CN108435180A - A kind of support type ozone high grade oxidation catalyst and preparation method thereof - Google Patents
A kind of support type ozone high grade oxidation catalyst and preparation method thereof Download PDFInfo
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- CN108435180A CN108435180A CN201810111083.XA CN201810111083A CN108435180A CN 108435180 A CN108435180 A CN 108435180A CN 201810111083 A CN201810111083 A CN 201810111083A CN 108435180 A CN108435180 A CN 108435180A
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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
- B01J23/755—Nickel
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0207—Pretreatment of the support
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
Abstract
The invention discloses a kind of preparation methods of support type ozone high grade oxidation catalyst, include the following steps：S1. γ Al are chosen2O3Sphere is carrier；S2. nickel nitrate and deionized water are mixed to obtain and stablize nickel nitrate solution, copper nitrate and deionized water are mixed to obtain and stablize copper nitrate solution, the mass ratio of the nickel nitrate and copper nitrate is 19:1；S3. the prepared nickel nitrate solutions of step S2 and copper nitrate solution are mixed with the step S1 carriers chosen, and persistently rocks 4 8h of concussion；S4. dry after the maceration extract after elimination step S3 dippings；S5. γ Al step S4 being prepared2O3Sphere is obtained with constant heating rate constant temperature calcining with γ Al2O3Sphere is carrier, NiO and the support type ozone high grade oxidation catalyst that CuO is active component.The present invention ozone high grade oxidation catalyst simultaneously have absorption and activation synergistic effect, can efficient absorption organic pollutants, while again can catalytic activation ozone molecule, obtain good O3 catalytic oxidation effect.
Description
Technical field
The present invention relates to catalyst technical field, it particularly relates to a kind of support type ozone high grade oxidation catalyst and
Preparation method.
Background technology
In recent years, with the rapid development of the industries such as petrochemical industry, plastics, synthetic fibers, coking, printing and dyeing, it is various containing
The waste water of the organic pollution of a large amount of difficult for biological degradation accordingly increases, they cause serious pollution into water body to environment.
Hardly degraded organic substance refers to that speed is very slow when being decomposed by the microorganisms, and it (also includes certain to decompose halfway organic matter
The metabolite of organic matter), this pollutant is easily enriched in vivo, also easily becomes the potential pollution source of water body.It is this kind of
Pollutant includes polycyclic aromatic hydrocarbon, halogenated hydrocarbons, heterocycle compound, organic atmosphere compound, organophosphorus pesticide, surfactant, organic
The toxic persistent organic pollutants such as dyestuff.The common feature of these substances is that toxicity is big, complex in composition, and chemical oxygen consumption (COC) is high,
General microorganism is hardly degraded effect to it, if these substances with being not added with improvement to environmental emission, certainly will be seriously dirty
It contaminates environment and threatens the health of the mankind.Therefore, very urgent to the research of the treatment technology of substance of this kind.
The treatment technology of difficult-degradation organic sewage bed include bioanalysis, biological reinforcing technology, optimum organization treatment process,
Physico-chemical process, oxidizing process.Bioanalysis is mainly the metabolism using microorganism, passes through the cohesion, absorption, oxygenolysis of microorganism
The effects that come the organic matter in sewage of degrading, have many advantages, such as to have a wide range of application, treating capacity is big, at low cost.But when waste water contains
When the organic matter of noxious material or bio-refractory, the treatment effect of bioanalysis is not good enough, or even cannot handle.Biological reinforcing technology
It is by improving outside environmental elements, improving biodegradable efficiency of the prior art to toxic hardly degraded organic substance, but dominant bacteria
Adaptability and regeneration issues of the kind in new environment are to be solved.It is dirty that optimum organization treatment process key adds powder activity carbon activity
Bricklayer's's skill：Using this technique, makes organic matter in addition to being handled by microbiological oxidation, also adsorbed by activated carbon.Due to activated carbon
The sludge sludge age on surface is longer, and pollutant is much larger than hydraulic detention time with microorganism time of contact, to make toxicity difficult to degrade
Organic removal rate improves, but similar with Fenton reagent method, will produce a large amount of mud, subsequent processing easily causes secondary pollution.
The document report that physico-chemical process handles persistent organic pollutants is rare, mainly there is absorption method, extraction, various membrane technologies
Deng all referring to the process of after-treatment.In oxidizing process, ozonation technology is widely applied in water treatment field,
Increasingly it is taken seriously.But due to the problems such as its ozone utilization rate is low, operating cost is high, seriously constrain the popularization of this technology with
Using.
