CN109205756A - A kind of nanometer thin sheet CuCo2O4/ CuO class Fenton method for treating water - Google Patents
A kind of nanometer thin sheet CuCo2O4/ CuO class Fenton method for treating water Download PDFInfo
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- CN109205756A CN109205756A CN201811209133.4A CN201811209133A CN109205756A CN 109205756 A CN109205756 A CN 109205756A CN 201811209133 A CN201811209133 A CN 201811209133A CN 109205756 A CN109205756 A CN 109205756A
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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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- 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
-
- 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
-
- 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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- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Materials Engineering (AREA)
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Abstract
The present invention provides a kind of nanometer thin sheet CuCo2O4/ CuO class Fenton method for treating water, belongs to environment functional material and water-treatment technology field.Using cetyl trimethylammonium bromide or polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, the nitrate of metal, urea as raw material, the nanometer thin sheet CuCo with flourishing cellular structure is prepared by hydro-thermal method2O4/CuO.CuCo prepared by the present invention2O4/ CuO is used for class Fenton's reaction, has good removal effect to persistent organic pollutants in wider pH range (3-10).Meanwhile CuCo during the reaction2O4The active component dissolution of/CuO is far below same type catalyst.
Description
Technical field
The invention belongs to environment functional materials and water-treatment technology field, and in particular to a kind of nanometer thin sheet CuCo2O4/
CuO class Fenton method for treating water.
Background technique
High-level oxidation technology based on potentiometric titrations is with oxidability is strong, mineralization degree is high, oxidant itself is steady
The advantages that qualitative good, therefore receive more and more attention.Key using persulfate high-level oxidation technology is to find efficiently
The method for activating persulfate.Heterogeneous catalysis activation method because solid catalyst is easy to be separated from the water recycling, operation and
Low Meteorological is considered as optimal activation method.However, the biography of solid catalyst and Organic Pollutants In Water, oxidant
Matter resistance is larger；The not high dissolution for causing active component of catalyst stability, brings secondary pollution and reduction catalyst uses the longevity
Life.The presence of these problems limits application of the heterogeneous class Fenton technology in practical water process.Therefore, exploitation is efficient, steady
Fixed catalyst is the hot spot of current heterogeneous class Fenton area research.
The present invention in view of the above problems, proposes a kind of nanometer thin sheet CuCo2O4/ CuO class Fenton water process side
Method.Currently, the patent and document that copper cobalt metal oxide is applied in Fenton-like are less.Existing related patents are as follows:
It is mesoporous that patent CN105772052A provides α-surface copper-graphite nitrogen carbide complex compound modification copper cobalt codope
Alumina solid (g-C3N4/CuCo-γ-Al2O3) fenton catalyst preparation, and be applied to Fenton-like.The catalysis
Agent has good place to go effect to Some Organic Pollutants under neutral and solutions of weak acidity, but preparation process complexity is cumbersome,
And the dissolution of copper and cobalt is higher, respectively 0.5mg/L and 0.2mg/L.
Patent CN106630103A prepares CuCo using chemical precipitation method2O4, it is used for activation potassium peroxydisulfate degradation benzene
Phenol.However, the CuCo of this method preparation2O4Alkaline condition (pH=11) catalytic activity much stronger than condition of neutral pH.
The CuCo prepared in the present invention2O4/ CuO is capable of providing by having the nanometer thin sheet of flourishing cellular structure to be assembled into
More active sites accelerate interfacial reaction rate；There is very strong catalytic activity in wider pH range (3-10)；Have in removal
With good stability during machine pollutant, the dissolution of catalyst activity component is extremely low, well below pertinent literature and specially
The report of benefit.Therefore, it is based on nanometer thin sheet CuCo2O4The class Fenton technology of/CuO has good application in practical water process
Prospect.
