CN110124671A - A kind of Cu1-XCoXFe2O4Class fenton catalyst and its preparation method and application - Google Patents
A kind of Cu1-XCoXFe2O4Class fenton catalyst and its preparation method and application Download PDFInfo
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- CN110124671A CN110124671A CN201910305112.0A CN201910305112A CN110124671A CN 110124671 A CN110124671 A CN 110124671A CN 201910305112 A CN201910305112 A CN 201910305112A CN 110124671 A CN110124671 A CN 110124671A
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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
- B01J23/74—Iron group metals
- B01J23/75—Cobalt
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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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- 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
Abstract
The present invention relates to a kind of Cu1‑XCoXFe2O4Class fenton catalyst and its preparation method and application.The preparation method includes the following steps: surfactant will to be added after copper source, cobalt source and ferric iron source mixed dissolution, stirs, and adjusts after pH is 8.0~10.0 and stirs, and in 180~200 DEG C of hydro-thermal reactions 20~for 24 hours, washing is dry after Magnetic Isolation, grinds to obtain the final product.Preparation method simple process of the invention, material source is wide, at low cost and no pollution to the environment；The Cu being prepared1‑XCoXFe2O4Class fenton catalyst, catalytic activity are high, and applied widely, reaction condition is mild and simple and easy, the refractory organic compounds such as drug capable of being fast degraded, PPCPs.In addition, H2O2It is a kind of oxidant of green, is catalyzed H using such fenton catalyst2O2And then handling Technology of Sewage is a kind of environmentally friendly technology.
Description
Technical field
The invention belongs to water process catalysis material fields, and in particular to a kind of Cu1-XCoXFe2O4Class fenton catalyst and its
Preparation method and application.
Background technique
In recent years, drug (such as anti-inflammatory drug, antibiotic, hypolipidemic) and personal-care supplies (such as cosmetics, hair care
Product, articles for washing etc.) as a kind of emerging pollutant all over the world underground water, surface water, drinking water, tap water, ocean,
Deposit and soil is medium is detected, causes people and widely pays close attention to.Currently, every country is not yet made PPCPs sternly
The discharge standard of lattice.And it is widely used in the trend of cumulative year after year.Although concentration only has ng/L to these substances in water
~ug/L, but itself there is bioaccumulation and chronic toxicity, and there is stable structure, difficulty is degraded by microorganisms.Perhaps
Drug is easy to cause the chronic accumulation of toxicity in vivo, to interfere the normal breeding of aquatile, makes aquatic ecological
System is destroyed.Studies have shown that the methods of coagulation, precipitating, filtering and traditional sewage disposal technology are to PPCPs removal effect
It is unobvious.Therefore, the security presence of the PPCPs environmental pollution and the mankind in water potential threat.
High-level oxidation technology is to go PPCPs most efficient method in water removal at present.Class fenton catalyst technology is advanced oxygen
One of change technology, it overcomes the shortcomings that homogeneous Fenton generates iron cement and stringent pH condition, while recyclable,
Avoid secondary pollution.However that all there is catalytic activity is lower for most class fenton catalysts at present, degrades difficult to degrade organic
The slower disadvantage of substance.Therefore, it is high to develop a kind of catalytic activity, the fast novel class Fenton catalysis material of degradation speed has weight
Want meaning.
Summary of the invention
It is an object of the invention to overcome in the prior art class fenton catalyst catalytic activity it is low, degrade hardly degraded organic substance
Matter slow defect and deficiency, provide a kind of Cu1-XCoXFe2O4The preparation method of class fenton catalyst.Preparation side provided by the invention
Method simple process, material source is wide, at low cost and no pollution to the environment；The Cu being prepared1-XCoXFe2O4Class fenton catalyst
The catalytic performance of unit metal catalyst is not only remain, while there is the synergistic function between metal, catalytic activity is high,
Applied widely, reaction condition is mild and simple and easy, the refractory organic compounds such as drug capable of being fast degraded, PPCPs.
In addition, H2O2It is a kind of oxidant of green, is catalyzed H using class fenton catalyst provided by the invention2O2And then locate
Reason Technology of Sewage is a kind of environmentally friendly technology.
Another object of the present invention is to provide a kind of Cu1-XCoXFe2O4Class fenton catalyst.
Another object of the present invention is to provide above-mentioned Cu1-XCoXFe2O4Class fenton catalyst is in sewage treatment field
Using.
