CN108043466A - One kind is used for NOxThe zeolite imidazole ester skeleton structure composite material and preparation method and application of removing - Google Patents
One kind is used for NOxThe zeolite imidazole ester skeleton structure composite material and preparation method and application of removing Download PDFInfo
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/1691—Coordination polymers, e.g. metal-organic frameworks [MOF]
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- 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
- B01D53/8628—Processes characterised by a specific catalyst
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- 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
- B01D53/90—Injecting reactants
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- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0234—Nitrogen-, phosphorus-, arsenic- or antimony-containing compounds
- B01J31/0235—Nitrogen containing compounds
- B01J31/0244—Nitrogen containing compounds with nitrogen contained as ring member in aromatic compounds or moieties, e.g. pyridine
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
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- B01D2251/00—Reactants
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- B01D2251/206—Ammonium compounds
- B01D2251/2062—Ammonia
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/02—Compositional aspects of complexes used, e.g. polynuclearity
- B01J2531/0238—Complexes comprising multidentate ligands, i.e. more than 2 ionic or coordinative bonds from the central metal to the ligand, the latter having at least two donor atoms, e.g. N, O, S, P
- B01J2531/0241—Rigid ligands, e.g. extended sp2-carbon frameworks or geminal di- or trisubstitution
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/70—Complexes comprising metals of Group VII (VIIB) as the central metal
- B01J2531/72—Manganese
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Abstract
The invention discloses one kind to be used for NOxThe zeolite imidazole ester skeleton structure composite material and preparation method and application, preparation method of removing include the following steps：After raw material needed for the soluble-salt of manganese, synthetic zeolite imidazate skeleton structure composite material and solvent mixing, the zeolite imidazole ester skeleton structure composite material of Mn oxide modification is prepared using solvent-thermal method；Solvent, the soluble-salt of manganese and the mass ratio of raw material needed for synthetic zeolite imidazate skeleton structure composite material are 8 10：0.2‑0.75:1.The composite material of the present invention avoids Mn oxide reunion inactivation under reaction temperature by means of the larger surface area of zeolite imidazole ester skeleton structure composite material, temperature window is widened, it realizes and removes the efficient catalytic of nitrogen oxides at a lower temperature, improve the catalytic activity of catalyst.
Description
Technical field
It is more particularly to a kind of to be used for NO the invention belongs to atmosphere pollution control technology fieldxThe Mn oxide of removing is repaiied
The zeolite imidazole ester skeleton structure composite material and preparation method and application of decorations.
Background technology
Nitrogen oxides (mainly includes NO and NO2) it is a kind of common gas pollutant, improvement is always for a long time
The important content of environmental protection, source are broadly divided into moving source and stationary source, and stationary source refers mainly to the combustion of the fossils such as industrial production
The flue gas that the burning of material is discharged (such as the burning of coal and oil), moving source refer mainly to the discharge of motor-vehicle tail-gas.With modern age
Industrialized fast development, fossil fuel are largely developed and used so that be discharged into nitrogen oxides in air considerably beyond
The bearer cap and self-purification capacity of atmospheric environment.Nitrogen oxides is very big to environmental hazard, for example, photochemical fog, acid rain and
Ozone hole is related with the discharge of nitrogen oxides, threatens the life security of human and animal.Therefore, it is necessary to strengthen administering air
In nitrogen oxides.
At present, industrial most commonly seen, the Treatment process for the NOx being most widely used is mainly with NH3For reducing agent
Selective catalytic reduction (NH3-SCR).Catalyst is the key factor for influencing SCR denitration efficiency.Currently used catalyst
Mainly include noble metal catalyst, molecular sieve catalyst, metal oxide catalyst.Wherein V2O5-WO3/TiO2It is common at present
Commercial catalyst, the catalyst have higher catalytic activity in 350-500 DEG C of temperature window, but in practical applications, it should
It is higher with cost, and active component vanadium is volatilized at high temperature with bio-toxicity, and environment and the mankind are caused to poison, moreover, right
The temperature requirement of pending nitrogen oxides is higher, is difficult to obtain good catalyticing purifying effect under low temperature.Therefore exploitation low temperature is high
It is extremely urgent to imitate non-toxic catalyst.
