CN109967079A - A method of preparing the metal oxide for eliminating organic pollutants - Google Patents
A method of preparing the metal oxide for eliminating organic pollutants Download PDFInfo
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
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- 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
- B01J23/78—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 alkali- or alkaline earth metals
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
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Abstract
The present invention relates to catalysis material technologies of preparing, it is desirable to provide a method of prepare the metal oxide for eliminating organic pollutants.Include: to be dissolved in low-valent metal presoma and strong oxidizer in solvent respectively, strong oxidant solution is added dropwise in low-valent metal precursor solution, stirs evenly carry out redox reaction；React gained sediment it is washed, it is dry after, directly carry out calcination process and obtain metal oxide；Alternatively, first grinding, being uniformly mixed together with coagent by the sediment after drying, calcination process is then carried out again, obtains metal oxide；Product of the present invention has excellent catalytic effect, can realize the efficient elimination to organic pollutants under relatively mild conditions；Synthesis process of the invention is simple, at low cost, shows huge advantage compared to the prior art.
Description
Technical field
The present invention relates to catalysis material technology of preparing, in particular to a kind of gold prepared for eliminating organic pollutants
Belong to the method for oxide material.
Background technique
Nowadays, with the development of the society, all kinds of chemical plant are fast-developing, while bringing human economy benefit,
Many new problems are produced, for example, environmental problem.Plant produced institute waste discharge can directly cause seriously ecological environment
Destruction, by food chain transmitting can also indirect hazard human health.Often containing a large amount of organic in industrial discharge waste water
Object, therefore, effectively eliminating organic pollutants is an effective way for solving contaminated wastewater, but how to realize low temperature,
It is efficiently a crucial challenge to the elimination of Industry Waste Organic substance in water.Aerobic oxidation is in organic synthesis and industrial oxidation
In be considered as most basic one of reaction process, by organic pollutant degradation elimination be considered a kind of straight by oxidation reaction
Connect effective method.In current method, in use often to the common catalyst of the elimination of organic pollutants
It is difficult to high activity and long-time stability, so that practical application is limited, on the other hand, to organic pollutants
The problems such as the efficient oxidation is typically necessary very high operation temperature and huge energy consumption, therefore there are high risk, Gao Chengben, so
Design is prepared with excellent catalytic performance, and catalysis material cheap and easy to get, is realized at low temperature to organic pollutants
Efficient oxidation degradation have great importance.
Cobalt (Co) base, manganese (Mn) metal oxides are since its excellent oxidation susceptibility is in many class catalytic oxidation mistakes
There is outstanding performance in journey, for example, original performance is suffered from CO oxidation, ammoxidation, VOC are eliminated, to organic dirt
During the elimination for contaminating object, cobalt (Co) base, manganese (Mn) metal oxides also show its excellent catalytic activity.
Commercial oxidation cobalt or oxidation manganese material are due to its traditional preparation method (including surfactant aids precipitation
Method, coprecipitation, hydro-thermal method etc.), cause its surface to be difficult to the oxygen species for having high activity, thus in the elimination to organic matter
Meet demand is difficult in journey.Therefore, there is high activity by designing and preparing surface using new redox preparation method,
The cobalt oxide of active oxygen species aoxidizes manganese material, and is added by the auxiliary agent in later period, enriches it in organic pollutant elimination
Application have a very big significance.
Summary of the invention
The technical problem to be solved by the present invention is to overcome deficiency in the prior art, provide a kind of prepare for eliminating water
The method of the metal oxide of middle organic pollutant.
In order to solve the technical problem, solution of the invention is:
A kind of method preparing the metal oxide for eliminating organic pollutants is provided, is included the following steps:
Low-valent metal presoma and strong oxidizer are dissolved in solvent respectively, strong oxidant solution is added dropwise to low-valent metal
In precursor solution, carry out redox reaction is stirred evenly；React gained sediment it is washed, it is dry after, directly roasted
Burning handles to obtain metal oxide；Alternatively, first the sediment after drying being ground together with coagent, being uniformly mixed, then
Calcination process is carried out again, obtains metal oxide；
The low-valent metal presoma is any in divalent cobalt, manganese salt, divalent cobalt hydrate or manganese salt hydrate
It is a kind of；Strong oxidizer is potassium nitrite or potassium permanganate；Coagent is any in iron powder, magnesium powder, nickel powder, copper powder or zinc powder
It is one or more.
