CN108057433B - A kind of ozone oxidation catalyst and its preparation method and application - Google Patents
A kind of ozone oxidation catalyst and its preparation method and application Download PDFInfo
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- CN108057433B CN108057433B CN201711444510.8A CN201711444510A CN108057433B CN 108057433 B CN108057433 B CN 108057433B CN 201711444510 A CN201711444510 A CN 201711444510A CN 108057433 B CN108057433 B CN 108057433B
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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
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
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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
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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
- C02F2101/32—Hydrocarbons, e.g. oil
- C02F2101/322—Volatile compounds, e.g. benzene
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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
- C02F2101/34—Organic compounds containing oxygen
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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
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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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
- C02F2101/38—Organic compounds containing nitrogen
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- Hydrology & Water Resources (AREA)
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Abstract
The present invention relates to a kind of preparation methods of ozone oxidation catalyst, comprising the following steps: mixes sepiolite sepiolite, active component with water, prepares the spherical pellet that partial size is 1-9mm；Wherein, active component is zinc oxide；By pellet, constant temperature handles 10-24h at 60-90 DEG C, and then calcining and activating handles 2-5h at 450-550 DEG C, obtains the ozone oxidation catalyst using sepiolite as carrier.The present invention, which is also claimed, to be used prepared by above-mentioned preparation method using sepiolite as the ozone oxidation catalyst of carrier.The invention also discloses application of the above-mentioned ozone oxidation catalyst in ozone oxidation organic matter.Method of the invention is simple, at low cost, and catalyst has good catalytic performance in ozone oxidation catalysis reaction.
Description
Technical field
The present invention relates to catalyst preparation technical field and sewage treatment field more particularly to a kind of ozone oxidation catalysts
And its preparation method and application.
Background technique
Ozone has extremely strong oxidability, can be with direct oxidation degradation of organic substances, but its oxidation selectivity constrains
To the ability of dirty Organic substance in water depth mineralising processing.In order to improve the ability of ozone utilization rate and deeply treating wastewater, generally
Using the method that catalyst is added into ozone oxidation sewerage.Catalyst has the function of that ozone, ozone quilt is catalytically decomposed
It is converted to the stronger hydroxyl free of oxidation susceptibility, hydroxyl radical free radical can substantially aoxidize all organic matters, have depth
Manage the ability of sewage.
Currently used catalyst is divided into homogeneous and two class of out-phase.Homogeneous catalyst is not influenced by alternate diffusion, is easy to
Control, but the metal ion put into water is difficult to separate and cannot be recycled, and can make underwater gold category ion concentration is excessively high to make
The pairs of secondary pollution of environment and the increase of operating cost.The problem of different-phase catalyst can be to avoid homogeneous catalyst,
But compared with homogeneous catalyst, there are alternate diffusional resistance, active sites in heterogeneous catalysis system contacts with reaction substrate
The problems such as rate is low.Therefore different-phase catalyst performance is improved, the production cost of catalyst is reduced, simplifies scale production process, is
The essential condition of different-phase catalyst business application.
In addition, catalyst cost accounts for maximum a part of cost in catalytic ozonation processing sewage system, wastewater treatment
It generally requires that more fund is spent to buy catalyst in project, this handles the popularization of waste water technology to catalytic ozonation
Bring very big obstruction.Therefore the cost of catalyst how is reduced under conditions of guaranteeing catalyst performance is technical staff
The major issue for needing to solve.Many researcher doors select cheap raw material such as: Fe2O3、MnO2Etc. producing 1-9mm's
Spheric catalyst, but catalyst catalytic performance is often lower, cannot meet simultaneously not only reduces cost but also guarantees catalyst performance
Energy.And CuO, CeO2, etc. prices costly, this not only increases biggish economic pressures to production, also constrains ozone
Popularization of the catalytic oxidation technologies in sewage treatment field.
