CN108144622A - A kind of Fenton catalysis material and its preparation method and application - Google Patents
A kind of Fenton catalysis material and its preparation method and application Download PDFInfo
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- CN108144622A CN108144622A CN201711382999.0A CN201711382999A CN108144622A CN 108144622 A CN108144622 A CN 108144622A CN 201711382999 A CN201711382999 A CN 201711382999A CN 108144622 A CN108144622 A CN 108144622A
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- catalysis material
- cerium oxide
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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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- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/023—Reactive oxygen species, singlet oxygen, OH radical
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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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
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Abstract
The present invention relates to pollution waters restoration technical field, particularly a kind of Fenton catalysis material, the catalysis material is Fe2O3 doping cerium oxide.The purpose of the present invention is to provide a kind of Fenton catalysis material, while the method that also offer prepares Fe2O3 doping cerium oxide type Fenton catalysis material, to overcome general heterogeneous class Fenton catalysis material activity low, the problem of rate of catalysis reaction is slower.The cost of material relative moderate that the method uses, reaction condition is mild, can carry out under normal pressure, without using surfactant and other organic solvents, reduces manufacturing cost, and reduce the pollution generated in preparation process.
Description
Technical field
The present invention relates to pollution waters restoration technical field, particularly a kind of Fenton catalysis material and preparation method thereof and should
With.
Background technology
Pollution of chromium is essentially from the industrial wastewaters such as chrome ore and metal smelt, plating, process hides, exhaust gas and waste residue.Chromium is human body
One of necessary trace element, but excessive chromium is to human health;The toxicity of Cr VI is stronger, is more absorbed by the body,
There is carcinogenesis, and can accumulate in vivo.Due to chromium extensive use in the industrial production, the amount of Cr VI gradually increases in environment
It is more, potential hazard and threat can be caused to human body and animal body, therefore, develop and optimize pollution of chromium repair materials, it is dirty to administer chromium
Contaminating water body becomes one of urgent problem to be solved in current water pollution.At present, domestic and international common chrome waste water processing method has
Bioanalysis, electrolytic reduction etc..Nano zero valence iron, can be by Cr ((VI) also as a kind of emerging environment pollution treatment material
Originally be Cr (III), and be co-precipitated with Fe (III), generate (CrxFe1-x) (OH) 3 grade products, finally with precipitation form by its
Thoroughly removal.
The synthetic method of traditional nano zero valence iron mainly has Physical and chemical method etc..Physical refers to through physics side
Method prepares iron particle to nanoscale, including vaporization condensation process, freeze-drying etc.;Chemical method refers to using sodium borohydride etc. also
Iron ion is restored generation nano zero valence iron by former agent, common to have liquid phase reduction, microemulsion method etc..But these traditional conjunctions
It is higher into method cost, it needs to consume more energy, technics comparing is complicated, generates secondary pollution problems and hinders nanometer zero
The industrialized utilization of valency iron.
In recent years, the green synthesis method that nano zero valence iron is prepared using reducing plant extract ferric ion is caused
The extensive concern of people it is relatively common at present be to synthesize nano zero valence iron using the extracting solutions such as tealeaves, pomelo peel, and tealeaves etc.
Industrial crops cost is higher, is not suitable for large-scale production.Tuber fern is distributed widely in subtropical and tropical zones, and growth is vigorous, and one
Year can multi-harvest, planting cost is low, be conducive to carry out industrialization production.
In view of the seriousness of China's water body pollution of chromium, there is an urgent need for develop a kind of economic, efficiently, practical Treatment process to repair
Chromium pollution water.
Invention content
The purpose of the present invention is to provide a kind of Fenton catalysis material, while also offer prepares Fe2O3 doping cerium oxide type Fenton
The method of catalysis material, to overcome general heterogeneous class Fenton catalysis material activity low, the problem of rate of catalysis reaction is slower.This
The cost of material relative moderate that method uses, reaction condition is mild, can carry out under normal pressure, without using surfactant and its
His organic solvent, reduces manufacturing cost, and reduce the pollution generated in preparation process.
The present invention specific technical solution be:A kind of Fenton catalysis material, the catalysis material are aoxidized for Fe2O3 doping
Cerium material.
In above-mentioned Fenton catalysis material, in the Fe2O3 doping cerium oxide ferro element for ferrous ion or iron from
Son.