In the present invention, the mass ratio of the low-valent metal presoma and strong oxidizer is 10~1；Coagent and at a low price gold
The mass ratio for belonging to presoma is 0~1；When using various active auxiliary agent, keep the adding proportion of each coagent identical.
In the present invention, the solvent is any one in water, methanol, ethyl alcohol, toluene, acetone or methylene chloride.
In the present invention, the roasting, which refers to, to be roasted in air with 150~800 DEG C of conditions.
Inventive principle description:
Inventive principle of the present invention is as follows: low-valent metal presoma, strong oxidizer being dissolved in solvent first, then
Strong oxidant solution is slowly dropped in low-valent metal precursor solution, is sent out between the process middle or low price element and high valence elements
Raw redox reaction, generates solid sediment matter, and using later washing, the addition of dry and auxiliary agent and calcination process can
To prepare the oxide material that can be used for organic pollutants elimination of high activity.
Compared with prior art, the beneficial effects of the present invention are:
1, in the prior art, the oxidation of organic pollutants is eliminated often using a large amount of expensive oxidants
And carried out under harsh reaction condition, or use precious metal catalytic material, this resulted in a large amount of energy loss with
And the increase of material cost.It can be real under relatively mild conditions using the cheap metal oxide material prepared in the present invention
Now to the efficient elimination of organic pollutants, for example, high to the phenol degrading rate of 200ppm content in water under oxygen atmosphere
Up to 99%, excellent catalytic effect is shown during the elimination to organic pollutants.
2, synthesis process of the invention is simple, at low cost, shows huge advantage compared to the prior art.
Specific embodiment
Present invention is further described in detail With reference to embodiment:
The following examples can make the professional technician of this profession that the present invention be more fully understood, but not with any side
The formula limitation present invention.
Embodiment 1
By 10.0g cobalt chloride (CoCl2) be dissolved in 20mL water, 10g potassium nitrite is dissolved in 50mL water, is sufficiently dissolved to it
Later, potassium nitrite solution is slowly dropped in cobalt chloride solution, and is stirred evenly in beaker, the precipitating that will finally obtain
Object washing, drying, then 400 DEG C of roasting 4h in Muffle furnace, obtain cobalt oxide material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 83.0%.
Embodiment 2
By 10.0g cobalt chloride (CoCl2) be dissolved in 20mL water, 5g potassium nitrite is dissolved in 50mL water, is sufficiently dissolved to it
Later, potassium nitrite solution is slowly dropped in cobalt chloride solution, and is stirred evenly in beaker, the precipitating that will finally obtain
Object washing, drying, then 400 DEG C of roasting 4h in Muffle furnace, obtain cobalt oxide material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 70.0%.
Embodiment 3
By 10.0g cobalt chloride (CoCl2) be dissolved in 20mL water, 1.7g potassium nitrite is dissolved in 50mL water, sufficiently molten to it
After solution, potassium nitrite solution is slowly dropped in cobalt chloride solution, and is stirred evenly in beaker, it is finally heavy by what is obtained
Starch washing, drying, then 400 DEG C of roasting 4h in Muffle furnace, obtain cobalt oxide material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 56.6%.
Embodiment 4
By 10.0g cobalt chloride (CoCl2) be dissolved in 20mL water, 10g potassium nitrite is dissolved in 50mL water, is sufficiently dissolved to it
Later, potassium nitrite solution is slowly dropped in cobalt chloride solution, and is stirred evenly in beaker, the precipitating that will finally obtain
Object washing, drying, then 150 DEG C of roasting 4h in Muffle furnace, obtain cobalt oxide material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 34.2%.
Embodiment 5
By 10.0g cobalt chloride (CoCl2) be dissolved in 20mL water, 10g potassium nitrite is dissolved in 50mL water, is sufficiently dissolved to it
Later, potassium nitrite solution is slowly dropped in cobalt chloride solution, and is stirred evenly in beaker, the precipitating that will finally obtain
Object washing, drying, then 600 DEG C of roasting 4h in Muffle furnace, obtain cobalt oxide material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 78.9%.
Embodiment 6
By 10.0g cobalt chloride (CoCl2) be dissolved in 20mL water, 10g potassium nitrite is dissolved in 50mL water, is sufficiently dissolved to it
Later, potassium nitrite solution is slowly dropped in cobalt chloride solution, and is stirred evenly in beaker, the precipitating that will finally obtain
Object washing, drying, then 800 DEG C of roasting 4h in Muffle furnace, obtain cobalt oxide material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 73.6%.