Summary of the invention
In order to solve the above technical problems, the object of the present invention is to provide a kind of ozone oxidation catalyst and preparation method thereof and
Using method of the invention is simple, and at low cost, catalyst has good catalytic performance in ozone oxidation catalysis reaction.
The present invention provides a kind of preparation methods of ozone oxidation catalyst, comprising the following steps:
(1) sepiolite powder, active component are mixed with water, prepares the spherical pellet that partial size is 1-9mm；Wherein, active group
It is divided into zinc oxide；Preferably, the partial size of spherical pellet is 3-5mm；
(2) by pellet, constant temperature handles 10-24h at 60-90 DEG C, and then calcining and activating handles 2-5h at 450-550 DEG C,
Obtain the ozone oxidation catalyst using sepiolite as carrier.
Further, in step (1), the partial size of sepiolite powder is 200-325 mesh.Physico-chemical property is selected to stablize, it is mechanical
Intensity is big, and easily molded sepiolite powder is carrier.
Further, in step (1), the mass ratio of sepiolite powder and active component is 90-96:4-10.
Further, in step (1), the mass ratio of sepiolite powder and water is 1.5-2.5:1.
Further, it in step (1), is pelletized using round as a ball moulding process.Round as a ball moulding process, have quickly,
The advantages of simple and easy amplification.
Further, it in step (1), is pelletized using spheronizator, comprising the following steps: by sepiolite powder, activity
Component is added in the disk of spheronizator, sprays into spray water and forms spherical pellet as adhesive.
Further, the revolving speed of the disk of spheronizator is 20-60rpm.
Sepiolite have it is cheap easily obtain, nontoxic, physico-chemical property is stable, grain diameter is small, good hydrophilic property, easily molded etc. excellent
Point, and original pattern, preferable mechanical strength are still able to maintain after high-temperature activation, it is commonly to be carried in commercial catalysts
Body, wherein content of MgO is 21~25wt%, and basic anhydride MgO and ozone have stronger interaction force, is conducive to ozone
Dissolution in water, and can promote ozone and decompose the generation stronger hydroxyl radical free radical of oxidation.
Step (2) is to confer to the pass of the certain mechanical strength of catalyst in more mild 60-90 DEG C of temperature range of condition
Key can promote the hydration reaction of sepiolite and water, pass through sepiolite in more mild 60-90 DEG C of temperature range of condition
Glue connection act on obtaining the bigger sample of mechanical strength, and can make sample that preferable spherical morphology be kept not crack.It is living through high temperature
After change, water, constitution water are adsorbed inside removing sepiolite ball, hole increases after water is removed inside sepiolite, so that catalyst
Ball specific surface area with higher obtains mechanical strength >=80N catalyst granules.
The present invention is also claimed using ozone oxidation catalyst prepared by above-mentioned preparation method.
The invention also discloses application of the above-mentioned ozone oxidation catalyst in catalytic ozonation organic matter.
Further, organic matter is phenol, to one in biphenol, benzoquinones, tetranitro-phenol, benzene, toluene and sodium oxalate
Kind is several.
Further, in application, the dosage of ozone is 0.2-1.2g/L, the dosage of catalyst is 5-15g/L.
According to the above aspect of the present invention, the present invention has at least the following advantages:
Use cheap and high catalytic performance zinc oxide for active component, using sepiolite as carrier, by a step it is round as a ball at
Ozone catalytic oxidation catalyst is quickly mass produced in the technique of type.
The present invention solves the problems, such as that ozone oxidation catalyst cost input and catalytic performance are low in sewage treatment.Chemical industry is former
ZnO powder price is 20000 yuan/ton to material in the market, hence it is evident that lower than common production ozone catalytic oxidation catalyst active component CuO
(40000 yuan/ton), CeO2Etc. prices (40000 yuan/ton).The interaction of ZnO and ozone are better than CuO and CeO2, in sepiolite
Loading zinc oxide is solubility of the ozone in waste water in catalyst catalytic ozonation degrading waste water in the system of organic matter
Greater than the system in other two kinds of catalyst；To reduce the concentration of ozone in exhaust gas, the utilization efficiency of ozone is improved and to useless
The removal rate of Organic substance in water.
