CN105771967A - Metal oxide-vanadate/attapulgite catalyst - Google Patents
Metal oxide-vanadate/attapulgite catalyst Download PDFInfo
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- CN105771967A CN105771967A CN201610188507.3A CN201610188507A CN105771967A CN 105771967 A CN105771967 A CN 105771967A CN 201610188507 A CN201610188507 A CN 201610188507A CN 105771967 A CN105771967 A CN 105771967A
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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
- 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
- B01D53/8665—Removing heavy metals or compounds thereof, e.g. mercury
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/32—Manganese, technetium or rhenium
- B01J23/34—Manganese
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
- B01D2258/0283—Flue gases
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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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
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Abstract
The invention relates to a metal oxide-vanadate/attapulgite catalyst, which is characterized in that the metal oxide-vanadate/attapulgite catalyst is prepared by loading metal oxide TOx and vanadate RVO4 together on attapulgite ATP. T in the metal oxide TOx is Ce, Zr or Mn. R in the vanadate RVO4 is Ce, Mn or Fe. The invention loads the metal oxide and the vanadate together on the clay material attapulgite, the metal oxide-vanadate/attapulgite catalyst is used for flue gas denitrification and demercuration and dye waste water decolorization, and compared with the prior art, the metal oxide-vanadate/attapulgite catalyst has the following remarkable advantages: (1) the existing catalyst cost of coal-fired flue gas denitrification and demercuration can be reduced; (2) the rate of simultaneous coal-fired flue gas denitrification and demercuration can be increased; (3) SCR (Selective Catalytic Reduction) denitrification equipment can be utilized when demercuration is performed with the catalyst, so equipment cost is reduced; (4) dye waste water adsorbent is mainly active carbon at present, so the cost is high; the catalyst disclosed by the invention reduces waste water COD (Chemical Oxygen Demand) while decolorizing dye waste water, so the cost is low.
Description
Technical field
The invention belongs to field of environmental technology, particularly relate to the loaded catalyst of a kind of separation technology field, available
The decolouring of Elemental Mercury and waste water from dyestuff is taken off in flue gas.
Background technology
In recent years, it should be noted that some materials produced in coal combustion process have large effect to environment, these things
Matter just includes hydrargyrum and nitrogen oxides.The coal-fired sulfur dioxide produced and nitrogen oxides are the most former of formation " acid rain " and " acid mist "
One of because of, and the hydrargyrum of severe toxicity, is also one of intoxicating factor in haze weather.Owing to hydrargyrum has in environmental and biological materials
Extra high accumulation, even therefore in the case of concentration is low-down, the mankind and wild animals and plants are also had the biggest by it
Toxicity, hydrargyrum is defined as a kind of element with highly dangerous by EPA.
Selective catalytic reduction (SCR) catalyst is industrially mainly used in denitrating flue gas at present, and the method can reach
To the NO of 80%~90%XReduction rate.The most many researcher research SCR catalyst demercurations, metal-oxide needs to be supported on load
On body can demercuration, commonly utilized carrier is titanium dioxide, silicon dioxide and activated carbon etc., but such catalyst is easy
Easily poisoning, it is difficult to regeneration, cost is the highest is difficult to industrialization.
Vanadate is due to its higher catalysis activity, and the advantages such as pyrolytic degree is little, are a kind of important selective catalysis
Oxidation catalyst.And China's attapulgite resource is enriched, its level of resource utilization is relatively low.Attapulgite (ATP) also known as Paligorskite,
It is a kind of layer chain richness magnesium silicate clay mineral, in needle-like or threadiness, there is bigger specific surface area (146~210m2/
G), there is-OH the tissue that can react on surface, and special layer chain structure can produce the zeolites duct of prosperity, and has general
Viscous soil characteristics: cation commutativity, water absorption, expansiveness etc..Due to the character that it is special, conventional the doing of attapulgite is adsorbed
The carrier of agent, catalyst and catalyst.