Embodiment 7
By 10.0g cobalt chloride (CoCl2) be dissolved in 20mL methanol, 10g potassium nitrite is dissolved in 50mL methanol, sufficiently to it
After dissolution, potassium nitrite solution is slowly dropped in cobalt chloride solution, and is stirred evenly in beaker, will finally be obtained
Sediment washing, drying, then 400 DEG C of roasting 4h in Muffle furnace, obtain cobalt oxide material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 75.2%.
Embodiment 8
By 10.0g cobalt chloride (CoCl2) be dissolved in 20mL ethyl alcohol, 10g potassium nitrite is dissolved in 50mL ethyl alcohol, sufficiently to it
After dissolution, potassium nitrite solution is slowly dropped in cobalt chloride solution, and is stirred evenly in beaker, will finally be obtained
Sediment washing, drying, then 400 DEG C of roasting 4h in Muffle furnace, obtain cobalt oxide material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 82.0%.
Embodiment 9
By 10.0g cobalt chloride (CoCl2) be dissolved in 20mL toluene, 10g potassium nitrite is dissolved in 50mL toluene, sufficiently to it
After dissolution, potassium nitrite solution is slowly dropped in cobalt chloride solution, and is stirred evenly in beaker, will finally be obtained
Sediment washing, drying, then 400 DEG C of roasting 4h in Muffle furnace, obtain cobalt oxide material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 60.2%.
Embodiment 10
By 10.0g cobalt chloride (CoCl2) be dissolved in 20mL acetone, 10g potassium nitrite is dissolved in 50mL acetone, sufficiently to it
After dissolution, potassium nitrite solution is slowly dropped in cobalt chloride solution, and is stirred evenly in beaker, will finally be obtained
Sediment washing, drying, then 400 DEG C of roasting 4h in Muffle furnace, obtain cobalt oxide material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 55.1%.
Embodiment 11
By 10.0g cobalt chloride (CoCl2) be dissolved in 20mL methylene chloride, 10g potassium nitrite is dissolved in 50mL methylene chloride,
After sufficiently being dissolved to it, potassium nitrite solution is slowly dropped in cobalt chloride solution, and is stirred evenly in beaker, finally
Obtained sediment is washed, drying, then 400 DEG C of roasting 4h in Muffle furnace, obtain cobalt oxide material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 59.3%.
Embodiment 12
By 10.0g cobalt chloride (CoCl2) be dissolved in 20mL water, 10g potassium nitrite is dissolved in 50mL water, is sufficiently dissolved to it
Later, potassium nitrite solution is slowly dropped in cobalt chloride solution, and is stirred evenly in beaker, the precipitating that will finally obtain
Object washing, drying, and be fully ground and be uniformly mixed with 2g iron powder, then 400 DEG C of roasting 4h in Muffle furnace, obtain Fe2O3 doping oxygen
Change cobalt material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 86.9%.
Embodiment 13
By 10.0g cobalt chloride (CoCl2) be dissolved in 20mL water, 10g potassium nitrite is dissolved in 50mL water, is sufficiently dissolved to it
Later, potassium nitrite solution is slowly dropped in cobalt chloride solution, and is stirred evenly in beaker, the precipitating that will finally obtain
Object washing, drying, and be fully ground and be uniformly mixed with 2g magnesium powder, then 400 DEG C of roasting 4h in Muffle furnace, obtain magnesium doping oxygen
Change cobalt material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 80.3%.
Embodiment 14
By 10.0g cobalt chloride (CoCl2) be dissolved in 20mL water, 10g potassium nitrite is dissolved in 50mL water, is sufficiently dissolved to it
Later, potassium nitrite solution is slowly dropped in cobalt chloride solution, and is stirred evenly in beaker, the precipitating that will finally obtain
Object washing, drying, and be fully ground and be uniformly mixed with 2g nickel powder, then 400 DEG C of roasting 4h in Muffle furnace, obtain nickel doping oxygen
Change cobalt material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 76.4%.
Embodiment 15
By 10.0g cobalt chloride (CoCl2) be dissolved in 20mL water, 10g potassium nitrite is dissolved in 50mL water, is sufficiently dissolved to it
Later, potassium nitrite solution is slowly dropped in cobalt chloride solution, and is stirred evenly in beaker, the precipitating that will finally obtain
Object washing, drying, and be fully ground and be uniformly mixed with 2g copper powder, then 400 DEG C of roasting 4h in Muffle furnace, obtain Copper-cladding Aluminum Bar oxygen
Change cobalt material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 85.0%.