The above description is only an overview of the technical scheme of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, the following is a detailed description of the preferred embodiments of the present invention and the accompanying drawings.
Detailed description of the invention
Fig. 1 is the optical photograph of ozone oxidation catalyst prepared by embodiment 1；
Fig. 2 is the X-ray diffraction spectrogram of ozone oxidation catalyst prepared by embodiment 1；
Fig. 3 is different catalysts phenol concentration versus time curve in the experiment of catalytic ozonation phenol.
Specific embodiment
With reference to the accompanying drawings and examples, specific embodiments of the present invention will be described in further detail.Implement below
Example is not intended to limit the scope of the invention for illustrating the present invention.
Embodiment 1
(1) sepiolite of 325 mesh and zinc oxide are mixed, obtains mixture, wherein contain 4-10% mass in mixture
The zinc oxide of percentage.Round as a ball molding is carried out using spheronizator.The round as a ball disk of 1-3m is chosen, it is past with 100kg/h charging rate
It is continuously added to mixture in the rounding disk of unlatching, while spraying into water into rounding disk according to 50kg/L rate, diameter to be obtained is
When the bead of 1-9mm or so, taking-up is spare, obtains required pellet.
(2) pellet gathered is placed in closed system, and constant temperature is handled for 24 hours at 90 DEG C.
(3) by step (2), treated that pellet is added continuously in vertical kiln, passes through control furnace bottom discharging speed, adjusts
Material-saving ball stops 3h in 450 DEG C of regions of kiln constant temperature, obtains ozone oxidation catalyst.
Fig. 1,2 are optical photograph, the X-ray diffraction spectrogram of ozone oxidation catalyst prepared by embodiment 1 respectively, as a result table
Bright, 1 sample of embodiment is ZnO and sepiolite, and table 1 is 1 sample machinery intensity data table of example, as can be seen from the table
1 sample mechanical strength of example is all larger than 80N, illustrates there is preferable mechanical strength using the sample of technique preparation.
Table 1 is 1 sample of test case five times mechanical strength tables of data
Embodiment 2
(1) sepiolite of 200 mesh and zinc oxide are mixed, obtains mixture, wherein contain 4-10% mass in mixture
The zinc oxide of percentage.Round as a ball molding is carried out using spheronizator.The round as a ball disk of 1-3m is chosen, it is past with 100kg/h charging rate
It is continuously added to mixture in the rounding disk of unlatching, while spraying into suitable water into rounding disk according to 50kg/L rate, it is to be obtained
When diameter is the bead of 6-9mm or so, taking-up is spare, obtains required pellet.
(2) pellet gathered is placed in closed system, and constant temperature is handled for 24 hours at 60 DEG C.
(3) by step (2), treated that pellet is added continuously in vertical kiln, passes through control furnace bottom discharging speed, adjusts
Material-saving ball stops 3h in 500 DEG C of regions of kiln constant temperature, obtains ozone oxidation catalyst.
Embodiment 3
(1) sepiolite of 325 mesh and zinc oxide are mixed, obtains mixture, wherein contain 4-10% mass in mixture
The zinc oxide of percentage.Round as a ball molding is carried out using spheronizator.The round as a ball disk of 1-3m is chosen, it is past with 100kg/h charging rate
Mixture is continuously added in the rounding disk of unlatching, at the same sprayed into rounding disk according to 50kg/L rate water be then sprayed into it is suitable
Water, when diameter to be obtained is the bead of 1-3mm or so, taking-up is spare, obtains required pellet.
(2) pellet gathered is placed in closed system, and constant temperature is handled for 24 hours at 90 DEG C.