Summary of the invention
While research, denitration demercuration catalyst is mainly SCR catalyst at present, but metal-oxide needs to be supported on load
On body can demercuration, commonly utilized carrier is titanium dioxide, silicon dioxide and activated carbon etc., but such catalyst is easy
Poisoning, it is difficult to regeneration, cost is the highest is difficult to industrialization.The oxygenation efficiency of the fine Elemental Mercury of SCR catalyst denitration effect simultaneously
Low, demercuration rate is the highest.
Vanadate has higher catalysis activity, and pyrolytic degree is little, is important selective oxidation catalyst.I
State's attapulgite resource is enriched, and its level of resource utilization is relatively low.Attapulgite has bigger specific surface area, special layer chain
Structure can produce the zeolites duct of prosperity, therefore can be as the carrier of adsorbent, catalyst and catalyst.Use attapulgite
Carrier as SCR catalyst can be substantially reduced catalyst cost, therefore can also improve catalysis with it as catalyst carrier
The denitration rate of agent and demercuration rate.Not only there is adsorption function but also there is certain catalysis, at decoloring dye waste water due to it again
And the reduction aspect of COD also has good effect.
It is an object of the invention to provide a kind of metal-oxide-alum salts/Attapulgite Catalyst, at denitrating flue gas
Demercuration and the decolouring of waste water from dyestuff.
The present invention also aims to provide the preparation method of a kind of metal-oxide-alum salts/Attapulgite Catalyst.
The present invention is achieved through the following technical solutions: a kind of metal-oxide-alum salts/Attapulgite Catalyst,
It is characterized in that: by metal-oxide TOxWith alum salts RVO4Mutual load is prepared from attapulgite ATP.
Described metal-oxide TOxIn T be Ce, Zr or Mn.
Described alum salts RVO4In R be Ce, Mn or Fe.
The preparation method of described metal-oxide-alum salts/Attapulgite Catalyst, it is characterised in that: first use hydro-thermal
Synthetic method prepares RVO4/ ATP, then use sol-gal process to prepare metal-oxide-alum salts/Attapulgite Catalyst TOx-
RVO4/ATP。
Preparation process is as follows:
(1) weigh the ammonium metavanadate of equimolar amounts and manganese nitrate or cerous nitrate or ferric nitrate, be respectively placed in two beakers addition
Suitable quantity of water is dissolved;
(2) weigh appropriate pure attapulgite ATP to add in deionized water, be simultaneously introduced a small amount of dispersant PEG400, stir
Mixing certain time makes it be uniformly dispersed;
(3) step (2) prepare ATP deionized water in be slowly added dropwise respectively ammonium metavanadate solution and cerous nitrate or manganese nitrate or
Iron nitrate solution, moves into hydrothermal reaction kettle after adding proper ammonia regulation pH=9 ~ 14 interior at 120 ~ 180 DEG C after stirring certain time
Under the conditions of react 7 ~ 12 hours;
(4) it is washed with deionized after sucking filtration, until using AgNO3Detection is without Cl-Exist;Dry at 80 DEG C, grind and obtain RVO4/
ATP, R are Ce, Mn or Fe;
(5) configure the citric acid solution of 2mol/L, weigh appropriate manganese nitrate or cerous nitrate or zirconium nitrate to join citric acid molten
In liquid, after being completely dissolved, form manganese or the precursor citric acid solution of cerium or zirconium;
(6) RVO that appropriate step (4) prepares is weighed4/ ATP joins in the precursor citric acid solution that step (5) prepares, and fills
Add appropriate glacial acetic acid after dividing stirring under the conditions of uniform temperature, stir ageing 12 ~ 16 hours;
(7) regulate pH=9 ~ 14 with ammonia, react at a certain temperature to gel;Muffle furnace is put at sky after drying 24 hours
Roasting under gas atmosphere, grinding obtain metal-oxide-alum salts/Attapulgite Catalyst TOx-RVO4/ ATP, wherein T is Ce, Zr
Or Mn;R is Ce, Mn or Fe.
Described step (6): wherein add appropriate glacial acetic acid and stir ageing 12 hours under the conditions of 60 DEG C.
Described step (7): regulate pH=8 with ammonia, reacts to gel at temperature 80 DEG C, dries 24 at 80 DEG C
Hour put into Muffle furnace in air atmosphere at 400 DEG C roasting grind after 6 hours and obtain metal-oxide-alum salts/attapulgite
Soil catalyst TOx-RVO4/ ATP, wherein T is Ce, Zr or Mn;R is Ce, Mn or Fe.