In above-mentioned Fenton catalysis material, ferro element and cerium molar ratio are in the Fe2O3 doping cerium oxide:1:
10-1:0.5。
Meanwhile the invention also discloses a kind of Fe2O3 doping cerium oxide type Fenton catalysis material preparation method, including walking as follows
Suddenly:
Step 1:Presoma is prepared using dissolvable ferrous iron/molysite and cerium salt;
Step 2:Presoma is calcined to obtain Fe2O3 doping cerium oxide type Fenton catalysis material.
In above-mentioned Fe2O3 doping cerium oxide type Fenton catalysis material preparation method, the specific side of presoma preparation
Method is:
Dissolvable ferrous iron/molysite and cerium salt are dispersed in water by a certain percentage, 45 DEG C of constant temperature stir evenly;It adds in appropriate
Precipitating reagent, regulation system pH continues to stir;Temperature remains unchanged, and carries out still aging overnight;Separation of solid and liquid is carried out later,
The solid precipitation of acquisition is cleaned, is dry, obtains presoma.
In above-mentioned Fe2O3 doping cerium oxide type Fenton catalysis material preparation method, in the step 1, ferrous iron/molysite, cerium
Salt molar ratio is 1:10-1:0.5, metal ion total ion concentration is 0.01-0.25mol/L.
In above-mentioned Fe2O3 doping cerium oxide type Fenton catalysis material preparation method, precipitating reagent is sodium hydroxide, hydroxide
Potassium, ammonium hydroxide, sodium carbonate, ammonium carbonate or its mixture add system pH ranging from 7.0-12.0 after precipitating reagent.
In above-mentioned Fe2O3 doping cerium oxide type Fenton catalysis material preparation method, in step 2, calcination temperature for 300 DEG C-
800 DEG C, calcination time 1-6h.
It is described meanwhile the present invention also provides a kind of purposes of Fe2O3 doping cerium oxide type Fenton catalysis material as described above
Catalysis material for organic polluting water processing.
Compared with prior art, the beneficial effects of the present invention are:
(1) the cost of material relative moderate that the present invention uses, reaction condition is mild, can carry out under normal pressure, without using
Surfactant and other organic solvents, reduce manufacturing cost, and reduce the pollution generated in preparation process.
(2) FeCeOx material characters prepared by the present invention are stablized, and structure destruction is not susceptible in reaction process, and reaction terminates
Separation of solid and liquid is easily carried out afterwards.
(3) FeCeOx materials catalytic activity prepared by the present invention is high, the organic contamination that can be catalyzed in Fenton's reaction degradation water
Object rate is fast, and can work in wider pH ranges.
Cerium is one of rare earth element that reserves are most rich in nature, and oxide is due to huge specific surface area, enriching
Lacking oxygen and relatively low Ce3+/Ce4+ oxidation-reduction potentials, and frequently as catalyst for waste gas purification and organic synthesis
Research and application.The characteristics of ferro element is made composite catalyst, fully combines iron and cerium respectively is introduced in cerium oxide, is improved
The activity of catalyst and the removal efficiency to organic contamination are expected to accelerate promoting the use for heterogeneous class Fenton technology.
Therefore the present invention utilizes cheap raw material, and it is fragrant to prepare Fe2O3 doping cerium oxide catalysis class using coprecipitation
Pause reaction degradation organic pollutants.
Description of the drawings
Fig. 1 is the SEM image of material FeCeOx prepared by embodiment 1;
Fig. 2 is the TEM image of material FeCeOx prepared by embodiment 1;
Fig. 3 is the XPS images of material FeCeOx prepared by embodiment 1;
Fig. 4 is the influence relational graph that material FeCeOx dosages remove organic dyestuff;
Fig. 5 is the influence relational graph that material H2O2 dosages remove organic dyestuff;
Fig. 6 is the influence relational graph that the initial pH of reaction system removes organic dyestuff.
Fig. 7 is the influence relational graph that different Fe2O3 doping amount material FeCeOx remove organic dyestuff;
Specific embodiment
With reference to embodiment, technical scheme of the present invention is described in further detail, but do not formed pair
Any restrictions of the present invention.