For achieving the above object, the present invention adopts the following technical scheme:
A kind of Cu1-XCoXFe2O4The preparation method of class fenton catalyst, includes the following steps:
Solvent will be added after copper source, cobalt source and ferric iron source mixed dissolution, stir, adjusts after pH is 8.0~10.0 and stir
It mixes, in 180~200 DEG C of hydro-thermal reactions 20~for 24 hours, washing is dry after Magnetic Isolation, grinds up to the Cu1-XCoXFe2O4Class
Fenton catalyst；Wherein 0.25≤X≤0.75.
The present invention prepares Cu using hydro-thermal method1-XCoXFe2O4Class fenton catalyst, simple process, material source is wide, at
This low and no pollution to the environment.In addition, individual CuFeO2Or CoFeO2Catalyst H2O2Effect it is relatively poor；This
Invent the Cu being prepared1-XCoXFe2O4The regulation that class fenton catalyst is matched by each metal, not only remains unit metal
The catalytic performance of catalyst, while there is the synergistic function between metal, catalytic activity is high, and it is applied widely, react item
Part is mild and simple and easy, the refractory organic compounds such as drug capable of being fast degraded, PPCPs.
In addition, H2O2It is a kind of oxidant of green, is catalyzed H using class fenton catalyst provided by the invention2O2Technology
It is a kind of environmentally friendly technology.
Copper source, cobalt source and the ferric iron source of this field routine are used equally in the present invention.
Preferably, copper source is one or more of copper nitrate, copper sulphate or copper chloride.
Preferably, the cobalt source is one or more of cobalt nitrate, cobaltous sulfate or cobalt chloride.
Preferably, the ferric iron source is one or more of ferric nitrate or iron chloride.
Preferably, the surfactant is one or more of ethylene glycol or polyethylene glycol.
Preferably, the X=0.75.
Preferably, it is 8 that pH is adjusted in the preparation method.
Preferably, pH is adjusted using ammonium hydroxide.
Preferably, the temperature of the hydro-thermal reaction is 180 DEG C, and the time is for 24 hours.
Preferably, the process of the washing is successively to wash through deionized water and dehydrated alcohol.
A kind of Cu1-XCoXFe2O4Class fenton catalyst is prepared by above-mentioned preparation method.
Preferably, the Cu1-XCoXFe2O4The partial size of class fenton catalyst is 5~20nm.
Above-mentioned Cu1-XCoXFe2O4Application of the class fenton catalyst in sewage treatment field is also in protection scope of the present invention
It is interior.
Preferably, the Cu1-XCoXFe2O4Class fenton catalyst is in the sewage of processing drug containing or personal-care supplies
Application.
Preferably, the drug is one or more of anti-inflammatory drug, antibiotic or hypolipidemic；The use in personal care
Product are one of cosmetics, treatment or articles for washing.
Antipyrine is one of typical PPCPs.
It is further preferable that the Cu1-XCoXFe2O4Application of the class fenton catalyst in sewage of the processing containing antipyrine.
Compared with prior art, the invention has the following beneficial effects:
Preparation method simple process provided by the invention, material source is wide, at low cost and no pollution to the environment；It is prepared into
The Cu arrived1-XCoXFe2O4Class fenton catalyst not only remains the catalytic performance of unit metal catalyst, at the same have metal it
Between synergistic function, catalytic activity is high, and applied widely, reaction condition is mild and simple and easy, drug capable of being fast degraded,
The refractory organic compounds such as PPCPs.
In addition, H2O2It is a kind of oxidant of green, is catalyzed H using class fenton catalyst provided by the invention2O2Technology is
A kind of environmentally friendly technology.
Detailed description of the invention
Fig. 1 is the Cu that the embodiment of the present invention 1 provides0.25Co0.75Fe2O4The scanning electron microscope (SEM) photograph of class fenton catalyst；
Fig. 2 is the Cu that the embodiment of the present invention 1 provides0.25Co0.75Fe2O4Class fenton catalyst at various ph values replaces peace
Than the removal effect figure of woods；
Fig. 3 is the Cu that the embodiment of the present invention 1 provides0.25Co0.75Fe2O4Class fenton catalyst is under different catalysts dosage
To the removal effect figure of antipyrine；
Fig. 4 is the Cu that the embodiment of the present invention 1~3 provides1-XCoXFe2O4The removal effect figure of class fenton catalyst；
The Cu that Fig. 5 embodiment of the present invention 1 provides0.25Co0.75Fe2O4Class fenton catalyst and CuFeO2And CoFeO2To peace
For the removal effect figure than woods.