(3) by step (2), treated that pellet is added continuously in vertical kiln, passes through control furnace bottom discharging speed, adjusts
Material-saving ball stops 3h in 550 DEG C of regions of kiln constant temperature, obtains ozone oxidation catalyst.
Embodiment 4
In order to prepare catalyst using copper oxide as active component as control, the specific steps are as follows:
(1) sepiolite of 325 mesh and copper oxide are mixed, obtains mixture, wherein contain 4-10% mass in mixture
The copper oxide of percentage.Round as a ball molding is carried out using spheronizator.The round as a ball disk of 1-3m is chosen, it is past with 100kg/h charging rate
Mixture is continuously added in the rounding disk of unlatching, at the same sprayed into rounding disk according to 50kg/L rate water be then sprayed into it is suitable
Water, when diameter to be obtained is the bead of 3-5mm or so, taking-up is spare, obtains required pellet.
(2) pellet gathered is placed in closed system, and constant temperature is handled for 24 hours at 90 DEG C.
(3) by step (2), treated that pellet is added continuously in vertical kiln, passes through control furnace bottom discharging speed, adjusts
Material-saving ball stops 3h in 450 DEG C of regions of kiln constant temperature, obtains ozone oxidation catalyst.
Embodiment 5
In order to prepare catalyst using ceria as active component as control, the specific steps are as follows:
(1) sepiolite of 325 mesh and ceria are mixed, obtains mixture, wherein contain 4-10% matter in mixture
Measure the ceria of percentage.Round as a ball molding is carried out using spheronizator.The round as a ball disk of 1-3m is chosen, is fed with 100kg/h fast
It spends and is continuously added to mixture into the rounding disk opened, while spraying into water into rounding disk according to 50kg/L rate and being then sprayed into
Suitable water, when diameter to be obtained is the bead of 3-5mm or so, taking-up is spare, obtains required pellet.
(2) pellet gathered is placed in closed system, and constant temperature is handled for 24 hours at 90 DEG C.
(3) by step (2), treated that pellet is added continuously in vertical kiln, passes through control furnace bottom discharging speed, adjusts
Material-saving ball stops 3h in 450 DEG C of regions of kiln constant temperature, obtains ozone oxidation catalyst.
Embodiment 6
It is the useless of simulating pollution object that catalyst prepared in embodiment 1,4,5, which is used for catalytic ozonation degradation of phenol,
In water, specific implementation step is as follows:
Select phenol as simulating pollution object, phenol concentration 250ppm.Respectively into configured phenol solution
Above-mentioned catalyst is added, wherein the mass volume ratio of catalyst and aqueous solution is 10g:1L.Open magnetic agitation or mechanical stirring
Guarantee that the reaction of reaction vessel interior uniformly occurs, is passed through ozone, the dosage of ozone and the ratio of waste water are 0.5g:1L.
Reaction time is 1h.The phenol concentration under different time in solution is measured, as a result as shown in figure 3, it is seen that implementing
The removal rate and removal speed of the catalyst Pyrogentisinic Acid of example 1 is substantially better than control experiment (embodiment 4 and 5), embodiment 1,4,5
In the removal rate of catalyst Pyrogentisinic Acid be respectively 88.0%, 79.1%, 72%, illustrate to prepare using method of the invention
The catalyst of good catalytic is provided, and reduces production cost.And sepiolite is carrier loaded zinc oxide object
Change property to stablize, is insoluble in water, greatly reduces the loss of catalyst, extend the service life of catalyst.