Summary of the invention
Nanometer thin sheet CuCo provided by the invention2O4The preparation method of/CuO, includes the following steps:
(1) surfactant is dissolved in distilled water, is then separately added into Gerhardite, six hydration nitre in the solution
Sour cobalt and urea, stir to dissolve；
(2) aqueous solution in step (1) is transferred in the autoclave with polytetrafluoroethylliner liner, is put after sealing
Enter to be heated to 110-130 DEG C in electric drying oven with forced convection, and keep the temperature 10-14h under the conditions of the temperature, to cool down after reaction
To room temperature；
(3) mixture for obtaining step (2) is washed out, dries by filtering separation；
(4) the russet powder for obtaining step (3) 500-600 DEG C of calcining in Muffle furnace, 1-5 DEG C of heating rate/
Min keeps the temperature 3-4h, to be cooled to after room temperature, obtains nanometer thin sheet CuCo2O4/CuO。
The surfactant being added in step (1) is cetyl trimethylammonium bromide, polyethylene oxide-polycyclic oxygen third
One of alkane-polyethylene oxide triblock copolymer, additional amount 0-1.0g；The Gerhardite of addition, six hydrations
The molar ratio of cobalt nitrate is 1:2；The total mol concentration of metal salt is 0.043-0.108mol/L；The mole that urea is added is gold
Belong to 1.6-2 times of salt mole sum.
The nanometer thin sheet CuCo of above method preparation2O4/ CuO, specific surface area 14.6-42.3m2/ g, pore volume are
0.268-0.635m3/ g, CuCo2O4Content with CuO is respectively 62.4%-73.5% and 26.5%-37.6%.
The nanometer thin sheet CuCo of above method preparation2O4Application of/the CuO in class Fenton water treatment technology, technique ginseng
Number are as follows:
(1) the pH range of pending water is 3.0-10.0；
(2) copper-cobalt/cobalt oxide dosage is 20.0-150.0mg/L；
(3) dosage of peroxide is 0.16-0.97mmol/L；
(4) reaction time is 15-60min.
The nanometer thin sheet CuCo of above method preparation2O4Application method of/the CuO in class Fenton water treatment technology: city
City's sanitary sewage or industrial wastewater are after grid-setting pot-primary sedimentation tank-biochemistry pool-secondary settling tank processing, using being filled with
CuCo2O4The filter tank of/CuO filler carries out advanced treating, is then discharged；It, can be in direction of groundwater flow when being used for groundwater remediation
Direction on place a Filter column, by CuCo2O4/ CuO powder fills in Filter column, injects peroxide agent by injection well,
After underground water passes through Filter column, it will be able to be purified.
The CuCo of above method preparation is observed by scanning electron microscope2O4/ CuO (attached drawing 2), it can be seen that
CuCo2O4For/CuO by having the nanometer thin sheet of flourishing cellular structure to be assembled into, this makes catalyst be capable of providing more activity
Site, to accelerate interfacial reaction rate.CuCo prepared by the above method2O4/ CuO is used under the conditions of different solutions pH degrade
2- hydroxyl-4-methoxybenzophenone-5-sulfonic acid (attached drawing 6) finds CuCo2O4/ CuO has very at wider pH range (3-10)
Strong catalytic activity.In addition, the CuCo of above method preparation2O4/ CuO has good steady during removing removal organic polluter
Qualitative, the dissolution of catalyst activity component is extremely low (attached drawing 4), well below the report of pertinent literature and patent.
Detailed description of the invention
Fig. 1 is the CuCo synthesized in embodiment 1,2,32O4The X ray diffracting spectrum of/CuO.
Fig. 2 is the CuCo synthesized in embodiment 22O4The scanning electron microscope diagram of/CuO.
Fig. 3 is the CuCo that embodiment 1,2,3 synthesizes in pure aquatic system2O4/ CuO activates peroxy-monosulfate degradation 2- hydroxyl -4-
Methoxyl group -5- sulfonic acid benzophenone efficiency figure.
Fig. 4 is the CuCo that embodiment 1,2,3 synthesizes in pure aquatic system2O4/ CuO activates peroxy-monosulfate degradation 2- hydroxyl -4-
The dissolution of copper and cobalt in methoxyl group -5- sulfonic acid benzophenone reaction process.