The method have the advantages that and propose metal-oxide and alum salts mutual load first in clay material
Attapulgite is also used for denitrating flue gas demercuration and decoloring dye waste water.Compared with prior art there is a following remarkable advantage:
(1) coal-fired flue gas denitration demercuration existing catalyst cost is reduced.
(2) coal-fired flue-gas denitration demercuration rate simultaneously is improved.
(3) may utilize SCR denitration equipment during this catalyst demercuration, reduce equipment cost.
(4) dye wastewater adsorbent is mainly activated carbon at present, and cost is high, and the catalyst of the present invention takes off for waste water from dyestuff
Color reduces waste water COD simultaneously, with low cost.
Detailed description of the invention
Metal-oxide-alum salts/Attapulgite Catalyst the TO of the present inventionx-RVO4/ ATP is a kind of denitrating flue gas demercuration
Catalyst and decoloring dye waste water agent, it is by TOx(T is Ce, Zr, Mn) and RVO4(R is Ce, Mn, Fe) mutual load is in recessed
Convex rod soil is prepared from.It utilizes hydrothermal synthesis method to prepare RVO4/ ATP(R is Ce, Mn, Fe), and use sol-gal process to prepare
TOx-RVO4/ ATP(T is Ce, Zr, Mn;R is Ce, Mn, Fe).
Preparation method:
(1) weigh original attapulgite to be scattered in deionized water, after being sufficiently stirred for, form suspension, add appropriate six phosphorus partially
Acid sodium, after ultrasonic Treatment 4 ~ 12h, falls to analyse upper strata turbid solution, attapulgite is cleaned multiple times with distilled water after centrifugation, then at
Dry at 80 DEG C attapulgite clay after purifying soil is standby.
(2) ammonium metavanadate and the manganese nitrate (cerous nitrate, ferric nitrate) that weigh equimolar amounts add in two beakers
Suitable quantity of water is dissolved.
(3) (adding a small amount of dispersant PEG400) stirring in a certain amount of pure ATP addition deionized water is weighed certain
Time chien shih its be uniformly dispersed.
(4) ammonium metavanadate solution and cerous nitrate (manganese nitrate, ferric nitrate) solution it are slowly added dropwise respectively, after stirring certain time
7 ~ 12h is reacted under the conditions of 120-~ 180 DEG C in immigration hydrothermal reaction kettle after adding proper ammonia regulation pH=9 ~ 14.
(5) it is washed with deionized after sucking filtration, until without Cl-Exist and (use AgNO3Detection).Drying at 80 DEG C, grinding obtains
RVO4/ ATP(R is Ce, Mn, Fe).
(6) configure the citric acid solution 500ml of 2mol/L, weigh a certain amount of manganese nitrate (cerous nitrate, zirconium nitrate) and add
In 100ml citric acid solution, the two is made to be dissolved completely in citric acid solution the precursor citric acid of formation manganese (cerium, zirconium) molten
Liquid.
(7) appropriate RVO is weighed4/ ATP(R is Ce, Mn, Fe) add (5) mixed liquor be sufficiently stirred for after add appropriate glacial acetic acid in one
Ageing 12 ~ 16h is stirred under the conditions of fixed temperature.
(8) regulate pH=9 ~ 14 with ammonia, react at a certain temperature to gel.Muffle furnace is put into after drying 24 hours
Roasting in air atmosphere, grinding obtain TOx-RVO4/ ATP(T is Ce, Zr, Mn;R is Ce, Mn, Fe).
Embodiment 1:MnO2-CeVO4The preparation of/ATP
(1) weigh 4mmol ammonium metavanadate and 4mmol cerous nitrate in two beakers, add suitable quantity of water dissolving.
(2) weigh 4gATP to add (adding a small amount of dispersant PEG400) in 20ml water and stir 1 hour and make it disperse
Uniformly.
(3) being slowly added dropwise ammonium metavanadate solution and cerous nitrate solution respectively, stirring 1 as a child added proper ammonia regulation pH
Keep 8 hours under the conditions of 150 DEG C in immigration hydrothermal reaction kettle after=10.