With going deep into for research, advanced chemical oxidation technology comes into being.The basis of high-level oxidation technology is to use light
Irradiation, electricity, sound, catalyst.Ozone high grade oxidation is that catalyst is combined with oxidant, generates the extremely strong OH of activity in the reaction
Free radical, then by adduction, substitution, electronics transfer, the scission of link etc. between free radical and organic compound, make big point in water body
Son, hardly degraded organic substance oxidative degradation is at low toxicity or nontoxic small-molecule substance, or even is directly degraded into CO2And H2O, close to complete
Full mineralising.
Promote ozone to convert the efficiency of OH free radicals using catalyst as background, reduce the technology of operating cost
It attracts attention.High-efficiency catalytic activity and the strong transition-metal catalyst of stability have been a hot spot of research.
Therefore, with high-efficiency catalytic activity, strong, cheap, service life length and non-secondary pollution the ozone of stability
High grade oxidation catalytic agent is imperative.
For the problems in the relevant technologies, currently no effective solution has been proposed.
Invention content
For above-mentioned technical problem in the related technology, the present invention propose a kind of support type ozone high grade oxidation catalyst and
Preparation method can solve above-mentioned technical problem.
To realize the above-mentioned technical purpose, the technical proposal of the invention is realized in this way：
A kind of support type ozone high grade oxidation catalyst, with γ-Al2O3Sphere is carrier, and NiO and CuO are active component.
Further, it counts in mass ratio, the active component NiO：CuO is 1-9:1.
Further, the γ-Al2O3The grain size of sphere is 3-5mm.
A kind of preparation method of support type ozone high grade oxidation catalyst, includes the following steps：
S1. γ-Al are chosen in the selection and processing of carrier2O3Sphere is carrier；
S2. solution is configured, nickel nitrate and deionized water are mixed to obtain and stablize nickel nitrate solution, by copper nitrate and deionization
Water, which is mixed to obtain, stablizes copper nitrate solution, and the mass ratio of the nickel nitrate and copper nitrate is 1-9:1；
S3. it impregnates, the prepared nickel nitrate solutions of step S2 and copper nitrate solution is mixed with the step S1 carriers chosen, and
Persistently rock concussion 4-8h；
S4. it dries, filters off the maceration extract after step S3 dippings, the γ-Al that will be obtained2O3It is dried；
S5. it roasts, the γ-Al that step S4 is prepared2O3Sphere is with constant heating rate constant temperature calcining, calcination temperature
It it is 400-650 DEG C, soaking time 3-7h, product after roasting is the support type ozone high grade oxidation catalyst.
Further, step S1, γ-Al2O3The output time is less than direct use in 2 months；More than 2 months in 90-
It is dry at 150 DEG C.
Further, concussion frequency is rocked described in step S3：Preceding 2h is 15-30min/ times, follow-up time 30-60min/
It is secondary.
Further, the drying temperature described in step S4 is 90-150 DEG C, and step S4 is prepared by drying time 4-7h
γ-the Al arrived2O3Sphere is placed in Muffle furnace and is roasted.
Further, the heating rate described in step S5 is 4-6 DEG C/min.
A kind of support type ozone high grade oxidation catalyst is for adsorbing organic pollutants and catalytic activation ozone molecule.
Beneficial effects of the present invention：The ozone high grade oxidation catalyst of the present invention is by active component NiO and CuO active component
It is carried on γ-Al2O3Inside spherome surface, duct, the active component area ratio of catalyst is substantially increased, is extended using the longevity
The cost for handling sewage difficult to degrade is ordered and reduced, repeats and recycles, compared with traditional technology, removal efficiency is high and uses
It is not necessarily to other additional medicaments in the process；The ozone high grade oxidation catalyst of the present invention has absorption and activation synergistic effect simultaneously,
Can efficient absorption organic pollutants, while again can catalytic activation ozone molecule, generate the OH free radicals of high oxidative,
In catalyst surface, the absorption of organic pollution and the activation synergistic effect of oxidant obtain good O3 catalytic oxidation effect
Fruit.
Specific implementation mode
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
The every other embodiment that technical staff is obtained, shall fall within the protection scope of the present invention.