Specific embodiment
Below with reference to embodiment, the present invention is further explained.These embodiments are merely to illustrate the present invention rather than limitation
The scope of the present invention.Test method without specific conditions in lower example embodiment usually according to this field normal condition or is pressed
The condition suggested according to manufacturer；Used raw material, reagent etc., unless otherwise specified, being can be from the business such as conventional market
The raw materials and reagents that approach obtains.The variation for any unsubstantiality that those skilled in the art is done on the basis of the present invention
And replacement belongs to scope of the present invention.
Embodiment 1
The present embodiment provides a kind of Cu0.25Co0.75Fe2O4Class fenton catalyst is prepared via a method which to obtain.
Weigh 8.08g ferric nitrate (Fe (NO3)3·9H2O), 2.18g cobalt nitrate (Co (NO3)2·6H2) and 0.60g nitric acid O
Copper (Cu (NO3)2·6H2O) put into beaker, be added 30mL deionized water and stir be completely dissolved after, be added 50mL ethylene glycol it is molten
Agent after magnetic stirs 30min, is added dropwise ammonium hydroxide and continues magnetic to pH value of solution=8 and stir 1h, then transfer them to polytetrafluoroethylene (PTFE)
In the hydrothermal reaction kettle of substrate, reacted for 24 hours under the conditions of 180 DEG C, after cooled to room temperature, sediment deionized water and nothing
Water-ethanol respectively washs 3 times, is dried in vacuo 12h in 60 DEG C of baking ovens after Magnetic Isolation, and finally grinding obtains
Cu0.25Co0.75Fe2O4Catalyst fines.It is scanning electron microscope (SEM) photograph such as Fig. 1, partial size is 5~20nm.
Embodiment 2
The present embodiment provides a kind of Cu0.5Co0.5Fe2O4Preparation in class fenton catalyst, preparation method and embodiment 1
Method is approximate.
The present embodiment weighs 8.08g ferric nitrate (Fe (NO3)3·9H2O), 1.45g cobalt nitrate (Co (NO3)2·
6H2) and 1.21g copper nitrate (Cu (NO O3)2·6H2O it) puts into beaker.Remaining step and condition and embodiment 1 are consistent, grain
Diameter is 5~20nm.
Embodiment 3
The present embodiment provides a kind of Cu0.75Co0.25Fe2O4System in class fenton catalyst, preparation method and embodiment 1
Preparation Method is approximate.
The present embodiment weighs 8.08g ferric nitrate (Fe (NO3)3·9H2O), 0.73g cobalt nitrate (Co (NO3)2·
6H2) and 1.81g copper nitrate (Cu (NO O3)2·6H2O it) puts into beaker.Remaining step and condition and embodiment 1 are consistent, grain
Diameter is 5~20nm.
Embodiment 4
The present embodiment provides a kind of Cu0.25Co0.75Fe2O4Class fenton catalyst is prepared via a method which to obtain.
Weigh 8.08g ferric nitrate (Fe (NO3)3·9H2O), 2.11g cobaltous sulfate (CoSO4·7H2) and 0.62 g copper sulphate O
(CuSO4·5H2O) put into beaker, be added 30mL deionized water and stir be completely dissolved after, be added 50mL polyethylene glycol surface
Activating agent after magnetic stirs 30min, is added dropwise ammonium hydroxide and continues magnetic to pH value of solution=10 and stir 1h, then transfer them to polytetrafluoro
In the hydrothermal reaction kettle of ethylene substrate, reacted for 24 hours under the conditions of 180 DEG C, after cooled to room temperature, sediment deionized water
It is respectively washed with dehydrated alcohol 3 times, is dried in vacuo 12h in 60 DEG C of baking ovens after Magnetic Isolation, finally grinding obtains
Cu0.25Co0.75Fe2O4Catalyst fines.Partial size is about 16nm.
Embodiment 5
The present embodiment provides a kind of Cu0.25Co0.75Fe2O4Class fenton catalyst is prepared via a method which to obtain.
