CN106964358A - A kind of cadmium ferrite/concave convex rod nano composite material of carbon quantum dot modification and its preparation method and application - Google Patents
A kind of cadmium ferrite/concave convex rod nano composite material of carbon quantum dot modification and its preparation method and application Download PDFInfo
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- CN106964358A CN106964358A CN201710270150.8A CN201710270150A CN106964358A CN 106964358 A CN106964358 A CN 106964358A CN 201710270150 A CN201710270150 A CN 201710270150A CN 106964358 A CN106964358 A CN 106964358A
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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
- B01J23/825—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 gallium, indium or thallium
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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
- B01D53/8628—Processes characterised by a specific catalyst
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/20—Reductants
- B01D2251/206—Ammonium compounds
- B01D2251/2062—Ammonia
Abstract
The invention belongs to denitration catalyst manufacture technology field in environmental protection, and in particular to a kind of cadmium ferrite/concave convex rod nano composite material of carbon quantum dot modification and its preparation method and application.Lanthanum nitrate, ferric nitrate, citric acid and concave convex rod are added in deionized water and stir abundant, is then transferred into water-bath, evaporation obtains wet gel at 50 DEG C~100 DEG C, is impregnated in carbon quantum dot solution, is ground after drying after drying calcining.Photocatalysis denitration is carried out as catalyst using the composite, compared with traditional SCR denitration, energy consumption is greatly reduced, and NO transformation efficiency is significantly improved under low temperature.
Description
Technical field
The invention belongs to denitration catalyst manufacture technology field in environmental protection, and in particular to a kind of iron of carbon quantum dot modification
Sour lanthanum/concave convex rod nano composite material and its preparation method and application.
Background technology
Air pollution is increasingly severe in recent years, and nitrogen oxides is as one of major pollutants of air, to the body of the mankind
Body Health and Living environment causes great harm, such as breathing problem, acid rain, photochemical fog and solid particulate matter PM
2.5 etc., therefore, the prevention and cure of pollution of nitrogen oxides become particularly urgent.
The method of traditional denitration is mainly selective catalytic reduction (SCR), its mainly utilize vanadium titanium catalyst, ammonia or
Nitrogen oxides is decomposed into harmless nitrogen as reducing agent by urea, but has that low temperature active is relatively low, and the larger shortcoming of energy consumption.
By the use of solar energy catalyzing and degrading pollutant matter as new, the potential denitration technology of tool, ground as environmental protection science
The focus studied carefully.
The content of the invention
In order to solve the technical problem of photocatalysis denitration, NO is farthest changed into N under the irradiation of visible ray2,
The invention provides a kind of cadmium ferrite/concave convex rod nano composite material of carbon quantum dot modification, the composite is with carbon quantum dot
Modify the LaFeO that concave convex rod is combined with cadmium ferrite3/ ATP, the composition formula of the composite is expressed as：μ %CQDs/LaFeO3/
In ATP, formula, μ % are carbon quantum dot relative to the mass percent of cadmium ferrite/concave convex rod, μ=1~5.
Present invention also offers a kind of preparation side of cadmium ferrite/concave convex rod nano composite material of above-mentioned carbon quantum dot modification
Method：
(1) lanthanum nitrate, ferric nitrate, citric acid and concave convex rod are added in deionized water and stir abundant, be then transferred into
In water-bath, evaporation obtains wet gel at 50 DEG C~100 DEG C, and grinding produces LaFeO after drying calcining3The nano combined materials of/ATP
Material；
(2) by the LaFeO of gained in step (1)3/ ATP nano composite materials are impregnated in carbon quantum dot solution, after drying
Grinding obtains cadmium ferrite/concave convex rod nano composite material of carbon quantum dot modification,
Wherein, by citric acid, the hydro-thermal method preparation in hydrogen peroxide is obtained carbon quantum dot, hydrogen peroxide and lemon in hydrogen peroxide
The mol ratio of lemon acid is 0.3~0.6：1, hydro-thermal method is specially 160 DEG C of reaction 8h,
Dip time is 15~24h, and drying temperature is 60 DEG C~100 DEG C.