Embodiment 1：
（1）Carrier is chosen first, and the carrier selected is γ-Al2O3Producing the time is less than 2 months, Carrier diameters 3-
5mm；
（2）Configure solution：With deionized water dissolving Cu（NO3）2•3H2O obtains the copper nitrate solution 500ml of 2.7mol/L, and stirs
It mixes uniformly；With deionized water dissolving Ni（NO3）2•6H2O obtains the nickel nitrate solution 500ml of 0.32mol/L, and stirs evenly；Match
Set complete use；
（3）Dipping：The above-mentioned copper nitrates of 125ml and nickel nitrate solution are taken respectively, the γ-Al chosen with 300g2O3Carrier mixes simultaneously
6h is persistently rocked and shakes, preceding 2h frequencies are 15min/ times, and rear 4h frequencies are 30min/ times；
（4）It is dry：Maceration extract is filtered, impregnated carrier, 120 DEG C of drying 360min are taken out；
（5）Roasting：Material after drying is positioned in Muffle furnace, 600 DEG C are warming up to the constant heating rates of 5 DEG C/min,
Calcining at constant temperature 360min；Support type ozone high grade oxidation catalyst is can be obtained, obtained support type ozone high grade oxidation catalysis
The mass ratio of carrier and active material is γ-Al in agent2O3：CuO:NiO=100:9:1
Example 2：
（1）Carrier is chosen first, and the carrier selected is γ-Al2O3The time is produced more than 2 months, then is pre-processed：
120 DEG C of drying 7h, Carrier diameters 3-5mm；
（2）Configure solution：With deionized water dissolving Cu（NO3）2•3H2O obtains the copper nitrate solution 500ml of 2.7mol/L, and stirs
It mixes uniformly；With deionized water dissolving Ni（NO3）2•6H2O obtains the nickel nitrate solution 500ml of 0.32mol/L, and stirs evenly；Match
Set complete use；
（3）Dipping：The above-mentioned copper nitrates of 125ml and nickel nitrate solution are taken respectively, are mixed with the 300g carriers chosen and are persistently rocked
And 4h is shaken, preceding 2h frequencies are 20min/ times, and rear 2h frequencies are 60min/ times；
（4）It is dry：Maceration extract is filtered, impregnated carrier, 90 DEG C of drying 420min are taken out；
（5）Roasting：Material after drying is positioned in Muffle furnace, 500 are warming up to the heating rate that 4.2 DEG C/min is constant
DEG C, calcining at constant temperature 300min；Support type ozone high grade oxidation catalyst is can be obtained, obtained support type ozone high grade oxidation is urged
The mass ratio of carrier and active material is γ-Al in agent2O3：CuO:NiO=100:9:1.
Example 3：
（1）Carrier is chosen first, and the carrier selected is γ-Al2O3The time is produced more than 2 months, then is pre-processed：
150 DEG C of drying 5h, Carrier diameters 3-5mm；
（2）Configure solution：With deionized water dissolving Cu（NO3）2•3H2O obtains the copper nitrate solution 500ml of 2.4mol/L, and stirs
It mixes uniformly；With deionized water dissolving Ni（NO3）2•6H2O obtains the nickel nitrate solution 500ml of 0.81mol/L, and stirs evenly；Match
Set complete use；
（3）Dipping：The above-mentioned copper nitrates of 125ml and nickel nitrate solution are taken respectively, are mixed with the 300g carriers chosen and are persistently rocked
And 8h is shaken, preceding 2h frequencies are 30min/ times, and rear 6h frequencies are 40min/ times；
（4）It is dry：Maceration extract is filtered, impregnated carrier, 150 DEG C of drying 180min are taken out；
（5）Roasting：Material after drying is positioned in Muffle furnace, 650 DEG C are warming up to the constant heating rates of 5 DEG C/min,
Calcining at constant temperature 180min；Support type ozone high grade oxidation catalyst is can be obtained, obtained support type ozone high grade oxidation catalysis
The mass ratio of carrier and active material is γ-Al in agent2O3：CuO:NiO=100:8:2.5.
Example 4：
（1）Carrier is chosen first, and the carrier selected is γ-Al2O3The time is produced more than 2 months, then is pre-processed：
90 DEG C of drying 6h, Carrier diameters 3-5mm；
（2）Configure solution：With deionized water dissolving Cu（NO3）2•3H2O obtains the copper nitrate solution 500ml of 0.3mol/L, and stirs
It mixes uniformly；With deionized water dissolving Ni（NO3）2•6H2O obtains the nickel nitrate solution 500ml of 0.162mol/L, and stirs evenly；
It configures spare；
（3）Dipping takes the above-mentioned copper nitrates of 415ml and nickel nitrate solution respectively, mixes with the 1000g carriers chosen and persistently rocks
And shake 6h；Preceding 3h frequencies are 30min/ times, and rear 3h frequencies are 60min/ times；
（4）It is dry：Maceration extract is filtered, impregnated carrier, 110 DEG C of drying 240min are taken out；
（5）Roasting：Material after drying is positioned in Muffle furnace, 400 DEG C are warming up to the constant heating rates of 5 DEG C/min,
Calcining at constant temperature 360min；Support type ozone high grade oxidation catalyst is can be obtained, obtained support type ozone high grade oxidation catalysis
The mass ratio of carrier and active material is γ-Al in agent2O3：CuO:NiO=200：2：1.