Fig. 5 is 2- hydroxyl-4-methoxybenzophenone-5-sulfonic acid degradation efficiency figure in embodiment 5.
Fig. 6 is the CuCo that embodiment 2 synthesizes2O4/ CuO degrades 2- hydroxyl -4- methoxyl group -5- under the conditions of different solutions pH
Sulfonic acid benzophenone efficiency figure.
Specific embodiment
The present invention will be further described in conjunction with specific embodiments, but the present invention is not limited only to these embodiments.
Embodiment 1
It weighs 0.2416g Gerhardite, 0.5821g cabaltous nitrate hexahydrate and 0.3604g urea and is dissolved in 70.0mL steaming
In distilled water, magnetic agitation is made it dissolve.Above-mentioned solution is transferred to the polytetrafluoroethylliner liner (volume 100.0mL) having
It is put into autoclave, after sealing in electric drying oven with forced convection and is heated to 110 DEG C, and keep the temperature 12h under the conditions of the temperature, to
It is cooled to room temperature after reaction.By obtained mixture by filtering separation, with dehydrated alcohol and water washing is distilled for several times, so
It is placed on 60 DEG C of drying overnight in hot blast drying box.By the powder after drying in Muffle furnace 550 DEG C of calcining 3h.To prepared
Metal oxide characterized: Fig. 1 is X ray diffracting spectrum, it can be seen from the figure that prepared metal oxide is main
By Spinel CuCo2O4Composition, with a small amount of CuO.
Embodiment 2
It weighs 1g cetyl trimethylammonium bromide to be dissolved in 70.0mL distilled water, then weighs 0.2416g tri- and be hydrated nitre
Sour copper, 0.5821g cabaltous nitrate hexahydrate and 0.3003g urea are added in above-mentioned solution, and magnetic agitation makes it dissolve.Solution is turned
It moves in the autoclave for the polytetrafluoroethylliner liner (volume 100.0mL) having, electric heating forced air drying is put into after sealing
It is heated to 120 DEG C in case, and keeps the temperature 14h under the conditions of the temperature, to be cooled to room temperature after reaction.The mixture that will be obtained
It is separated by filtering, with dehydrated alcohol and distills water washing for several times, be subsequently placed in 60 DEG C of drying overnight in hot blast drying box.It will
Powder after drying 500 DEG C of calcining 4h in Muffle furnace.Characterize to prepared metal oxide: Fig. 1 is X-ray diffraction
Map, it can be seen from the figure that object of the addition of cetyl trimethylammonium bromide without the prepared metal oxide of change
Phase composition；Fig. 2 is scanning electron microscope diagram, from the figures it is clear that prepared CuCo2O4/ CuO is had by surface
The nano flake of flourishing cellular structure forms.
Embodiment 3
It weighs 0.5g polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer and is dissolved in 70.0mL distilled water
In, it then weighs 0.2416g Gerhardite, 0.5821g cabaltous nitrate hexahydrate and 0.3604g urea and above-mentioned solution is added
In, magnetic agitation makes it dissolve.Solution is transferred to the reaction under high pressure for the polytetrafluoroethylliner liner (volume 100.0mL) having
It is put into kettle, after sealing in electric drying oven with forced convection and is heated to 120 DEG C, and keep the temperature 14h under the conditions of the temperature, to the end of reacting
After be cooled to room temperature.By obtained mixture by filtering separation, with dehydrated alcohol and distills water washing for several times, be subsequently placed in heat
60 DEG C of drying overnight in air dry oven.By the powder after drying in Muffle furnace 500 DEG C of calcining 3h.To prepared metal oxygen
Compound is characterized: Fig. 1 is X ray diffracting spectrum, it can be seen from the figure that polyethylene oxide-polypropylene oxide-polycyclic oxygen second
Object phase composition of the addition of alkane triblock copolymer without the prepared metal oxide of change.