Embodiment 16
By 10.0g cobalt chloride (CoCl2) be dissolved in 20mL water, 10g potassium nitrite is dissolved in 50mL water, is sufficiently dissolved to it
Later, potassium nitrite solution is slowly dropped in cobalt chloride solution, and is stirred evenly in beaker, the precipitating that will finally obtain
Object washing, drying, and be fully ground and be uniformly mixed with 2g zinc powder, then 400 DEG C of roasting 4h in Muffle furnace, obtain zinc doping oxygen
Change cobalt material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 77.3%.
Embodiment 17
By 10.0g cobalt chloride (CoCl2) be dissolved in 20mL water, 10g potassium nitrite is dissolved in 50mL water, is sufficiently dissolved to it
Later, potassium nitrite solution is slowly dropped in cobalt chloride solution, and is stirred evenly in beaker, the precipitating that will finally obtain
Object washing, drying, and be fully ground and be uniformly mixed with 5g iron powder, then 400 DEG C of roasting 4h in Muffle furnace, obtain Fe2O3 doping oxygen
Change cobalt material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 74.8%.
Embodiment 18
By 10.0g cobalt chloride (CoCl2) be dissolved in 20mL water, 10g potassium nitrite is dissolved in 50mL water, is sufficiently dissolved to it
Later, potassium nitrite solution is slowly dropped in cobalt chloride solution, and is stirred evenly in beaker, the precipitating that will finally obtain
Object washing, drying, and be fully ground and be uniformly mixed with 10g iron powder, then 400 DEG C of roasting 4h in Muffle furnace, obtain Fe2O3 doping
Cobalt oxide material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 66.8%.
Embodiment 19
By 10.0g cobalt chloride (CoCl2) be dissolved in 20mL water, 10g potassium nitrite is dissolved in 50mL water, is sufficiently dissolved to it
Later, potassium nitrite solution is slowly dropped in cobalt chloride solution, and is stirred evenly in beaker, the precipitating that will finally obtain
Object washing, drying, and be fully ground and be uniformly mixed with 1g iron powder and 1g copper powder, then 400 DEG C of roasting 4h in Muffle furnace, obtain
Iron, Copper-cladding Aluminum Bar cobalt oxide material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 89.6%.
Embodiment 20
By 10.0g cobalt chloride (CoCl2) be dissolved in 20mL water, 10g potassium nitrite is dissolved in 50mL water, is sufficiently dissolved to it
Later, potassium nitrite solution is slowly dropped in cobalt chloride solution, and is stirred evenly in beaker, the precipitating that will finally obtain
Object washing, drying, and with 0.7g iron powder, 0.7g copper powder and 0.7g magnesium powder be fully ground it is uniformly mixed, then 400 in Muffle furnace
DEG C roasting 4h, obtains iron, copper, magnesium adulterates cobalt oxide material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 94.1%.
Embodiment 21
By 10.0g cobalt chloride (CoCl2) be dissolved in 20mL water, 10g potassium nitrite is dissolved in 50mL water, is sufficiently dissolved to it
Later, potassium nitrite solution is slowly dropped in cobalt chloride solution, and is stirred evenly in beaker, the precipitating that will finally obtain
Object washing, drying, and with 0.5g iron powder, 0.5g copper powder and 0.5g magnesium powder, 0.5g zinc powder be fully ground it is uniformly mixed, then in horse
Not 400 DEG C of roasting 4h in furnace, obtain iron, copper, magnesium, zinc doping cobalt oxide material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 90.6%.
Embodiment 22
By 10.0g cobalt chloride (CoCl2) be dissolved in 20mL water, 10g potassium nitrite is dissolved in 50mL water, is sufficiently dissolved to it
Later, potassium nitrite solution is slowly dropped in cobalt chloride solution, and is stirred evenly in beaker, the precipitating that will finally obtain
Object washing, drying, and with 0.4g iron powder, 0.4g copper powder and 0.4g magnesium powder, 0.4g zinc powder, it is equal that 0.4g nickel powder is fully ground mixing
Even, then 400 DEG C of roasting 4h in Muffle furnace, obtain iron, copper, magnesium, zinc, nickel doping cobalt oxide material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 82.1%
Embodiment 23
By 10.0g cobalt nitrate (Co (NO3)2) be dissolved in 20mL water, 10g potassium nitrite is dissolved in 50mL water, sufficiently molten to it
After solution, potassium nitrite solution is slowly dropped in cobalt nitrate solution, and is stirred evenly in beaker, it is finally heavy by what is obtained
Starch washing, drying, and with 0.7g iron powder, 0.7g copper powder and 0.7g magnesium powder be fully ground it is uniformly mixed, then in Muffle furnace
400 DEG C of roasting 4h, obtain iron, copper, and magnesium adulterates cobalt oxide material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 93.6%.