Present invention also offers a kind of application of cadmium ferrite/concave convex rod nano composite material of above-mentioned carbon quantum dot modification：
Photocatalysis denitration is carried out using the composite as catalyst.
The beneficial effects of the present invention are：
Often particle diameter is excessive for carbon quantum dot obtained by existing preparation technology, in this regard, the present invention is in citric acid carbon source water
Hydrogen peroxide is added in thermal process, finds to provide after hydroxyl environment as hydrothermal system, effectively controls generated carbon amounts
The particle diameter of son point is less than 5nm；
Carbon quantum dot/cadmium ferrite/palygorskite nano composite material is prepared using infusion process, perovskite particle diameter is small,
Load Balanced, the microcellular structure of concave convex rod surface molecular sieve analog promotes to NH3Absorption, while cost is reduced, play
The effect of three's concerted catalysis；
Carbon quantum dot has good absorption to visible ray, both can be as electron donor or can be as electron acceptor, can
Light induced electron is faster conducted, be conducive to the raising of catalytic activity；
The present invention has given full play to the excellent photocatalytic activity that carbon quantum dot modification perovskite is produced so that NOx need not be borrowed
High temperature SCR is helped to react, directly at low temperature i.e. can be with reduction decomposition, low temperature active is good, while energy consumption is reduced.
Brief description of the drawings
Fig. 1 is raw material ATP, prepared CQDs, CQDs/LaFeO in embodiment 13/ ATP XRD spectra.
Fig. 2 is the CQDs/LaFeO prepared by embodiment 13The TEM photos of/ATP in 5nm scale ranges.
Fig. 3 is the CQDs/LaFeO prepared by embodiment 13The TEM photos of/ATP in 50nm scale ranges.
Fig. 4 (a) is the 3%CQDs/LaFeO prepared by comparative example 13In/ATP, CQD is in 10nm scale ranges
TEM photos；Fig. 4 (b) is the 3%CQDs/LaFeO prepared by embodiment 13In/ATP, CQD shines in the TEM of 10nm scale ranges
Piece.
Fig. 5 is the raw material A TP of embodiment 1, the LaFeO of the step of embodiment 1 (1) preparation3It is prepared by/ATP, the step of embodiment 1 (2)
3%CQDs/LaFeO34%CQDs/LaFeO prepared by/ATP, embodiment 435%CQDs/ prepared by/ATP, embodiment 5
LaFeO3The inversion cuvers of/ATP respectively to nitrogen oxides.
Embodiment
Embodiment 1
The preparation of carbon quantum dot：
The citric acid for weighing 0.53g is dissolved in the hydrogen peroxide that 20ml concentration of hydrogen peroxide is 0.055mol/L, ultrasonic dissolution
10min, obtains colourless solution；Above-mentioned solution is put into 100ml ptfe autoclaves, then 160 DEG C of hydro-thermal reaction 8h；Instead
Reactor is taken out after should terminating, obtained solution is first centrifuged, bag filter (molecular cut off MWCO=1000) two is transferred to
Dialyse 12h in secondary water, is finally transferred to 70 DEG C of vacuum drying chamber dryings, obtains carbon quantum dot particle CQDs；
(1) 0.4012g lanthanum nitrates, 0.4988g ferric nitrates, 0.5g citric acid 1g concave convex rods are added to 100ml deionizations
Stir abundant in water, be then transferred into water-bath, 18h is evaporated at 60 DEG C and obtains wet gel, with 600 DEG C after 80 DEG C of drying
(heating rate is 1 DEG C/min) calcining 2h, grinding produces LaFeO3/ ATP nano composite materials；
(2) the carbon quantum dot particle 0.03g of above-mentioned preparation is dissolved in 20ml deionized water and obtains carbon quantum dot solution,
Take the LaFeO of gained in step (1)3/ ATP nano composite materials 1g impregnates in the carbon quantum dot solution under room temperature (25 DEG C)
18h, grinding obtains cadmium ferrite/concave convex rod nano composite material 3%CQDs/ of carbon quantum dot modification after 80 DEG C of drying
LaFeO3/ATP。
Cadmium ferrite/concave convex rod nano composite material to the carbon quantum dot modification prepared by the present embodiment carries out X-ray powder
Last diffraction experiment, and observe under transmission electron microscope its pattern and structure,
XRD spectrum is as shown in figure 1, occur in that carbon quantum dot, cadmium ferrite and the respective spy of concave convex rod in the XRD of composite
Diffraction maximum is levied, in combination with TEM photos Fig. 2, it was demonstrated that carbon quantum dot successfully loads to LaFeO3Above/ATP；
Shown in TEM photos such as Fig. 3, Fig. 4 (b), it can be seen that cadmium ferrite particle be less than 10nm and with concave convex rod compared with
To be equably combined with each other；Add the CQDs for preparing of hydrogen peroxide, particle size is uniform, and particle diameter is less than 5nm, with concave convex rod compared with
It is consistent with XRD result to be equably combined with each other.