Embodiment 4
2- hydroxyl-4-methoxybenzophenone-5-sulfonic acid solution 200.0mL with distilled water with 10.0mg/L is in beaker
In, it is 7.8 that boric acid/sodium tetraborate, which is added, and adjusts pH value of solution.The preparation of 20.0mg embodiment 1/2/3 is added in the above solution
CuCo2O4/ CuO, peroxy-monosulfate, which is added, makes its concentration 0.65mmol/L, is sufficiently stirred is reacted at room temperature.In setting
Time interval takes 5.0mL reaction solution, and being rapidly added the hypo solution that 200.0 μ L concentration are 150.0mmol/L makes to react
Stop, the dense of 2- hydroxyl-4-methoxybenzophenone-5-sulfonic acid is measured by high performance liquid chromatography after 0.45 μm of filter filters
Degree measures the concentration of the copper and cobalt of catalyst dissolution in reaction solution by inductivity coupled plasma mass spectrometry.As a result see Fig. 3 and figure
4。
Compared with the oxidation of independent peroxy-monosulfate, CuCo2O4/ CuO's adds so that 2- hydroxyl -4- methoxyl group -5- sulfonic acid two
Benzophenone efficient degradation.After reacting 15min, 2- hydroxyl-4-methoxybenzophenone-5-sulfonic acid is substantially completely removed.At this point, copper
Dissolution with cobalt is below 30.0 μ g/L, provides far below correlation water standard.
The above-mentioned nanometer thin sheet CuCo for showing embodiment 1,2,3 and preparing2O4/ CuO can efficiently activate peroxy-monosulfate drop
Organic pollutant is solved, and there is good stability during removing removal organic polluter.
Embodiment 5
Match the 2- hydroxyl -4- methoxyl group -5- sulfonic acid hexichol of 10.0mg/L in city domestic sewage treatment plant secondary effluent
Ketone solution 200.0mL is in beaker.The CuCo of the preparation of 20.0mg embodiment 2 is added in the above solution2O4/ CuO, was added
One sulfate makes its concentration 0.65mmol/L, is sufficiently stirred is reacted at room temperature.Take 1.0mL anti-in the time interval of setting
Liquid is answered, being rapidly added the hypo solution that 50.0 μ L concentration are 150.0mmol/L stops reaction, through 0.45 μm of filter mistake
The concentration of 2- hydroxyl-4-methoxybenzophenone-5-sulfonic acid is measured after filter by high performance liquid chromatography.As a result see Fig. 5.
Although due to the presence of natural organic matter and inorganic ions, 2- hydroxyl in city domestic sewage treatment plant secondary effluent
The degradation of base -4- methoxyl group -5- sulfonic acid benzophenone by a degree of inhibition, but still have more than 95% 2- hydroxyl -
4- methoxyl group -5- sulfonic acid benzophenone is degraded after reacting 1h.The experimental results showed that prepared nanometer thin sheet
CuCo2O4/ CuO can be used for class Fenton water treatment technology, efficient degradation low concentration persistent organic pollutants.
Embodiment 6
Nanometer thin sheet CuCo2O4/ CuO class Fenton method for treating water can be applied to city domestic sewage or industrial wastewater
After grid-setting pot-primary sedimentation tank-biochemistry pool-secondary settling tank processing, using filled with CuCo2O4The filter tank of/CuO filler into
Row advanced treating, is then discharged；When being used for groundwater remediation, a filtering can be placed on the direction of direction of groundwater flow
Column, by CuCo2O4/ CuO powder fills in Filter column, injects peroxide agent by injection well, after underground water is by Filter column,
It can be purified.
Claims (7)
1. a kind of nanometer thin sheet CuCo2O4/ CuO class Fenton method for treating water, it is characterised in that CuCo2O4/ CuO is by having prosperity
The nano flake in duct assembles, and can efficiently activate peroxide and generate free radicals, and improves sanitary sewage, industrial wastewater and ground
It is lauched the degradation property of middle low concentration persistent organic pollutants.