The content of the invention
Technical problem present in for the above-mentioned prior art, the object of the present invention is to provide one kind to be used for NOxRemoving
Zeolite imidazole ester skeleton structure composite material and preparation method and application.
In order to solve the above technical problems, the technical scheme is that：
One kind is used for NOxThe preparation method of the zeolite imidazole ester skeleton structure composite material of removing, includes the following steps：
After raw material needed for the soluble-salt of manganese, synthetic zeolite imidazate skeleton structure composite material and solvent mixing, adopt
The zeolite imidazole ester skeleton structure composite material of Mn oxide modification is prepared with solvent-thermal method；
Solvent, the soluble-salt of manganese and the mass ratio of raw material needed for synthetic zeolite imidazate skeleton structure composite material are 8-
10：0.2-0.75:1.
Preferably, the soluble-salt of the manganese is manganese nitrate.Research shows compared with manganese chloride, manganese acetate, uses nitre
Catalyst activity higher prepared by sour manganese.
Preferably, the solvent is more than 99.5% absolute methanol for content.Classical zeolite imidazole ester skeleton structure material
Solvent used in the synthesis of material be absolute methanol and n,N-Dimethylformamide, and it has been investigated that, use N, N- dimethyl
The zeolite imidazole ester skeleton structure composite material thermal stability of Mn oxide modification prepared by formamide is poor, in NH3- SCR is anti-
Ying Zhong, catalytic activity just starts drastically to decline when temperature reaches 300 DEG C.
Preferably, the temperature of the solvent-thermal method is 135-145 DEG C, reaction time 20-30h.
Preferably, before being prepared using solvent-thermal method, ultrasonic pretreatment is carried out to the solution after mixing.Ultrasound can be located
Reason can make active material manganese salt it is scattered evenly.
It is further preferred that the time of ultrasound pretreatment is 5-10min, supersonic frequency 20-40kHz.
Preferably, the preparation method further includes the step of being activated to the composite material being prepared, specific as follows：
Dried composite material is put into tube furnace, is passed through nitrogen thereto, 250 are warming up to according to the rate of 5-10 DEG C/min
DEG C, 3-5h is kept, the zeolite imidazole ester skeleton structure composite material modified after cooling up to the Mn oxide of high activity.
It is further preferred that the nitrogen is High Purity Nitrogen, the flow of nitrogen is 45-55mL/min.
The zeolite imidazole ester skeleton structure composite material for the Mn oxide modification that above-mentioned preparation method is prepared.
The zeolite imidazole ester skeleton structure composite material of above-mentioned Mn oxide modification is in catalysis NH3- SCR reaction removals NOx
In application.
The zeolite imidazole ester skeleton structure composite material of above-mentioned Mn oxide modification is as catalyst NH3- SCR reacts
Method, specifically comprise the following steps：
1) the zeolite imidazole ester skeleton structure composite material preforms for modifying the Mn oxide after activation are sieved, and make composite wood
The grain size of material is 60-80 mesh, obtains catalyst；
2) pending flue gas is flowed through into catalyst, and NH is passed through into flue gas3As reducing agent, at 230-400 DEG C into
Row denitration reaction.
Using the composite material as catalyst, it can realize that the high efficiency of nitrogen oxides in effluent takes off at a lower temperature
It removes, the removal efficiency of nitrogen oxides is up to more than 90%.
Preferably, the NH being passed through in step 2)3Concentration be 500ppm.
Beneficial effects of the present invention
1st, composite material of the invention is avoided by means of the larger surface area of zeolite imidazole ester skeleton structure composite material
Mn oxide is reunited inactivation under reaction temperature, has been widened temperature window, has been realized nitrogen oxides at a lower temperature efficient
Catalytic eliminating improves the catalytic activity of catalyst.
