CN109225237A - A kind of 3DOM Ce-Co-M composite catalyst and preparation method and application - Google Patents
A kind of 3DOM Ce-Co-M composite catalyst and preparation method and application Download PDFInfo
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- CN109225237A CN109225237A CN201810884912.8A CN201810884912A CN109225237A CN 109225237 A CN109225237 A CN 109225237A CN 201810884912 A CN201810884912 A CN 201810884912A CN 109225237 A CN109225237 A CN 109225237A
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/16—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation
- C07C51/21—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen
- C07C51/255—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of compounds containing six-membered aromatic rings without ring-splitting
- C07C51/265—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of compounds containing six-membered aromatic rings without ring-splitting having alkyl side chains which are oxidised to carboxyl groups
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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Abstract
The invention discloses a kind of 3DOM Ce-Co-M composite catalysts, have three-dimensional ordered mesoporous structure 3DOM Ce-Co-M, M=Cu or Mn, wherein in terms of atomic molar ratio, Ce:Co:M=0.5~1:0.5~1:0.5~2；The invention also discloses the preparation methods of 3DOM Ce-Co-M composite catalyst, comprising the following steps: (1) weighs cerous nitrate and cobalt nitrate dissolution in a solvent；(2) polyethylene glycol is added, stirs evenly；(3) 40~60% ethyl alcohol is added while stirring, at least one of copper nitrate and manganese nitrate are added after mixing, is completely dissolved rear stirring in water bath；(4) citric acid is added and stirs, then solution is placed under ice bath, PMMA template is added, is stirred under ice bath；(5) obtained product is stood to 3~5h under condition of ice bath, obtained solid is gone into template and calcining again after dry.
Description
Technical field
The present invention relates to the catalyst fields for VOCs exhaust-gas treatment, compound more particularly to a kind of 3DOM Ce-Co-M
Catalyst and preparation method and application.
Background technique
Volatile organic matter (Volatile Organic Compounds, abbreviation VOCs) refer to boiling spread 50~
Between 260 DEG C, saturated vapour pressure is more than 133.32Pa at room temperature, and the one kind being present in air in vapour form at normal temperature has
Machine object, including it is non-methane hydrocarbon (alkane, alkene, alkynes, halogenated hydrocarbons etc.), oxygen-bearing organic matter (aldehyde, ketone, alcohol etc.), nitrogenous organic
Object, sulfurous organic compound etc..According to its chemical structure and concentration, photochemical fog can produce, secondary particulate and troposphere are smelly
Oxygen etc., will also result in global warming aggravation and stratospheric ozone layer deteriorates, and Long Term Contact VOCs leads to a series of respiratory system diseases
Disease, leukemogenesis, liver and kidney failure increase cancer morbidity, have serious harmfulness to human body and environment.
Benzene homologues (benzene,toluene,xylene) are the important components of VOCs, have the characteristics that toxicity is big, difficult to degrade.Two
Toluene is a kind of important Organic Chemicals, and can be used as fabulous industrial solvent, be widely used in coating, resin, dyestuff,
The industries such as ink, medicine, explosive, pesticide；Also it can be used as high octane gasoline component；It can be also used for the pitch of removal vehicle body；
Hospital pathology department is mainly used for the transparent and dewaxing of tissue, slice.
Since most of VOCs are harmful to environment and human health, many technologies can be used for controlling VOC emission, traditional
Method such as absorption, absorption, burning, photochemical catalytic oxidation and catalysis burning.But these methods come with some shortcomings, if condensation method is to waving
The higher exhaust-gas treatment effect of hair property is bad；Absorption process processing cost is lower and effect is good, but the post-processing of absorbent at
This height easily causes secondary pollution；Bioanalysis is not well suited for the organic exhaust gas that processing has bio-toxicity.Low-temperature catalytic oxidation is due to it
High efficiency and low cost are considered as reducing one of most promising approach of VOCs, and wherein critical issue is high performance catalyst
Availability.Therefore, it is intended that manufacture low temperature high activity catalyst, to reduce the high energy of removal low concentration VOC.
