0.1: 0.04 to 0.1.
7. Para NO according to claim 2xThe preparation method of the core-shell catalyst with efficient and synergistic removal of toluene is characterized in that in the step (2), the temperature of condensation reflux is 50-80 ℃, and the time is 1-5 hours.
8. Para NO according to claim 2xThe preparation method of the core-shell catalyst with efficient and synergistic removal of toluene is characterized in that in the step (2), the drying temperature is 50-100 ℃, and the drying time is 10-24 hours.
9. Para NO according to claim 2xThe preparation method of the core-shell catalyst with efficient and synergistic removal of toluene is characterized in that in the step (2), the calcination is carried out in an inert environmentThe temperature is 400-600 ℃, and the time is 2-5 hours.
CN201910936837.XA 2019-09-29 2019-09-29 For NOxCore-shell structure catalyst capable of efficiently and synergistically removing methylbenzene and preparation method thereof Pending CN110586177A (en)

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CN114160147A (en) * 2021-11-29 2022-03-11 华南理工大学 Composite oxide catalyst for synchronously removing VOCs and NOx in sulfur-containing flue gas and preparation method and application thereof

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Application publication date: 20191220