2nd, raw material of the present invention is easy to get, preparation method is simple, high catalytic efficiency, highly practical, easy to spread.
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.It is unless another
It indicates, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " bag
Include " when, indicate existing characteristics, step, operation, device, component and/or combination thereof.
Example 1：The preparation method of the zeolite imidazole ester skeleton structure composite material of Mn oxide modification
(1) precise 3.528g zinc nitrate hexahydrates, 1.944g methylimidazoles, 0.807g sodium formates, same to 78.5ml
Absolute methanol mixes, magnetic agitation, and 50% manganese nitrate solutions of 1.5mL are added dropwise, and keeps magnetic agitation 5min.
(2) gained mixed solution handles 5min under 30kHz ultrasounds.
(3) in the reaction kettle for the polytetrafluoroethyllining lining that the mixed liquor of gained ultrasound pretreatment is put into 100mL, it is placed in baking oven
In, it is to slowly warm up to 140 DEG C and keeps for 24 hours.
(4) gained suspension is after absolute methanol washs 3 times, the dry 8h in 60 DEG C of baking ovens.
(5) obtained solid powder is provided into tube furnace, after good seal, is passed through the High Purity Nitrogen of 50mL/min；Tube furnace is pressed
250 DEG C are warming up to according to the rate of 5 DEG C/min, 3h is kept, is taken out after natural cooling, you can obtains the Mn oxide modification of high activity
Zeolite imidazole ester skeleton structure composite material.
Example 2：The preparation method of the zeolite imidazole ester skeleton structure composite material of Mn oxide modification
(1) precise 3.528g zinc nitrate hexahydrates, 1.944g methylimidazoles, 0.807g sodium formates, with 74ml without
Water methanol mixes, magnetic agitation, and 50% manganese nitrate solutions of 6mL are added dropwise, and keeps magnetic agitation 5min.
(2) the lower processing 10min of gained mixed solution 30kHz ultrasounds.
(3) in the reaction kettle for the polytetrafluoroethyllining lining that the mixed liquor of gained ultrasound pretreatment is put into 100mL, it is placed in baking oven
In, it is to slowly warm up to 140 DEG C and keeps for 24 hours.
(4) gained suspension is after absolute methanol washs 3 times, in 60 DEG C of dry 12h.
(5) obtained solid powder is provided into tube furnace, after good seal, is passed through the High Purity Nitrogen of 50mL/min；Tube furnace is pressed
250 DEG C are warming up to according to the rate of 5 DEG C/min, 5h is kept, is taken out after natural cooling, you can obtains the Mn oxide modification of high activity
Zeolite imidazole ester skeleton structure composite material.
Comparative example 1
Difference with example 2 is：Omit the ultrasonic pre-treatment step of step (2).
Comparative example 2
Difference with example 2 is：Solvent in step (1) is N,N-dimethylformamide.
Comparative example 3
Difference with example 2 is：Omit the activation step of step (5).