150mg the present embodiment raw material A TP, this reality are separately added into the quartz ampoule of photocatalysis auxiliary-SCR denitration device
Apply the LaFeO of a step (1) preparation3CQDs/LaFeO prepared by/ATP, the present embodiment step (2)3/ATP；NH3, NO, O2Just
Beginning concentration is respectively 1000ppm, 1000ppm, 3% (relative to total gas flow rate), and remaining is nitrogen, and air speed is 25000h-1, gas
The control of body total flow is in 100ml/min, and used light source is 200W xenon lamp (plus ultraviolet filter plate)；Flue gas is used after reaction 8h
Detector detects residue NO concentration, measures ATP, LaFeO3/ATP、CQDs/LaFeO3The inversion cuver such as Fig. 5 institutes of/ATP to NO
Show, it can be seen that ATP is about 20%, LaFeO to NOx conversion ratio3/ ATP to NO conversion ratio up to more than 50%,
And CQDs/LaFeO3/ ATP is to NO conversion ratio up to more than 95%.
Comparative example 1
Compared to embodiment 1, any hydrogen peroxide is not added in the preparation process of carbon quantum dot, remaining operation is with implementation
Example 1：
The preparation of carbon quantum dot：
The citric acid for weighing 0.53g is dissolved in 20ml deionized waters, and ultrasonic dissolution 10min obtains colourless solution；Will be above-mentioned
Solution is put into 100ml ptfe autoclaves, then 160 DEG C of hydro-thermal reaction 8h；Reaction takes out reactor after terminating, and will obtain
Solution first centrifuge, transfer to the 12h that dialysed in bag filter (molecular cut off MWCO=1000) secondary water, be finally transferred to 70
DEG C vacuum drying chamber is dried, and obtains carbon quantum dot particle CQDs；
(1) be the same as Example 1；
(2) be the same as Example 1.
Cadmium ferrite/concave convex rod nano composite material to the carbon quantum dot modification prepared by this comparative example is electric in transmission
Its pattern of Microscopic observation and structure：
Shown in TEM photos such as Fig. 4 (a), it can be seen that the CQDs of hydrogen peroxide preparation is not added, particle size point
Cloth is uneven, there is a situation where that particle diameter is significantly greater than 10nm.
The CQDs/LaFeO prepared in photocatalysis auxiliary-SCR denitration test experience be the same as Example 1, comparative example 13/
ATP only reaches 82% to NO conversion ratio.
Embodiment 2
(1) be the same as Example 1；
(2) the carbon quantum dot particle 0.01g prepared in embodiment 1 is dissolved in 20ml deionized water and obtains carbon quantum dot
Solution, takes the LaFeO of gained in step (1)3/ ATP nano composite materials 1g is in the carbon quantum dot solution under room temperature (25 DEG C)
24h is impregnated, grinding obtains cadmium ferrite/concave convex rod nano composite material of carbon quantum dot modification after 100 DEG C of drying.