2. nanometer thin sheet CuCo described in claim 12O4The preparation of/CuO can be completed according to the following steps:
(1) surfactant is dissolved in distilled water, is then separately added into Gerhardite, cabaltous nitrate hexahydrate in the solution
And urea, it stirs to dissolve；
(2) aqueous solution in step (1) is transferred in the autoclave with polytetrafluoroethylliner liner, electricity is put into after sealing
It is heated to 110-130 DEG C in hot blast drying box, and keeps the temperature 10-14h under the conditions of the temperature, to be cooled to room after reaction
Temperature；
(4) mixture for obtaining step (2) is washed out, dries by filtering separation；
(4) the russet powder for obtaining step (3) 500-600 DEG C of calcining in Muffle furnace, 1-5 DEG C of heating rate/min are protected
Warm 3-4h, it is to be cooled to after room temperature, obtain nanometer thin sheet CuCo2O4/CuO。
3. nanometer thin sheet CuCo as claimed in claim 22O4The preparation of/CuO, it is characterised in that: the table being added in step (1)
Face activating agent is cetyl trimethylammonium bromide, in polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer
One kind, additional amount 0-1.0g；The Gerhardite of addition, the molar ratio of cabaltous nitrate hexahydrate are 1:2；Metal salt it is total
Molar concentration is 0.043-0.108mol/L；The mole that urea is added is 1.6-2.0 times of metal salt mole sum.
4. nanometer thin sheet CuCo described in claim 12O4/ CuO, it is characterised in that its specific surface area is 14.6-42.3m2/
G, pore volume 0.268-0.635m3/ g, CuCo2O4Content with CuO is respectively 62.4%-73.5% and 26.5%-
37.6%.
5. peroxide described in claim 1 is hydrogen peroxide, single peroxy-monosulfate, peroxydisulfate.
6. nanometer thin sheet CuCo described in claim 12O4/ CuO class Fenton method for treating water, technological parameter are as follows:
(1) the pH range of pending water is 3.0-10.0；
(2) copper-cobalt/cobalt oxide dosage is 20.0-150.0mg/L；
(3) dosage of peroxide is 0.16-0.97mmol/L；
(4) reaction time is 15-60min.
7. nanometer thin sheet CuCo described in claim 12O4/ CuO class Fenton method for treating water can be applied to urban life dirt
Water or industrial wastewater are after grid-setting pot-primary sedimentation tank-biochemistry pool-secondary settling tank processing, using filled with CuCo2O4/CuO
The filter tank of filler carries out advanced treating, is then discharged；When being used for groundwater remediation, can be put on the direction of direction of groundwater flow
A Filter column is set, by CuCo2O4/ CuO powder fills in Filter column, injects peroxide agent by injection well, passes through in underground water
After Filter column, it will be able to be purified.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110201699A (en) * | 2019-06-11 | 2019-09-06 | 武汉纺织大学 | A kind of CuO-CN peroxide composite catalyst and its preparation method and application for high-level oxidation technology |
| 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 |
| CN114917911A (en) * | 2022-06-10 | 2022-08-19 | 东北石油大学 | Preparation and application of three-dimensional supported copper cobaltate catalyst |
| CN115779964A (en) * | 2022-12-05 | 2023-03-14 | 东南大学 | Urea modified copper oxide material and preparation method and application thereof |
-
2018
- 2018-10-17 CN CN201811209133.4A patent/CN109205756A/en active Pending
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110201699A (en) * | 2019-06-11 | 2019-09-06 | 武汉纺织大学 | A kind of CuO-CN peroxide composite catalyst and its preparation method and application for high-level oxidation technology |
| CN110201699B (en) * | 2019-06-11 | 2022-04-15 | 武汉纺织大学 | CuO-CN peroxide composite catalyst for advanced oxidation technology and preparation method and application thereof |
| 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 |
| CN114917911A (en) * | 2022-06-10 | 2022-08-19 | 东北石油大学 | Preparation and application of three-dimensional supported copper cobaltate catalyst |
| CN115779964A (en) * | 2022-12-05 | 2023-03-14 | 东南大学 | Urea modified copper oxide material and preparation method and application thereof |
| CN115779964B (en) * | 2022-12-05 | 2024-04-23 | 东南大学 | Urea modified copper oxide material and preparation method and application thereof |
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Application publication date: 20190115 |