Weigh 5.41g iron chloride (FeCl3·6H2O), 1.78g cobalt chloride (CoCl2·6H2) and 0.43g copper chloride O
(CuCl2·6H2O) put into beaker, be added 30mL deionized water and stir be completely dissolved after, be added 50mL ethylene glycol solvent, magnetic
After stirring 30min, ammonium hydroxide is added dropwise and continues magnetic to pH value of solution=9 and stirs 1h, then transfers them to polytetrafluoroethylsubstrate substrate
In hydrothermal reaction kettle, 20h is reacted under the conditions of 200 DEG C, after cooled to room temperature, sediment deionized water and dehydrated alcohol
Each washing 3 times, dries 12h after Magnetic Isolation in 60 DEG C of baking ovens, and finally grinding obtains Cu0.25Co0.75Fe2O4Catalyst powder
End.Partial size is about 20 nm.
The Cu being prepared with Examples 1 to 31-XCoXFe2O4Class fenton catalyst and refractory organic compounds antipyrine
For measure the performance of its catalytic degradation refractory organic compounds.
(1) Cu that embodiment 1 provides0.25Co0.75Fe2O4Class fenton catalyst at various ph values removes antipyrine
Except effect
In the antipyrine solution that 50mL concentration is 50mg/L, in the waste water of pH 3.0,5.0,7.0,8.0 and 9.0
It is separately added into 0.5g/L Cu1-XCoXFe2O4Class fenton catalyst and 50mmol H2O2, 60min is reacted at room temperature, is degraded
Rate such as Fig. 2.As can be seen from Figure 2, under the conditions of pH is 7.0, degradation rate highest, up to 100%；Respectively higher than pH=3.0
(46.90%), pH=5.0 (89.67%), pH=8.0 (98.60%) and pH=9.0 (85.88%).As it can be seen that CuxCo1- xFe2O4Catalyst is to have higher catalytic activity in 5~9 range in pH value；Illustrate its with wider pH range, and
In neutral conditions, catalytic performance is best.
(2) Cu that embodiment 1 provides0.25Co0.75Fe2O4Class fenton catalyst under different catalysts dosage to peace for than
The removal effect of woods
In the antipyrine solution that 50mL concentration is 50mg/L, be separately added into 0 in the waste water that pH is 7.0,0.1,0.3,
0.5,0.7 and 1.0g/L Cu1-XCoXFe2O4Class fenton catalyst and 50mmol H2O2, 60min is reacted at room temperature, is dropped
Solution rate such as Fig. 3.As can be seen from Figure 3, when catalyst amounts are 0g/L, catalyst is insufficient to the suction-operated of antipyrine
1%, it can be neglected.With the increase of catalyst amounts, the degradation rate of antipyrine is also continuously improved.When catalyst adds
When amount is 0.5g/L, reaction 60min antipyrine is substantially degradable；Continue the amount of increase catalyst, the removal rate base of ANT
This is identical, or even is declined.Therefore, optimal dosage is 0.5g/L.
(3) Cu that Examples 1 to 3 provides1-XCoXFe2O4The lower removal effect to antipyrine of class fenton catalyst
In the antipyrine solution that 50mL concentration is 50mg/L, 0.5g/L implementation is separately added into the waste water that pH is 7.0
The Cu that example 1~3 provides1-XCoXFe2O4Class fenton catalyst and 50mmol H2O2, 60min, degradation rate are reacted at room temperature
Such as Fig. 4, the Cu under different ratio is known from figure1-XCoXFe2O4Catalyst shows higher catalytic performance.Wherein
Cu0.25Co0.75Fe2O4Removal rate be 97.27%, respectively higher than Cu0.5Co0.5Fe2O4(89.17%) and Cu0.75Co0.25Fe2O4
(69.86%).When Co content increases, the catalytic activity of catalyst also has significantly improved.As Co:Cu=3:1, it is catalyzed
H2O2To the removal rate highest of ANT.Illustrate that the content of Cu and Co have a certain impact to catalyst.
(4) Cu that embodiment 1 provides0.25Co0.75Fe2O4Class fenton catalyst and CuFeO2And CoFeO2To antipyrine
Removal effect.