In catalytic combustion technology, the core for being catalyzed burning is the activity and stability of catalyst.Catalyst performance it is excellent
It is bad to have conclusive influence to catalytic efficiency and reduction operating cost.Active component plays the property of catalyst conclusive
Effect, according to the difference of the active component of catalyst, catalyst can be divided into noble metal catalyst and non-precious metal catalyst.
At present in low temperature catalyst with more for noble metal, higher cost and resource is limited, in industrial applicability
Produce significant limitation.Non-noble metal research had become one of hot spot in recent years；Have many noble metals to combine
The research of non-precious metal catalyst, while also having the research of base metal multiplex catalyst.Noble metal be mainly Au, Pt,
Pd etc., base metal is mainly based on the non-noble metal oxides such as Cu, Mn, Cr, Co, Ce, Fe.Multiplex catalyst is main
It is the combination degrading benzene object of transition metal and rare earth metal, the composite catalysts such as including Mn-Ce, Ce-Co, Ce-Mn-Cu.
Summary of the invention
The present invention provides a kind of 3DOM Ce-Co-M composite catalysts, can better catalytic degradation VOCs (main diformazan
Benzene) exhaust gas.
A kind of 3DOM Ce-Co-M composite catalyst, have three-dimensional ordered mesoporous structure 3DOM Ce-Co-M, M=Cu or
Mn, wherein in terms of atomic molar ratio, Ce:Co:M=0.5~1:0.5~1:0.5~2.
A kind of preparation method of 3DOM Ce-Co-M composite catalyst, comprising the following steps:
(1) cerous nitrate and cobalt nitrate dissolution are weighed in a solvent；
(2) polyethylene glycol is added in the solution of step (1), stirs evenly；
(3) 40~60% ethyl alcohol is added while stirring in the solution that step (2) obtains, nitric acid is added after mixing
At least one of copper and manganese nitrate are completely dissolved rear stirring in water bath；
(4) citric acid is added in the solution that step (3) obtains and stirs, then solution is placed under ice bath, is added
PMMA template stirs under ice bath；
PMMA (polymethyl methacrylate) template is to be prepared using metal oxide as carrier using colloidal crystal templates method
It forms, partial size is 200~500nm, it is preferred that partial size is 250~350nm.
(5) product for obtaining step (4) stands 3~5h under condition of ice bath, then filters after removing extra solution,
It is placed on drying in drying box, then obtained solid is gone into template and calcining.
Specific solid is placed in tube type resistance furnace in quartz ampoule and goes template, calcining.
Preferably 99.7% dehydrated alcohol of solvent used in step (1), the mole of nitrate is between 0.5~2.Step
(1) and in step (3) three kinds of mixed metal ions are made to stablize in alcoholic solution, be uniformly dispersed using ultrasonic agitation process.
Polyethylene glycol (PEG400) is good surfactant and dispersing agent in step (2), and additive amount is the nitrate of M
The 10%~20% of alcoholic solution volume.
In order to be sufficiently mixed it more, guarantee that the composite catalyst being prepared has good catalytic effect, preferably
, in step (2), the water bath condition of stirring is at 30~40 DEG C.Mixing time is 15~30min.
Preferably, 0.8~2mol/L of total concentration of total metal ion in precursor solution, it is further preferred that forerunner
1~1.5mol/L of total concentration of total metal ion in liquid solution.
Efficiency and mixing uniformity in order to balance guarantee that the composite catalyst being prepared has good catalytic effect,
Preferably, it in step (3), is completely dissolved under ultrasound condition, stirring in water bath 8min~15min.Water bath condition is 30~40
℃。
Efficiency and mixing uniformity in order to balance guarantee that the composite catalyst being prepared has good catalytic effect,
Preferably, in step (4), citric acid is added and stirs 8min~15min.The citric acid of addition is complexing agent, is capable of increasing ratio
Surface area, the temperature of ice bath is generally at 9~15 DEG C.