It is discharged with certain petrochemical industry refinery high-concentration waste water（Rich in hard-degraded substance）For, embodiment 1-4 and different ozone height
Grade oxidation catalyst Contrast on effect see the table below 1- tables 4：
The oxidation catalysis effect of 1. embodiment 1 of table
The oxidation catalysis effect of 2. embodiment 2 of table
The oxidation catalysis effect of 3. embodiment 3 of table
The oxidation catalysis effect of 4. embodiment 4 of table
In conclusion by means of the above-mentioned technical proposal of the present invention, ozone high grade oxidation catalyst of the invention is by active component
NiO and CuO active components are carried on γ-Al2O3Inside spherome surface, duct, the active component area of catalyst is substantially increased
Than, it extends service life and reduces the cost for handling sewage difficult to degrade, repeat and recycle, compared with traditional technology,
Removal efficiency is high and use is not necessarily to other additional medicaments in the process；The ozone high grade oxidation catalyst of the present invention has absorption simultaneously
With activation act synergistically, can efficient absorption organic pollutants, while again can catalytic activation ozone molecule, generate high oxidation
Property OH free radicals, in catalyst surface, the absorption of organic pollution and the activation synergistic effect of oxidant obtain good
O3 catalytic oxidation effect.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (9)
1. a kind of support type ozone high grade oxidation catalyst, which is characterized in that with γ-Al2O3Sphere is carrier, and NiO and CuO are
Active component.
2. a kind of support type ozone high grade oxidation catalyst according to claim 1, which is characterized in that count in mass ratio, institute
State active component NiO：CuO is 1-9:1.
3. a kind of support type ozone high grade oxidation catalyst according to claim 1 or claim 2, which is characterized in that the γ-Al2O3
The grain size of sphere is 3-5mm.
4. a kind of preparation method of support type ozone high grade oxidation catalyst, which is characterized in that include the following steps：
S1. γ-Al are chosen in the selection and processing of carrier2O3Sphere is carrier；
S2. solution is configured, nickel nitrate and deionized water are mixed to obtain and stablize nickel nitrate solution, by copper nitrate and deionization
Water, which is mixed to obtain, stablizes copper nitrate solution, and the mass ratio of the nickel nitrate and copper nitrate is 1-9:1；
S3. it impregnates, the prepared nickel nitrate solutions of step S2 and copper nitrate solution is mixed with the step S1 carriers chosen, and
Persistently rock concussion 4-8h；
S4. it dries, filters off the maceration extract after step S3 dippings, the γ-Al that will be obtained2O3It is dried；
S5. it roasts, the γ-Al that step S4 is prepared2O3Sphere is with constant heating rate constant temperature calcining, calcination temperature
400-650 DEG C, soaking time 3-7h, product after roasting is the support type ozone high grade oxidation catalyst.
5. a kind of preparation method of support type ozone high grade oxidation catalyst according to claim 4, which is characterized in that step
S1, γ-Al2O3The output time is less than direct use in 2 months；It is dry at 90-150 DEG C more than 2 months.
6. a kind of preparation method of support type ozone high grade oxidation catalyst according to claim 4, which is characterized in that step
Concussion frequency is rocked described in S3：Preceding 2h is 15-30min/ times, and follow-up time is 30-60min/ times.
7. a kind of preparation method of support type ozone high grade oxidation catalyst according to claim 4, which is characterized in that step
Drying temperature described in S4 is 90-150 DEG C, drying time 4-7h, the γ-Al that step S4 is prepared2O3Sphere is placed in horse
Not roasted in stove.
8. a kind of preparation method of support type ozone high grade oxidation catalyst according to claim 4, which is characterized in that step
Heating rate described in S5 is 4-6 DEG C/min.
9. a kind of support type ozone high grade oxidation catalyst described in any one of claim 1-3 claims is for adsorbing in water
Organic pollution and catalytic activation ozone molecule.
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