Embodiment 24
By 10.0g Cobalt(II) nitrate hexahydrate (Co (NO3)2·6H2O it) is dissolved in 20mL water, 10g potassium nitrite is dissolved in 50mL
In water, after sufficiently being dissolved to it, potassium nitrite solution is slowly dropped in cobalt nitrate solution, and is stirred in beaker
It is even, finally obtained sediment is washed, drying, and be fully ground mixing with 0.7g iron powder, 0.7g copper powder and 0.7g magnesium powder
Even, then 400 DEG C of roasting 4h in Muffle furnace, obtain iron, copper, and magnesium adulterates cobalt oxide material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 93.9%.
Embodiment 25
By 10.0g manganese nitrate (Mn (NO3)2) be dissolved in 20mL water, 10g potassium permanganate is dissolved in 50mL water, sufficiently molten to it
After solution, liquor potassic permanganate is slowly dropped in manganese nitrate solution, and is stirred evenly in beaker, it is finally heavy by what is obtained
Starch washing, drying, then 400 DEG C of roasting 4h in Muffle furnace, obtain oxidation manganese material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 89.4%.
Embodiment 26
By 10.0g manganese nitrate (Mn (NO3)2) be dissolved in 20mL water, 5g potassium permanganate is dissolved in 50mL water, sufficiently molten to it
After solution, liquor potassic permanganate is slowly dropped in manganese nitrate solution, and is stirred evenly in beaker, it is finally heavy by what is obtained
Starch washing, drying, then 400 DEG C of roasting 4h in Muffle furnace, obtain oxidation manganese material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 86.8%.
Embodiment 27
By 10.0g manganese nitrate (Mn (NO3)2) be dissolved in 20mL water, 1g potassium permanganate is dissolved in 50mL water, sufficiently molten to it
After solution, liquor potassic permanganate is slowly dropped in manganese nitrate solution, and is stirred evenly in beaker, it is finally heavy by what is obtained
Starch washing, drying, then 400 DEG C of roasting 4h in Muffle furnace, obtain oxidation manganese material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 88.3%.
Embodiment 28
By 10.0g manganese nitrate (Mn (NO3)2) be dissolved in 20mL water, 10g potassium permanganate is dissolved in 50mL water, sufficiently molten to it
After solution, liquor potassic permanganate is slowly dropped in manganese nitrate solution, and is stirred evenly in beaker, it is finally heavy by what is obtained
Starch washing, drying, then 150 DEG C of roasting 4h in Muffle furnace, obtain oxidation manganese material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 85.0%.
Embodiment 29
By 10.0g manganese nitrate (Mn (NO3)2) be dissolved in 20mL water, 10g potassium permanganate is dissolved in 50mL water, sufficiently molten to it
After solution, liquor potassic permanganate is slowly dropped in manganese nitrate solution, and is stirred evenly in beaker, it is finally heavy by what is obtained
Starch washing, drying, then 600 DEG C of roasting 4h in Muffle furnace, obtain oxidation manganese material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 89.0%.
Embodiment 30
By 10.0g manganese nitrate (Mn (NO3)2) be dissolved in 20mL water, 10g potassium permanganate is dissolved in 50mL water, sufficiently molten to it
After solution, liquor potassic permanganate is slowly dropped in manganese nitrate solution, and is stirred evenly in beaker, it is finally heavy by what is obtained
Starch washing, drying, then 800 DEG C of roasting 4h in Muffle furnace, obtain oxidation manganese material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 80.5%.
Embodiment 31
By 10.0g manganese nitrate (Mn (NO3)2) be dissolved in 20mL methanol, 10g potassium permanganate is dissolved in 50mL methanol, is filled to it
Divide after dissolution, liquor potassic permanganate is slowly dropped in manganese nitrate solution, and is stirred evenly in beaker, will finally be obtained
Sediment washing, drying, then 400 DEG C of roasting 4h in Muffle furnace obtain aoxidizing manganese material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 87.5%.