Embodiment 1
The preparation method of material FeCeOx belongs to coprecipitation, includes the following steps:
1) prepared by presoma:Dissolvable ferrous salt, cerium salt are pressed 1:2 molar ratio is dispersed in 100ml water, total metal from
A concentration of 0.1mol/l of son, under the conditions of 40 DEG C of waters bath with thermostatic control, stirs evenly;Suitable concentrated ammonia liquor is added in, regulation system pH is 9.3
~9.5, continue to stir 2h;Temperature remains unchanged, still aging 12h;Separation of solid and liquid is carried out later, and the solid of acquisition is precipitated and is used
Deionization is washed 3 times, is placed in 105 DEG C of dry 10h in baking oven, obtains presoma.
(2) it calcines:The presoma of acquisition is placed in Muffle furnace, 500 DEG C of calcining 3h, natural cooling in air atmosphere
Afterwards, Fe2O3 doping cerium oxide type Fenton catalysis material FeCeOx is obtained.
Fig. 1 and Fig. 2 is the scanning electron microscope and transmission electron microscope results of material FeCeOx, and as a result display material is in granular form, grain
Diameter is in 10nm or so, it may be possible to occur a degree of reunion by magnetic force and van der Waals interaction.Particle surface is uneven,
Illustrate that material is stronger with larger specific surface area and more reactivity point position, catalytic capability.Fig. 3 is FeCeOx composite materials
XPS figure.From figure 3, it can be seen that Fe (II), Fe (III), Ce (III) and Ce (IV) coexist in catalysis material surface, this has
Hydroxyl radical free radical is generated conducive to catalysis hydrogen peroxide.
Embodiment 2
The preparation method of material FeCeOx belongs to coprecipitation, includes the following steps:
1) prepared by presoma:Dissolvable ferrous salt, cerium salt are pressed 1 respectively:0.5、1:1、1:2 and 1:3 molar ratio dispersion
In 100ml water, total concentration of metal ions is 0.1mol/l, under the conditions of 40 DEG C of waters bath with thermostatic control, is stirred evenly;It adds in suitable dense
Ammonium hydroxide, regulation system pH are 9.3~9.5, continue to stir 2h;Temperature remains unchanged, still aging 12h;Solid-liquid point is carried out later
From the solid of acquisition precipitation is washed with deionized water 3 times, is placed in 105 DEG C of dry 10h in baking oven, acquisition presoma.
(2) it calcines:The presoma of acquisition is placed in Muffle furnace, 500 DEG C of calcining 3h, natural cooling in air atmosphere
Afterwards, 4 kinds of different Fe2O3 doping cerium oxide type Fenton catalysis material FeCeOx are obtained.
Embodiment 3
The influence that material FeCeOx dosages remove organic dyestuff rhodamine B (RhB), includes the following steps:
1) according to material preparation method described in embodiment 1, material FeCeOx is prepared;
2) the material FeCeOx inputs of different quality are weighed respectively equipped with 100ml 100mg/l RhB solution (pH=5.0)
Conical flask in, the dosage for controlling material FeCeOx respectively is 0.5g/L, 1.0g/L, 1.5g/L and 2.0g/L, is separately added into
80mM hydrogen peroxide.
3) by mixed liquor at a temperature of 35 ± 1 DEG C with the speed of 250r/min under reacted in shaking table.In the time of setting
Point sampling analysis.
Fig. 4 is the influence relational graph that material FeCeOx dosages remove organic dyestuff rhodamine B (RhB).Fig. 4 it is found that
Catalyst amounts increase to 1.5g/L from 0.5g/L, and 2h dyestuffs degradation rate increases to 90% from about 40%, and 1.5g/L is added
Amount differs less than 5% with 2.0g/L effects.This is because oxidation reaction occurs mainly in catalysis material surface, increase with dosage
Add, the reactivity site in system is with increase so that reaction rate is promoted.When active site is close to saturation, continue to increase
The influence that catalyst amounts are brought is added to lessen.According to efficiency and cost principle of mutual, determine that 1.5g/L FeCeOx are catalyzed
Material is the optimum dosage that initial concentration is 100mg/L RhB solution of degrading.
Embodiment 4
The influence that H2O2 dosages remove organic dyestuff rhodamine B (RhB), includes the following steps:
1) according to material preparation method described in embodiment 1, material FeCeOx is prepared;
2) cone of the 1.5g/L materials FeCeOx inputs equipped with 100ml 100mg/l RhB solution (pH=5.0) is weighed respectively
In shape bottle, the dosage for controlling H2O2 respectively is 40mM, 60mM, 80mM and 100mM.