Embodiment 3
(1) be the same as Example 1；
(2) the carbon quantum dot particle 0.02g prepared in embodiment 1 is dissolved in 20ml deionized water and obtains carbon quantum dot
Solution, takes the LaFeO of gained in step (1)3/ ATP nano composite materials 1g is in the carbon quantum dot solution under room temperature (25 DEG C)
20h is impregnated, grinding obtains cadmium ferrite/concave convex rod nano composite material of carbon quantum dot modification after 80 DEG C of drying.
Embodiment 4
(1) be the same as Example 1；
(2) the carbon quantum dot particle 0.04g prepared in embodiment 1 is dissolved in 20ml deionized water and obtains carbon quantum dot
Solution, takes the LaFeO of gained in step (1)3/ ATP nano composite materials 1g is in the carbon quantum dot solution under room temperature (25 DEG C)
18h is impregnated, grinding obtains cadmium ferrite/concave convex rod nano composite material of carbon quantum dot modification after 80 DEG C of drying.
Embodiment 5
(1) be the same as Example 1；
(2) the carbon quantum dot particle 0.05g prepared in embodiment 1 is dissolved in 20ml deionized water and obtains carbon quantum dot
Solution, takes the LaFeO of gained in step (1)3/ ATP nano composite materials 1g is in the carbon quantum dot solution under room temperature (25 DEG C)
15h is impregnated, grinding obtains cadmium ferrite/concave convex rod nano composite material of carbon quantum dot modification after 60 DEG C of drying.
Claims (7)
1. a kind of cadmium ferrite/concave convex rod nano composite material of carbon quantum dot modification, it is characterised in that：Described composite with
Carbon quantum dot modifies the LaFeO that concave convex rod is combined with cadmium ferrite3/ATP。
2. a kind of preparation method of cadmium ferrite/concave convex rod nano composite material of carbon quantum dot modification as claimed in claim 1,
It is characterized in that：The preparation method is,
(1) lanthanum nitrate, ferric nitrate, citric acid and concave convex rod are added in deionized water and stir abundant, be then transferred into water-bath
In pot, evaporation obtains wet gel at 50 DEG C~100 DEG C, and grinding produces LaFeO after drying calcining3/ ATP nano composite materials；
(2) by the LaFeO of gained in step (1)3/ ATP nano composite materials are impregnated in carbon quantum dot solution, are ground after drying
Obtain cadmium ferrite/concave convex rod nano composite material of carbon quantum dot modification.
3. the preparation method of cadmium ferrite/concave convex rod nano composite material of carbon quantum dot modification as claimed in claim 2, it is special
Levy and be：By citric acid, the hydro-thermal method preparation in hydrogen peroxide is obtained carbon quantum dot described in step (2).
4. the preparation method of cadmium ferrite/concave convex rod nano composite material of carbon quantum dot modification as claimed in claim 3, it is special
Levy and be：In described hydrogen peroxide, the mol ratio of hydrogen peroxide and citric acid is 0.3~0.6：1.
5. the preparation method of cadmium ferrite/concave convex rod nano composite material of carbon quantum dot modification as claimed in claim 3, it is special
Levy and be：Described hydro-thermal method is specially 160 DEG C of reaction 8h.
6. the preparation method of cadmium ferrite/concave convex rod nano composite material of carbon quantum dot modification as claimed in claim 2, it is special
Levy and be：In step (2), dip time is 15~24h, and drying temperature is 60 DEG C~100 DEG C.
7. a kind of application of cadmium ferrite/concave convex rod nano composite material of carbon quantum dot modification as claimed in claim 1, it is special
Levy and be：Photocatalysis denitration is carried out using the composite as catalyst.
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| CN108822840A (en) * | 2018-08-29 | 2018-11-16 | 济南大学 | A kind of fiber crops are the preparation method of carbon source neodymium doped carbon quantum dot composite material |
| CN110773219A (en) * | 2019-10-30 | 2020-02-11 | 中国海洋大学 | photo-Fenton desulfurization and denitrification catalyst and preparation method thereof |
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| CN111185178A (en) * | 2020-02-03 | 2020-05-22 | 齐齐哈尔大学 | Preparation method of carbon quantum dot modified denitration catalyst |
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