(4) it is washed with deionized after sucking filtration, until without Cl-Exist and (use AgNO3Detection).Drying at 80 DEG C, grinding obtains
CeVO4/ATP。
(5) taking the manganese nitrate of 2mmol, to be dissolved in the 2mol/L citric acid solution of 50ml formation mixing precursor citric acid molten
Liquid.
(6) 2gCeVO is weighed4/ ATP adds (5) mixed liquor and is sufficiently stirred for.Stirring 1 the most afterwards add 2ml glacial acetic acid in
Stirring ageing 12 hours under the conditions of 60 DEG C.
(7) regulate pH to 8 with ammonia, react to gel at temperature 80 DEG C.Dry 24 hours at 80 DEG C, put into horse
Not stove in air atmosphere at 400 DEG C roasting grind after 6 hours and obtain MnO2-CeVO4/ATP。
Embodiment 2: catalyst flue gas demercuration active testing example
The catalyst 0.5g prepared in example 1 is placed in the fixed bed of catalyst test apparatus, under conditions of simulated flue gas,
Carry out catalyst flue gas demercuration evaluation.Simulated flue gas is by O2、CO2、SO2、NO、HCl、N2Composition, flue gas total flow is 1L/min,
Wherein O2Content is 6%, CO2Content is 12%, SO2Concentration be 400ppm, NO concentration be 800ppm, Cl2Concentration is 50ppm, NH3
Flow is 1ml/min, and remaining is N2。100ml/min N2(as the carrier of mercuryvapour), nonvalent mercury 20 ± 1 g/m3Simulation cigarette
Gas.Temperature is 200 DEG C, air speed is 38000h-1Under conditions of, when catalyst reaches the stably catalyzed stage, above-mentioned prepared by urge
Agent is 97.78% to denitrating flue gas rate, and Elemental Mercury removal efficiency and oxygenation efficiency respectively reach 97.70% and 90.44%.
Embodiment 3: catalyst is for the decolouring case study of red base GP waste water from dyestuff
Red base GP waste water from dyestuff former state absorbance under 464nm absorbing wavelength is 2.92, and COD is 3043.04mg/L.
Take 0.5g decolorising agent to put in 50ml waste water from dyestuff, add 0.5ml hydrogen peroxide, at regulation pH to 4, in temperature 40
1h is stirred at DEG C.Absorbance reduces to 0.31, and COD reduces to 305.22mg/L.Percent of decolourization reaches 92.76%, COD clearance 93.36%.
Claims (10)
1. metal-oxide-alum salts/Attapulgite Catalyst, it is characterised in that: by metal-oxide TOxWith alum salts
RVO4Mutual load is prepared from attapulgite ATP.
Metal-oxide-alum salts/Attapulgite Catalyst the most according to claim 1, it is characterised in that: described gold
Belong to oxide TOxIn T be Ce, Zr or Mn.
Metal-oxide-alum salts/Attapulgite Catalyst the most according to claim 1, it is characterised in that: described vitriol
Hydrochlorate RVO4In R be Ce, Mn or Fe.
Metal-oxide-alum salts/Attapulgite Catalyst the most according to claim 2, it is characterised in that: described vitriol
Hydrochlorate RVO4In R be Ce, Mn or Fe.