3) by mixed liquor at a temperature of 35 ± 1 DEG C with the speed of 250r/min under reacted in shaking table.In the time of setting
Point sampling analysis.
Fig. 5 is the influence relational graph that H2O2 dosages remove organic dyestuff rhodamine B (RhB).Fig. 5 is it is found that with dioxygen
The increase of water dosage, removal rate is also with promotion, but hydrogen peroxide is added after reaching a certain amount of, and dosage continues increase pair
The influence of reaction rate is little.This is because after hydrogen peroxide dosage increase, the hydrogen peroxide of catalysis material adsorption also increases,
So as to generate more active oxygen radical attack organic pollutions.But after hydrogen peroxide reaches a certain amount of, reaction tends towards stability, reaction
Rate is no longer promoted, thus hydrogen peroxide optimum dosage is 80mM.
Embodiment 5
Influence of the initial pH value to material FeCeOx catalysis class Fenton organics removals, includes the following steps:
1) according to material preparation method described in embodiment 1, material FeCeOx is prepared;
2) in the conical flask for measuring 100ml 100mg/l RhB solution, the pH for adjusting solution is 3.0,5.0,7.0 and 9.0,
1.5g/L material FeCeOx and 80mM H2O2 are added respectively.
3) by mixed liquor at a temperature of 35 ± 1 DEG C with the speed of 250r/min under reacted in shaking table.In the time of setting
Point sampling analysis.
Fig. 6 is influence figure of the initial pH value to FeCeOx catalysis class Fenton organics removals, and pH value is in 3.0,5.0,7.0 and
9.0 are changed from acid medium to alkaline medium, and the final removal rates of RhB are not much different, and can reach nearly 98%, but reaction rate is in
Now slightly downward trend.It is similar research shows that acid medium can promote catalyst surface iron ion to dissolve out, so as to make it is homogeneous and
Heterogeneous catalysis is coexisted in reaction system, and acid condition is conducive to the stronger hydroxyl radical free radical of oxidisability and generates, so as to have
Higher reaction rate.
Embodiment 6
The influence of different Fe2O3 doping amount FeCeOx catalysis class Fenton organics removals, includes the following steps:
1) according to embodiment 2 described in material preparation method, prepare material FeCeOx;
2) in the conical flask for measuring 100ml 100mg/l RhB solution, the pH for adjusting solution is 5.0, adds 1.5g/ respectively
L difference Fe2O3 doping amount material FeCeOx and 80mM H2O2.
3) by mixed liquor at a temperature of 35 ± 1 DEG C with the speed of 250r/min under reacted in shaking table.In the time of setting
Point sampling analysis.
Fig. 7 is doping to the influence figure of FeCeOx catalysis class Fenton organics removals, 4 kinds of different Fe2O3 doping amounts
FeCeOx can effectively be catalyzed class Fenton degradation RhB, but removal rate is slightly different, with the increase of cerium molar ratio in material,
Decolorization rate is first improved and is reduced afterwards, and the best material iron cerium molar ratio of effect is 1:2.
Above-described is only presently preferred embodiments of the present invention, all timess made in the range of the spirit and principles in the present invention
What modifications, equivalent substitutions and improvements etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of Fenton catalysis material, which is characterized in that the catalysis material is Fe2O3 doping cerium oxide.
2. Fenton catalysis material according to claim 1, which is characterized in that iron member in the Fe2O3 doping cerium oxide
Element is ferrous ion or iron ion.
3. Fenton catalysis material according to claim 1, which is characterized in that iron member in the Fe2O3 doping cerium oxide
Element and cerium molar ratio are:1:10-1:0.5.
4. a kind of Fe2O3 doping cerium oxide type Fenton catalysis material preparation method, which is characterized in that include the following steps:
Step 1:Presoma is prepared using dissolvable ferrous iron/molysite and cerium salt;
Step 2:Presoma is calcined to obtain Fe2O3 doping cerium oxide type Fenton catalysis material.