Embodiment 32
By 10.0g manganese nitrate (Mn (NO3)2) be dissolved in 20mL ethyl alcohol, 10g potassium permanganate is dissolved in 50mL ethyl alcohol, is filled to it
Divide after dissolution, liquor potassic permanganate is slowly dropped in manganese nitrate solution, and is stirred evenly in beaker, will finally be obtained
Sediment washing, drying, then 400 DEG C of roasting 4h in Muffle furnace obtain aoxidizing manganese material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 92.4%.
Embodiment 33
By 10.0g manganese nitrate (Mn (NO3)2) be dissolved in 20mL toluene, 10g potassium permanganate is dissolved in 50mL toluene, is filled to it
Divide after dissolution, liquor potassic permanganate is slowly dropped in manganese nitrate solution, and is stirred evenly in beaker, will finally be obtained
Sediment washing, drying, then 400 DEG C of roasting 4h in Muffle furnace obtain aoxidizing manganese material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 80.9%.
Embodiment 34
By 10.0g manganese nitrate (Mn (NO3)2) be dissolved in 20mL acetone, 10g potassium permanganate is dissolved in 50mL acetone, is filled to it
Divide after dissolution, liquor potassic permanganate is slowly dropped in manganese nitrate solution, and is stirred evenly in beaker, will finally be obtained
Sediment washing, drying, then 400 DEG C of roasting 4h in Muffle furnace obtain aoxidizing manganese material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 88.4%.
Embodiment 35
By 10.0g manganese nitrate (Mn (NO3)2) be dissolved in 20mL methylene chloride, 10g potassium permanganate is dissolved in 50mL methylene chloride
In, after sufficiently being dissolved to it, liquor potassic permanganate is slowly dropped in manganese nitrate solution, and is stirred evenly in beaker,
Finally obtained sediment is washed, drying, then 400 DEG C of roasting 4h in Muffle furnace, obtains oxidation manganese material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 82.1%.
Embodiment 36
By 10.0g manganese nitrate (Mn (NO3)2) be dissolved in 20mL ethyl alcohol, 10g potassium permanganate is dissolved in 50mL ethyl alcohol, is filled to it
Divide after dissolution, liquor potassic permanganate is slowly dropped in manganese nitrate solution, and is stirred evenly in beaker, will finally be obtained
Sediment washing, drying, and uniform with 2g iron powder ground and mixed, then 400 DEG C of roasting 4h in Muffle furnace, obtain Fe2O3 doping
Aoxidize manganese material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 95.8%.
Embodiment 37
By 10.0g manganese nitrate (Mn (NO3)2) be dissolved in 20mL ethyl alcohol, 10g potassium permanganate is dissolved in 50mL ethyl alcohol, is filled to it
Divide after dissolution, liquor potassic permanganate is slowly dropped in manganese nitrate solution, and is stirred evenly in beaker, will finally be obtained
Sediment washing, drying is and uniform with 2g magnesium powder ground and mixed, then 400 DEG C of roasting 4h in Muffle furnace, obtains magnesium and adulterates
Aoxidize manganese material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 88.2%.
Embodiment 38
By 10.0g manganese nitrate (Mn (NO3)2) be dissolved in 20mL ethyl alcohol, 10g potassium permanganate is dissolved in 50mL ethyl alcohol, is filled to it
Divide after dissolution, liquor potassic permanganate is slowly dropped in manganese nitrate solution, and is stirred evenly in beaker, will finally be obtained
Sediment washing, drying is and uniform with 2g nickel powder ground and mixed, then 400 DEG C of roasting 4h in Muffle furnace, obtains nickel and adulterates
Aoxidize manganese material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 90.2%.
Embodiment 39
By 10.0g manganese nitrate (Mn (NO3)2) be dissolved in 20mL ethyl alcohol, 10g potassium permanganate is dissolved in 50mL ethyl alcohol, is filled to it
Divide after dissolution, liquor potassic permanganate is slowly dropped in manganese nitrate solution, and is stirred evenly in beaker, will finally be obtained
Sediment washing, drying, and uniform with 2g copper powder ground and mixed, then 400 DEG C of roasting 4h in Muffle furnace, obtain Copper-cladding Aluminum Bar
Aoxidize manganese material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 98.4%.
Embodiment 40
By 10.0g manganese nitrate (Mn (NO3)2) be dissolved in 20mL ethyl alcohol, 10g potassium permanganate is dissolved in 50mL ethyl alcohol, is filled to it
Divide after dissolution, liquor potassic permanganate is slowly dropped in manganese nitrate solution, and is stirred evenly in beaker, will finally be obtained
Sediment washing, drying, and uniform with 2g zinc powder ground and mixed, then 400 DEG C of roasting 4h in Muffle furnace, obtain zinc doping
Aoxidize manganese material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 91.4%.