Efficiency and mixing uniformity in order to balance guarantee that the composite catalyst being prepared has good catalytic effect,
Preferably, in step (4), 20min~40min is stirred under ice bath.
In order to improve the effect of catalyst, it is preferred that in step (3), in obtained 3DOMCe-Co-M, rubbed with atom
You are than meter, Ce:Co:M=0.5~1:0.5~1:0.5~2.
In order to improve the effect of catalyst, it is further preferred that in step (3), in obtained 3DOM Ce-Co-M, with
Atomic molar is than meter, Ce-Co-M=0.5~1:0.5~1:0.5~1.
Lower dosage simultaneously in order to which polyethylene glycol plays best effect, it is preferred that in step (2), polyethylene glycol adds
Dosage is 10%~20%, the M=Cu or Mn of the nitrate alcoholic solution volume of M.
In order to improve catalyst quality, it is preferred that step (5) drying condition be 50~80 DEG C, the time be 12~for 24 hours, protect
Moisture in card template is evaporated.
In order to improve catalyst quality, it is further preferred that detailed process is as follows for the calcining of step (5): by obtained solid
It in quartz ampoule, is placed in tube type resistance furnace, in inert gas (N2) under atmosphere, with the rate less than or equal to 1 DEG C/min from
Room temperature rises to 200 DEG C~400 DEG C and keeps the temperature 2~5h, then to be raised to 400 DEG C~600 DEG C less than or equal to 1 DEG C/min and keep the temperature
0.5~2h, then it is placed on 500 DEG C~600 DEG C 3~8h of heat preservation in Muffle furnace.Finally obtained 3DOM Ce-Co-Cu composite catalyst.
Guarantee that the integrality of template, heating rate cause formwork structure to collapse, destroy its structure fastly.
Above-mentioned 3DOM Ce-Co-M composite catalyst is put into tube type resistance furnace by a kind of method of degradation organic waste gas
Quartz ampoule in catalysis organic exhaust gas carry out degradation reaction, reaction temperature is 80~320 DEG C, air speed is 15000~80000h-1。
The invention has the benefit that
(1) present invention is to be assisted using three-dimensional ordered mesoporous PMMA as template with polyethylene glycol (PEG400) and citric acid
Sol-gal process combines 3DOM Ce-Co-M composite catalyst obtained, is suitble to the preparation of a variety of mesopore oxides.
(2) transition metal of the invention and rare earth metal dispersion degree are higher, and catalyst preparation is easy to operate, and raw material is inexpensively easy
?.
(3) 3DOM Ce-Co-M composite catalyst specific surface area of the invention is high, oxygen storage capacity is big, by 3DOM Ce-Co-M (M
=Cu or Mn) catalyst is for removing organic exhaust gas (dimethylbenzene), 3DOM Ce-Co-Cu111, T90%=260 DEG C, be a kind of high
The low temperature catalyst of effect, and excellent low temperature, efficient catalytic are shown under the conditions of 1000ppm xylene concentration below
Energy.
(4) present invention obtains the catalyst being most suitable for compared with low-temperature catalytic burning by different metallic atom ratios.
Detailed description of the invention
Fig. 1 is that the 3DOM Ce-Co-Cu composite catalyst obtained using the method for embodiment 1 degrades two at different temperatures
The curve graph of toluene.
Fig. 2 is that the 3DOM Ce-Co-Mn composite catalyst obtained using the method for embodiment 2 degrades two at different temperatures
The curve graph of toluene.
Specific embodiment
The following example is only intended to that the present invention will be described in detail, and agents useful for same is that analysis is pure in following embodiment.