5. the preparation method of the metal-oxide-alum salts/Attapulgite Catalyst described in claim 4, it is characterised in that: first
RVO is prepared with hydrothermal synthesis method4/ ATP, then use sol-gal process to prepare metal-oxide-alum salts/attapulgite catalysis
Agent TOx-RVO4/ATP。
The preparation method of metal-oxide-alum salts/Attapulgite Catalyst the most according to claim 5, its feature exists
In: preparation process is as follows:
(1) weigh the ammonium metavanadate of equimolar amounts and manganese nitrate or cerous nitrate or ferric nitrate, be respectively placed in two beakers addition
Suitable quantity of water is dissolved;
(2) weigh appropriate pure attapulgite ATP to add in deionized water, be simultaneously introduced a small amount of dispersant PEG400, stir
Mixing certain time makes it be uniformly dispersed;
(3) step (2) prepare ATP deionized water in be slowly added dropwise respectively ammonium metavanadate solution and cerous nitrate or manganese nitrate or
Iron nitrate solution, moves into hydrothermal reaction kettle after adding proper ammonia regulation pH=9 ~ 14 interior at 120 ~ 180 DEG C after stirring certain time
Under the conditions of react 7 ~ 12 hours;
(4) it is washed with deionized after sucking filtration, until using AgNO3Detection is without Cl-Exist;Dry at 80 DEG C, grind and obtain RVO4/
ATP, R are Ce, Mn or Fe;
(5) configure the citric acid solution of 2mol/L, weigh appropriate manganese nitrate or cerous nitrate or zirconium nitrate to join citric acid molten
In liquid, after being completely dissolved, form manganese or the precursor citric acid solution of cerium or zirconium;
(6) RVO that appropriate step (4) prepares is weighed4/ ATP joins in the precursor citric acid solution that step (5) prepares, fully
Add appropriate glacial acetic acid after stirring under the conditions of uniform temperature, stir ageing 12 ~ 16 hours;
(7) regulate pH=9 ~ 14 with ammonia, react at a certain temperature to gel;Muffle furnace is put at sky after drying 24 hours
Roasting under gas atmosphere, grinding obtain metal-oxide-alum salts/Attapulgite Catalyst TOx-RVO4/ ATP, wherein T is Ce, Zr
Or Mn;R is Ce, Mn or Fe.
The preparation method of metal-oxide-alum salts/Attapulgite Catalyst the most according to claim 6, its feature exists
In:
Described step (6): wherein add appropriate glacial acetic acid and stir ageing 12 hours under the conditions of 60 DEG C.
The preparation method of metal-oxide-alum salts/Attapulgite Catalyst the most according to claim 6, its feature exists
In: described step (7): regulate pH=8 with ammonia, react at temperature 80 DEG C to gel, dry at 80 DEG C and put for 24 hours
Enter Muffle furnace in air atmosphere at 400 DEG C roasting grind after 6 hours and obtain metal-oxide-alum salts/attapulgite catalysis
Agent TOx-RVO4/ ATP, wherein T is Ce, Zr or Mn;R is Ce, Mn or Fe.
9. metal-oxide-alum salts/the Attapulgite Catalyst of one of claim 1-4 answering in denitrating flue gas demercuration
With.
10. metal-oxide-alum salts/the Attapulgite Catalyst of one of claim 1-4 answering in decoloring dye waste water
With.
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CN110215917A (en) * | 2019-04-19 | 2019-09-10 | 北京工业大学 | A kind of support type vanadic acid metal M salt SCR catalyst and preparation method |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN107042102A (en) * | 2016-12-07 | 2017-08-15 | 盐城复华环保产业开发有限公司 | Selective catalytic reduction low-temperature denitration catalyst and preparation method thereof |
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CN108993476B (en) * | 2017-06-06 | 2022-02-08 | 国家能源投资集团有限责任公司 | Metal oxide-vanadate/TiO2Catalyst, preparation method and application thereof |
CN107252693A (en) * | 2017-07-16 | 2017-10-17 | 常州大学 | A kind of V2O5Coat MnO2‑γ‑Fe2O3/ attapulgite clay low-temperature denitration catalyst and preparation method thereof |
CN109453758A (en) * | 2018-10-31 | 2019-03-12 | 福建工程学院 | A kind of denitrating catalyst and preparation method thereof |
CN109453758B (en) * | 2018-10-31 | 2021-06-25 | 福建工程学院 | Denitration catalyst and preparation method thereof |
CN110215917A (en) * | 2019-04-19 | 2019-09-10 | 北京工业大学 | A kind of support type vanadic acid metal M salt SCR catalyst and preparation method |
CN110215917B (en) * | 2019-04-19 | 2022-09-20 | 北京工业大学 | Supported vanadium acid metal M salt SCR catalyst and preparation method thereof |
CN112076730A (en) * | 2020-09-16 | 2020-12-15 | 盐城工学院 | Dye wastewater decolorizer and preparation method and application thereof |
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