Embodiment 41
By 10.0g manganese nitrate (Mn (NO3)2) be dissolved in 20mL ethyl alcohol, 10g potassium permanganate is dissolved in 50mL ethyl alcohol, is filled to it
Divide after dissolution, liquor potassic permanganate is slowly dropped in manganese nitrate solution, and is stirred evenly in beaker, will finally be obtained
Sediment washing, drying, and uniform with 5g iron powder ground and mixed, then 400 DEG C of roasting 4h in Muffle furnace, obtain Fe2O3 doping
Aoxidize manganese material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 93.2%.
Embodiment 42
By 10.0g manganese nitrate (Mn (NO3)2) be dissolved in 20mL ethyl alcohol, 10g potassium permanganate is dissolved in 50mL ethyl alcohol, is filled to it
Divide after dissolution, liquor potassic permanganate is slowly dropped in manganese nitrate solution, and is stirred evenly in beaker, will finally be obtained
Sediment washing, drying, and uniform with 10g iron powder ground and mixed, then 400 DEG C of roasting 4h in Muffle furnace, obtain iron and mix
Miscellaneous oxidation manganese material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 83.9%.
Embodiment 43
By 10.0g manganese nitrate (Mn (NO3)2) be dissolved in 20mL ethyl alcohol, 10g potassium permanganate is dissolved in 50mL ethyl alcohol, is filled to it
Divide after dissolution, liquor potassic permanganate is slowly dropped in manganese nitrate solution, and is stirred evenly in beaker, will finally be obtained
Sediment washing, drying, and uniform with 1g iron powder and 1g copper powder ground and mixed, then 400 DEG C of roasting 4h in Muffle furnace, obtain
To iron, Copper-cladding Aluminum Bar aoxidizes manganese material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 99.0%.
Embodiment 44
By 10.0g manganese nitrate (Mn (NO3)2) be dissolved in 20mL ethyl alcohol, 10g potassium permanganate is dissolved in 50mL ethyl alcohol, is filled to it
Divide after dissolution, liquor potassic permanganate is slowly dropped in manganese nitrate solution, and is stirred evenly in beaker, will finally be obtained
Sediment washing, drying, and with 0.7g iron powder and 0.7g copper powder, 0.7g zinc powder ground and mixed is uniform, then in Muffle furnace
400 DEG C of roasting 4h, obtain iron, copper, and zinc doping aoxidizes manganese material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 98.4%.
Embodiment 45
By 10.0g manganese nitrate (Mn (NO3)2) be dissolved in 20mL ethyl alcohol, 10g potassium permanganate is dissolved in 50mL ethyl alcohol, is filled to it
Divide after dissolution, liquor potassic permanganate is slowly dropped in manganese nitrate solution, and is stirred evenly in beaker, will finally be obtained
Sediment washing, drying, and with 0.5g iron powder, 0.5g copper powder and 0.5g zinc powder, 0.5g nickel powder ground and mixed is uniform, then exists
400 DEG C of roasting 4h in Muffle furnace obtain iron, copper, zinc, nickel doping oxidation manganese material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 99.0%.
Embodiment 46
By 10.0g manganese nitrate (Mn (NO3)2) be dissolved in 20mL ethyl alcohol, 10g potassium permanganate is dissolved in 50mL ethyl alcohol, is filled to it
Divide after dissolution, liquor potassic permanganate is slowly dropped in manganese nitrate solution, and is stirred evenly in beaker, will finally be obtained
Sediment washing, drying, and with 0.4g iron powder, 0.4g copper powder and 0.4g zinc powder, 0.4g nickel powder, 0.4g magnesium powder ground and mixed is equal
Even, then 400 DEG C of roasting 4h in Muffle furnace, obtain iron, copper, zinc, nickel, magnesium doping oxidation manganese material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 99.0%.
Embodiment 47
By 10.0g manganese chloride (MnCl2) be dissolved in 20mL ethyl alcohol, 10g potassium permanganate is dissolved in 50mL ethyl alcohol, sufficiently to it
It after dissolution, liquor potassic permanganate is slowly dropped in manganese chloride solution, and is stirred evenly in beaker, will finally obtained
Sediment washing, drying, then 400 DEG C of roasting 4h in Muffle furnace, obtain oxidation manganese material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 93.6%.