Embodiment 1
The preparation method of the 3DOM Ce-Co-Cu composite catalyst of the degradation VOCs exhaust gas of the present embodiment, including following step
It is rapid:
(1) it weighs cerous nitrate, cobalt nitrate each 5mmol, 10ml to be dissolved in the ethanol solution of 20ml, ultrasonic 5min,
It makes it completely dissolved；
(2) polyethylene glycol (PEG400) of 3ml, then water-bath are added in the mixed metal alcoholic solution that step (1) obtains
It stirs evenly, and stirs 20min under the conditions of 35 DEG C；
(3) ethyl alcohol of 10ml 50% is added while stirring in step (2), 5mmol copper nitrate is added after mixing,
It is completely dissolved under ultrasound condition, 35 DEG C of stirring 10min of water-bath；
(4) 2.10g citric acid is added in step (3), stirs 10min；Solution is placed under 10 DEG C of ice baths, and to its
Middle addition 2.5gPMMA template；And 30min is stirred under ice bath.
(5) 4h will be stood under step (4) condition of ice bath, then filters after removing extra solution, is placed on 70 DEG C of drying boxes
Middle drying for 24 hours, then by obtained solid is placed in tube type resistance furnace, in the quartz ampoule of d=8mm in N2Under atmosphere with 1 DEG C/
The rate of min rises to 300 DEG C from room temperature and keeps the temperature 3h, is then raised to 500 DEG C with 1 DEG C/min and keeps the temperature 1h, then is placed on Muffle furnace
In 500 DEG C of heat preservation 4h.Finally obtained 3DOM Ce-Co-Cu (in terms of atomic molar ratio, Ce:Co:Cu=1:1:1) composite catalyzing
Agent.
Embodiment 2
The preparation method of the 3DOM Ce-Co-Cu composite catalyst of the degradation VOCs exhaust gas of the present embodiment, including following step
It is rapid:
(1) it weighs cerous nitrate, cobalt nitrate each 5mmol, 10ml respectively to be dissolved in the ethanol solution of 20ml, ultrasound
5min makes it completely dissolved；
(2) polyethylene glycol (PEG400) of 3ml, then water-bath are added in the mixed metal alcoholic solution that step (1) obtains
It stirs evenly, and stirs 20min under the conditions of 35 DEG C；
(3) ethyl alcohol of 10ml 50% is added while stirring in step (2), 10mmol manganese nitrate is added after mixing,
It is completely dissolved under ultrasound condition, 35 DEG C of stirring 10min of water-bath；
(4) 2.10g citric acid is added in step (3), stirs 10min；Solution is placed under 10 DEG C of ice baths, and to its
Middle addition 2.5gPMMA template；And 30min is stirred under ice bath.
(5) 4h will be stood under step (4) condition of ice bath, then filters after removing extra solution, is placed on 70 DEG C of drying boxes
Middle drying for 24 hours, then by obtained solid is placed in tube type resistance furnace, in the quartz ampoule of d=8mm in N2Under atmosphere with 1 DEG C/
The rate of min rises to 300 DEG C from room temperature and keeps the temperature 3h, is then raised to 500 DEG C with 1 DEG C/min and keeps the temperature 1h, then is placed on Muffle furnace
In 500 DEG C of heat preservation 4h.Finally obtained 3DOM Ce-Co-Mn (in terms of atomic molar ratio, Ce:Co:Mn=1:1:2) composite catalyzing
Agent.