Embodiment 7
It is simulating pollution object that catalyst prepared in embodiment 1,4,5, which is used for catalytic ozonation degradation sodium oxalate,
In waste water, specific implementation step is as follows:
Select sodium oxalate as simulating pollution object, oxalic acid na concn is 1.2kg/L.Toward configured sodium oxalate water solution
In be separately added into above-mentioned catalyst, wherein the mass volume ratio of catalyst and aqueous solution be 10g:1L.Open magnetic agitation or machine
Tool stirs to guarantee that the reaction of reaction vessel interior uniformly occurs, and is passed through ozone, the dosage of ozone and the ratio of waste water are
0.65kg:1L.Reaction time is 120min.The COD concentration under different time in solution is measured, the results are shown in Table 1, from table
In can be seen that, the catalyst of example 1 is better than check experiment (embodiment 4 and 5) to the removal rate of COD in solution, embodiment 1,4,
Catalyst in 5 is respectively 43.0%, 38.4%, 33.8% to the removal rate of COD, illustrates to prepare using method of the invention
Provide the catalyst of good catalytic.
2 catalyst of table COD concentration in the experiment of catalytic ozonation sodium oxalate changes with time data
The above is only a preferred embodiment of the present invention, it is not intended to restrict the invention, it is noted that for this skill
For the those of ordinary skill in art field, without departing from the technical principles of the invention, can also make it is several improvement and
Modification, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (7)
1. a kind of preparation method of ozone oxidation catalyst, which comprises the following steps:
(1) sepiolite, active component are mixed with water, prepares the spherical pellet that partial size is 1-9mm；Wherein, the active component
For zinc oxide；The partial size of the sepiolite is 200-325 mesh；The mass ratio of the sepiolite and zinc oxide is 90-96:4-10；
The mass ratio of the sepiolite and water is 1.5-2.5:1；
(2) by the pellet, constant temperature handles 10-24h at 60-90 DEG C, and then calcining and activating handles 2-5h at 450-550 DEG C,
Obtain the ozone oxidation catalyst.
2. preparation method according to claim 1, it is characterised in that: in step (1), carried out using round as a ball moulding process
Granulation.
3. preparation method according to claim 2, it is characterised in that: in step (1), pelletized using spheronizator,
The following steps are included: the sepiolite, active component are added in the disk of spheronizator, spray water is sprayed into as adhesive with shape
At spherical pellet.
4. preparation method according to claim 3, it is characterised in that: the revolving speed of the disk of the spheronizator is 20-
60rpm。
5. ozone oxidation catalyst prepared by a kind of preparation method described in any one of -4 according to claim 1.
6. application of the ozone oxidation catalyst according to claim 5 in catalytic ozonation organic matter.
7. application according to claim 6, it is characterised in that: the organic matter is phenol, to biphenol, benzoquinones, four nitre
One or more of base phenol, benzene, toluene and sodium oxalate.
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| JP2001276194A (en) * | 2000-03-30 | 2001-10-09 | Toto Ltd | Deodorizing catalyst material |
| CN101885533A (en) * | 2010-07-19 | 2010-11-17 | 江南大学 | Ozonized water treatment method taking nano zinc oxide as catalyst |
| CN105080551A (en) * | 2014-05-06 | 2015-11-25 | 李小琴 | Efficient spherical particle ozonation catalyst and preparation method therefor |
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|---|---|---|---|---|
| JP2001276194A (en) * | 2000-03-30 | 2001-10-09 | Toto Ltd | Deodorizing catalyst material |
| CN101885533A (en) * | 2010-07-19 | 2010-11-17 | 江南大学 | Ozonized water treatment method taking nano zinc oxide as catalyst |
| CN105080551A (en) * | 2014-05-06 | 2015-11-25 | 李小琴 | Efficient spherical particle ozonation catalyst and preparation method therefor |
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| Title |
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| ZnO/clay nanoarchitectures: synthesis, characterization and evaluation as photocatalysts;M.Akkari等;《Applied Clay Science》;20151220;第131卷;第131-139页 * |
| 氧化锌纳米颗粒的简便合成及其臭氧化降解苯酚的催化性质;董玉明 等;《水处理技术》;20120831;第38卷(第8期);全文 * |
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