5. Fe2O3 doping cerium oxide type Fenton catalysis material preparation method according to claim 4, which is characterized in that described
Presoma prepare specific method be:
Dissolvable ferrous iron/molysite and cerium salt are dispersed in water by a certain percentage, constant temperature stirs evenly;Add in suitable precipitation
Agent, regulation system pH continue to stir;Temperature remains unchanged, and carries out still aging;Separation of solid and liquid is carried out later, by consolidating for acquisition
Body precipitation is cleaned, is dry, obtains presoma.
6. Fe2O3 doping cerium oxide type Fenton catalysis material preparation method according to claim 4 or 5, which is characterized in that institute
It states in step 1, ferrous iron/molysite, cerium salt molar ratio are 1:10-1:0.5, metal ion total ion concentration is 0.01-0.25mol/
L。
7. Fe2O3 doping cerium oxide type Fenton catalysis material preparation method according to claim 5, which is characterized in that reaction temperature
Spend is 30 DEG C -60 DEG C.
8. Fe2O3 doping cerium oxide type Fenton catalysis material preparation method according to claim 5, which is characterized in that precipitating reagent
For sodium hydroxide, potassium hydroxide, ammonium hydroxide, sodium carbonate, ammonium carbonate or its mixture, add system pH ranging from 7.0- after precipitating reagent
12.0。
9. Fe2O3 doping cerium oxide type Fenton catalysis material preparation method according to claim 4, which is characterized in that step 2
In, calcination temperature is 300 DEG C -800 DEG C, calcination time 1-6h.
10. a kind of purposes of Fe2O3 doping cerium oxide type Fenton catalysis material as described in claim 4-9 is any, feature exist
In the catalysis material is for organic polluting water processing.
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Cited By (5)
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CN110841649A (en) * | 2019-10-17 | 2020-02-28 | 华南师范大学 | Preparation method of copper-cerium bimetal Fenton catalytic material, prepared catalytic material and application thereof |
CN112337472A (en) * | 2020-11-27 | 2021-02-09 | 湖南湘牛环保实业有限公司 | Catalyst for removing COD (chemical oxygen demand) in wastewater by Fenton oxidation method, preparation method and application |
CN112705027A (en) * | 2020-12-10 | 2021-04-27 | 杭州电子科技大学 | Heterogeneous Fenton reaction denitration device and method based on atomization and cooling |
CN112774683A (en) * | 2020-12-31 | 2021-05-11 | 中国环境科学研究院 | Carbon-based coated Ac-Fe/Co catalyst and microemulsion preparation method and application |
CN113058602A (en) * | 2021-04-08 | 2021-07-02 | 南京大学 | Method for regulating and controlling selective generation of oxidation active substances of iron-based Fenton catalyst |
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Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110841649A (en) * | 2019-10-17 | 2020-02-28 | 华南师范大学 | Preparation method of copper-cerium bimetal Fenton catalytic material, prepared catalytic material and application thereof |
CN112337472A (en) * | 2020-11-27 | 2021-02-09 | 湖南湘牛环保实业有限公司 | Catalyst for removing COD (chemical oxygen demand) in wastewater by Fenton oxidation method, preparation method and application |
CN112337472B (en) * | 2020-11-27 | 2023-08-11 | 湖南湘牛环保实业有限公司 | Catalyst for removing COD in wastewater by Fenton oxidation method, preparation method and application |
CN112705027A (en) * | 2020-12-10 | 2021-04-27 | 杭州电子科技大学 | Heterogeneous Fenton reaction denitration device and method based on atomization and cooling |
CN112705027B (en) * | 2020-12-10 | 2023-03-14 | 杭州电子科技大学 | Heterogeneous Fenton reaction denitration device and method based on atomization and cooling |
CN112774683A (en) * | 2020-12-31 | 2021-05-11 | 中国环境科学研究院 | Carbon-based coated Ac-Fe/Co catalyst and microemulsion preparation method and application |
CN112774683B (en) * | 2020-12-31 | 2022-05-24 | 中国环境科学研究院 | Carbon-based coated Ac-Fe/Co catalyst, and microemulsion preparation method and application thereof |
CN113058602A (en) * | 2021-04-08 | 2021-07-02 | 南京大学 | Method for regulating and controlling selective generation of oxidation active substances of iron-based Fenton catalyst |
CN113058602B (en) * | 2021-04-08 | 2022-03-18 | 南京大学 | Method for regulating and controlling selective generation of oxidation active substances of iron-based Fenton catalyst |
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