In the antipyrine solution that 50mL concentration is 50mg/L, 0.5g/L implementation is separately added into the waste water that pH is 7.0
The Cu that example 1 provides0.25Co0.75Fe2O4Class fenton catalyst and 50mmol H2O2、0.5g/L CuFeO2Catalyst and 50mmol
H2O2、0.5g/L CoFeO2Catalyst and 50mmol H2O260min, degradation rate such as Fig. 5, Cong Tuke are reacted at room temperature
Know, under identical conditions, the Cu of the offer of embodiment 10.25Co0.75Fe2O4Class fenton catalyst is to the removal rate of antipyrine
95.21%, hence it is evident that be higher than CoFeO2(31.02%) and CuFeO2(44.86%).It can be seen that the Cu of synthesis0.25Co0.75Fe2O4Class is fragrant
Pause catalyst catalytic performance with higher, while also illustrating that the multi-metallic catalyst for adulterating Cu and Co has synergistic effect,
Higher activity is shown than monometallic catalyst during class Fenton.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of Cu1-XCoXFe2O4The preparation method of class fenton catalyst, which comprises the steps of:
Surfactant will be added after copper source, cobalt source and ferric iron source mixed dissolution, stir, adjusts after pH is 8.0~10.0 and stir
It mixes, in 180~200 DEG C of hydro-thermal reactions 20~for 24 hours, washing is dry after Magnetic Isolation, grinds up to the Cu1-XCoXFe2O4Class
Fenton catalyst；Wherein 0.25≤X≤0.75.
2. preparation method according to claim 1, which is characterized in that copper source is in copper nitrate, copper sulphate or copper chloride
One or more；The cobalt source is one or more of cobalt nitrate, cobaltous sulfate or cobalt chloride；The ferric iron source is nitric acid
One or more of iron or iron chloride；The surfactant is one or more of ethylene glycol or polyethylene glycol.
3. preparation method according to claim 1, which is characterized in that the X=0.75.
4. preparation method according to claim 1, which is characterized in that adjusting pH in the preparation method is 8.
5. preparation method according to claim 1, which is characterized in that the temperature of the hydro-thermal reaction is 180 DEG C, and the time is
24h。
6. preparation method according to claim 1, which is characterized in that the process of the washing is successively through deionized water and nothing
Water-ethanol washing.
7. a kind of Cu1-XCoXFe2O4Class fenton catalyst, which is characterized in that pass through any preparation method of claim 1~6
It is prepared.
8. Cu according to claim 71-XCoXFe2O4Class fenton catalyst, which is characterized in that the Cu1-XCoXFe2O4Class is fragrant
The partial size of catalyst is 5~20nm.
9. any Cu of claim 7~81-XCoXFe2O4Application of the class fenton catalyst in sewage treatment field.
10. applying according to claim 9, which is characterized in that the Cu1-XCoXFe2O4Class fenton catalyst is in processing drug containing
Application in the sewage of object or personal-care supplies.
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| CN110947395A (en) * | 2019-12-03 | 2020-04-03 | 中化环境控股有限公司 | Preparation method of Fenton-like catalytic material and sewage treatment method |
| CN111495369A (en) * | 2020-04-30 | 2020-08-07 | 中山大学 | Carbon felt loaded CuCo-BH Fenton catalyst and preparation method and application thereof |
| CN113332988A (en) * | 2021-05-31 | 2021-09-03 | 东北电力大学 | Porous magnetic conductive copper-self-doped copper-zinc ferrite catalyst and preparation method and application thereof |
| CN115282966A (en) * | 2022-07-21 | 2022-11-04 | 河北科技师范学院 | Ferrous ion doped copper cobaltate material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111495369A (en) * | 2020-04-30 | 2020-08-07 | 中山大学 | Carbon felt loaded CuCo-BH Fenton catalyst and preparation method and application thereof |
| CN111495369B (en) * | 2020-04-30 | 2021-07-27 | 中山大学 | Carbon felt loaded CuCo-BH Fenton catalyst and preparation method and application thereof |
| CN113332988A (en) * | 2021-05-31 | 2021-09-03 | 东北电力大学 | Porous magnetic conductive copper-self-doped copper-zinc ferrite catalyst and preparation method and application thereof |
| CN113332988B (en) * | 2021-05-31 | 2022-08-23 | 东北电力大学 | Porous magnetic conductive copper-self-doped copper-zinc ferrite catalyst and preparation method and application thereof |
| CN115282966A (en) * | 2022-07-21 | 2022-11-04 | 河北科技师范学院 | Ferrous ion doped copper cobaltate material and preparation method thereof |
| CN115282966B (en) * | 2022-07-21 | 2024-01-30 | 河北科技师范学院 | Ferrous ion doped copper cobaltate material and preparation method thereof |
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Application publication date: 20190816 |