The catalyst that embodiment 1 and embodiment 2 are prepared is tested for the property, test method are as follows: 1 He of Example
Each 125mg of the catalyst that embodiment 2 obtains, is respectively placed in the quartz ampoule in tube type resistance furnace, is fixed with silica wool.With
GC1690 continuously detects the concentration of quartz ampoule inlet end and outlet side dimethylbenzene, quartz ampoule inlet end and outlet side dimethylbenzene it is dense
The concentration before that is to say dimethylbenzene degradation and after degradation is spent, the available dimethylbenzene of concentration of calculating dimethylbenzene degradation front and back is passed through
Degradation rate.Wherein reaction gas forms are as follows: 300~1000ppm dimethylbenzene and 21% oxygen and 79% nitrogen, wherein using nitrogen
Carrier gas is done, the flow velocity of reaction gas is 100mL/min, air speed 48000h-1.Activity rating temperature is 80~360 DEG C, different temperatures
Under, the conversion ratio of catalyst reduction dimethylbenzene is shown in Table 1, and variation with temperature situation is as illustrated in fig. 1 and 2:
The degradation rate of 1. 3DOM Ce-Co-Cu composite catalyst paraxylene of table
Claims (10)
1. a kind of 3DOM Ce-Co-M composite catalyst, which is characterized in that there is three-dimensional ordered mesoporous structure 3DOM Ce-Co-M,
M=Cu or Mn, wherein in terms of atomic molar ratio, Ce:Co:M=0.5~1:0.5~1:0.5~2.
2. a kind of preparation method of 3DOM Ce-Co-M composite catalyst, which comprises the following steps:
(1) cerous nitrate and cobalt nitrate dissolution are weighed in a solvent；
(2) polyethylene glycol is added in the solution of step (1), stirs evenly；
(3) 40~60% ethyl alcohol is added while stirring in the solution that step (2) obtains, after mixing be added copper nitrate and
At least one of manganese nitrate is completely dissolved rear stirring in water bath；
(4) citric acid is added in the solution that step (3) obtains and stirs, then solution is placed under ice bath, PMMA mould is added
Plate stirs under ice bath；
(5) product for obtaining step (4) stands 3~5h under condition of ice bath, then filters after removing extra solution, is placed on
It is dry in drying box, then obtained solid is gone into template and calcining.
3. the preparation method of 3DOM Ce-Co-M composite catalyst as claimed in claim 2, which is characterized in that in step (2),
The water bath condition of stirring is at 30~40 DEG C.
4. the preparation method of 3DOM Ce-Co-M composite catalyst as claimed in claim 2, which is characterized in that in step (3),
It is completely dissolved under ultrasound condition, stirring in water bath 8min~15min.
5. the preparation method of 3DOM Ce-Co-M composite catalyst as claimed in claim 2, which is characterized in that in step (4),
Citric acid is added and stirs 8min~15min.
6. the preparation method of 3DOM Ce-Co-M composite catalyst as claimed in claim 2, which is characterized in that in step (4),
20min~40min is stirred under ice bath.
7. the preparation method of 3DOM Ce-Co-M composite catalyst as claimed in claim 2, which is characterized in that in step (3)
In, in obtained 3DOMCe-Co-M, in terms of atomic molar ratio, Ce:Co:M=0.5~1:0.5~1:0.5~2, M=Cu or
Mn。
8. the preparation method of 3DOM Ce-Co-M composite catalyst as claimed in claim 2, which is characterized in that in step (3)
In, in obtained 3DOM Ce-Co-M, in terms of atomic molar ratio, Ce-Co-M=0.5~1:0.5~1:0.5~1, M=Cu or
Mn。
9. the preparation method of 3DOM Ce-Co-M composite catalyst as claimed in claim 2, which is characterized in that in step (2),
The additive amount of polyethylene glycol is 10%~20%, the M=Cu or Mn of the nitrate alcoholic solution volume of M.
10. a kind of method of degradation organic waste gas, which is characterized in that will be by as described in claim 2~9 any claim
The composite catalyst that is prepared of preparation method of 3DOM Ce-Co-M composite catalyst be put into the quartz in tube type resistance furnace
It is catalyzed organic exhaust gas in pipe and carries out degradation reaction, reaction temperature is 80~320 DEG C, air speed is 15000~80000h-1。
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| CN113842922A (en) * | 2021-09-08 | 2021-12-28 | 南京工业大学 | Composite aerogel and preparation method and application thereof |
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