Embodiment 48
By 10.0g manganese sulfate (Mn (SO4)2) be dissolved in 20mL ethyl alcohol, 10g potassium permanganate is dissolved in 50mL ethyl alcohol, is filled to it
Divide after dissolution, liquor potassic permanganate is slowly dropped in manganese nitrate solution, and is stirred evenly in beaker, will finally be obtained
Sediment washing, drying, then 400 DEG C of roasting 4h in Muffle furnace obtain aoxidizing manganese material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 90.4%.
Embodiment 49
By 10.0g manganese nitrate hexahydrate ((Mn (SO4)2·6H2O it) is dissolved in 20mL ethyl alcohol, 10g potassium permanganate is dissolved in
In 50mL ethyl alcohol, after sufficiently being dissolved to it, liquor potassic permanganate is slowly dropped in manganese chloride solution, and is stirred in beaker
It mixes uniformly, finally washs obtained sediment, drying, then 400 DEG C of roasting 4h in Muffle furnace, obtain oxidation manganese material.
20mg above-mentioned material is added in 20mL phenol solution (200ppm phenol) as catalyst, is filled with 0.5MPa oxygen
Gas, 90 DEG C are reacted 5 hours, phenol conversion 94.6%.
Finally it should be noted that the above enumerated are only specific embodiments of the present invention.It is clear that the invention is not restricted to
Above embodiments can also have many variations.Those skilled in the art can directly lead from present disclosure
Out or all deformations for associating, it is considered as protection scope of the present invention.
Claims (4)
1. a kind of method for preparing the metal oxide for eliminating organic pollutants, which is characterized in that including walking as follows
It is rapid:
Low-valent metal presoma and strong oxidizer are dissolved in solvent respectively, strong oxidant solution is added dropwise to low-valent metal forerunner
In liquid solution, carry out redox reaction is stirred evenly；React gained sediment it is washed, it is dry after, directly carry out at roasting
Reason obtains metal oxide；Alternatively, first the sediment after drying ground together with coagent, be uniformly mixed, then again into
Row calcination process, obtains metal oxide；
The low-valent metal presoma is any one in divalent cobalt, manganese salt, divalent cobalt hydrate or manganese salt hydrate；
Strong oxidizer is potassium nitrite or potassium permanganate；Coagent is any one in iron powder, magnesium powder, nickel powder, copper powder or zinc powder
Or it is a variety of.
2. the method according to claim 1, wherein the mass ratio of the low-valent metal presoma and strong oxidizer
It is 10~1；The mass ratio of coagent and low-valent metal presoma is 0~1；When using various active auxiliary agent, keep each
The adding proportion of coagent is identical.
3. the method according to claim 1, wherein the solvent is water, methanol, ethyl alcohol, toluene, acetone or two
Any one in chloromethanes.
4. the method according to claim 1, wherein the roasting refers in air with 150~800 DEG C of items
Part roasting.
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| JPS6114133A (en) * | 1984-06-29 | 1986-01-22 | Mitsui Alum Kogyo Kk | Method for recovering gellium from dust produced by electrolyzing aluminum |
| CN105903464A (en) * | 2016-05-12 | 2016-08-31 | 太原理工大学 | NO oxidation catalyst with wide activity temperature window and preparation method and application thereof |
| CN107597138A (en) * | 2017-10-24 | 2018-01-19 | 上海纳米技术及应用国家工程研究中心有限公司 | Oxide-reduction method of cobalt manganese composite oxide applied to low concentration propane combustion reaction and products thereof and application |
| CN109250801A (en) * | 2018-10-24 | 2019-01-22 | 大连理工大学 | A kind of processing method of phenolic waste water |
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2019
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6114133A (en) * | 1984-06-29 | 1986-01-22 | Mitsui Alum Kogyo Kk | Method for recovering gellium from dust produced by electrolyzing aluminum |
| CN105903464A (en) * | 2016-05-12 | 2016-08-31 | 太原理工大学 | NO oxidation catalyst with wide activity temperature window and preparation method and application thereof |
| CN107597138A (en) * | 2017-10-24 | 2018-01-19 | 上海纳米技术及应用国家工程研究中心有限公司 | Oxide-reduction method of cobalt manganese composite oxide applied to low concentration propane combustion reaction and products thereof and application |
| CN109250801A (en) * | 2018-10-24 | 2019-01-22 | 大连理工大学 | A kind of processing method of phenolic waste water |
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Application publication date: 20190705 |