Effect experiment
By example 1 and 2, the zeolite imidazole ester skeleton structure composite material of Mn oxide modification prepared by comparative example 1-3 is made
It is used to be catalyzed NH for catalyst3- SCR reacts, and is as follows：
The zeolite imidazole ester skeleton structure composite material preforms that above-mentioned Mn oxide is modified are sieved, and take 0.3g grain sizes 60-
80 mesh catalyst, are put into quartz ampoule, are placed in tube furnace, and volume flow is 100mL/min by temperature programming instrument control system by temperature
NO, O2And N2Mixed gas continue through quartz ampoule, wherein NO in gaseous mixture as the mixed gas of simulated flue gasxIt is dense
It spends for 500ppm, while is passed through concentration as 500ppm NH3As reducing agent, carried out at 230 DEG C, 300 DEG C, 350 DEG C, 400 DEG C
Denitration reaction, and pass through the oxides of nitrogen gas concentration in flue gas analyzer dynamic monitoring tail gas.The removing of specific nitrogen oxides
Rate is as shown in table 1：
Table 1
| 230℃ | 300℃ | 350℃ | 400℃ | |
| Example 1 | 91% | 95% | 93% | 91% |
| Example 2 | 92% | 95% | 93% | 90% |
| Comparative example 1 | 82% | 84% | 83% | 80% |
| Comparative example 2 | 80% | 65% | 20% | 14% |
| Comparative example 3 | 71% | 78% | 77% | 67% |
The experimental results showed that the zeolite imidazole ester skeleton structure composite material of Mn oxide modification prepared by the present invention exists
To NO at 230-400 DEG CxRemoval efficiency up to more than 90%, and ultrasonic pre-treatment step, reaction dissolvent in preparation method and
Activation step can all influence the catalytic performance of composite material.
The foregoing is merely the preferred embodiments of the application, are not limited to the application, for the skill of this field
For art personnel, the application can have various modifications and variations.It is all within spirit herein and principle, made any repair
Change, equivalent substitution, improvement etc., should be included within the protection domain of the application.
Claims (10)
1. one kind is used for NOxThe preparation method of the zeolite imidazole ester skeleton structure composite material of removing, it is characterised in that：Including such as
Lower step：
After raw material needed for the soluble-salt of manganese, synthetic zeolite imidazate skeleton structure composite material and solvent mixing, use is molten
The zeolite imidazole ester skeleton structure composite material of Mn oxide modification is prepared in the hot method of agent；
Solvent, the soluble-salt of manganese and the mass ratio of raw material needed for synthetic zeolite imidazate skeleton structure composite material are 8-10：
0.2-0.75:1。
2. preparation method according to claim 1, it is characterised in that：The soluble-salt of the manganese is manganese nitrate.
3. preparation method according to claim 1, it is characterised in that：The solvent is for content more than 99.5% without water beetle
Alcohol.
4. preparation method according to claim 1, it is characterised in that：The temperature of the solvent-thermal method is 135-145 DEG C, instead
It is 20-30h between seasonable.
5. preparation method according to claim 1, it is characterised in that：Before being prepared using solvent-thermal method, to mixing
Solution afterwards carries out ultrasonic pretreatment；
Preferably, the time of ultrasound pretreatment is 5-10min, supersonic frequency 20-40kHz.
6. preparation method according to claim 1, it is characterised in that：It further includes and lives to the composite material being prepared
It is the step of change, specific as follows：Dried composite material is put into tube furnace, is passed through nitrogen thereto, according to 5-10 DEG C/
The rate of min is warming up to 250 DEG C, keeps 3-5h, the zeolite imidazole ester skeleton modified after cooling up to the Mn oxide of high activity
Structural composite material；
Preferably, the nitrogen is High Purity Nitrogen, and the flow of nitrogen is 45-55mL/min.
7. the zeolite imidazole ester skeleton structure for the Mn oxide modification that any preparation methods of claim 1-6 are prepared is answered
Condensation material.
8. the zeolite imidazole ester skeleton structure composite material that Mn oxide described in claim 7 is modified is in catalysis NH3- SCR reactions are gone
Except the application in NOx.
9. the zeolite imidazole ester skeleton structure composite material that Mn oxide described in claim 7 is modified is as catalyst NH3-
The method of SCR reactions, it is characterised in that：Specifically comprise the following steps：
1) the zeolite imidazole ester skeleton structure composite material preforms for modifying the Mn oxide after activation are sieved, and make composite material
Grain size is 60-80 mesh, obtains catalyst；
2) pending flue gas is flowed through into catalyst, and NH is passed through into flue gas3As reducing agent, denitration is carried out at 230-400 DEG C
Reaction.
10. according to the method described in claim 9, it is characterized in that：The NH being passed through in step 2)3Concentration be 500ppm.
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