CN108057433A - 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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- CN108057433A CN108057433A CN201711444510.8A CN201711444510A CN108057433A CN 108057433 A CN108057433 A CN 108057433A CN 201711444510 A CN201711444510 A CN 201711444510A CN 108057433 A CN108057433 A CN 108057433A
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- sepiolite
- ozone oxidation
- preparation
- catalyst
- oxidation catalyst
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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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- 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
-
- 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
-
- 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
-
- 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
-
- 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
Abstract
The present invention relates to a kind of preparation methods of ozone oxidation catalyst, comprise the following steps：Sepiolite sepiolite, active component with water are mixed, prepare the spherical pellet that grain size is 1 9mm；Wherein, active component is zinc oxide；By pellet, for 24 hours, then calcining and activating handles 2 5h at 450 550 DEG C, obtains the ozone oxidation catalyst using sepiolite as carrier for constant temperature processing 10 at 60 90 DEG C.The ozone oxidation catalyst using sepiolite as carrier used prepared by above-mentioned preparation method is also claimed in the present invention.The invention also discloses application of the above-mentioned ozone oxidation catalyst in ozone oxidation organic matter.The method of the present invention is simple, at low cost, and catalyst has good catalytic performance in ozone oxidation catalytic 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 technology
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 in into ozone oxidation sewerage.Catalyst plays an important role of that ozone, ozone quilt is catalytically decomposed
The stronger hydroxyl free of oxidation susceptibility is changed into, 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 from alternate diffusion influence, be easy to
Control, but the metal ion put into water is difficult to separate and cannot recycle, and can make underwater gold category ion concentration is excessively high to make
The paired secondary pollution of environment and the increase of operating cost.Different-phase catalyst can to avoid problem present in homogeneous catalyst,
But compared with homogeneous catalyst, there are alternate diffusional resistance, active sites in heterogeneous catalysis system to contact with reaction substrate
The low problem of rate.Therefore different-phase catalyst performance is improved, reduces the production cost of catalyst, simplifies scale production process, is
The essential condition of different-phase catalyst business application.
In addition, catalyst cost accounts for a maximum part for cost in catalytic ozonation treated sewage system, wastewater treatment
It generally requires that more fund is spent to buy catalyst in project, this is to the popularization of catalytic ozonation processing waste water technology
Bring very big obstruction.Therefore it is technical staff that the cost of catalyst how is reduced under conditions of catalyst performance is ensured
Need the major issue solved.Many researcher doors select cheap raw material such as：Fe2O3、MnO2Etc. producing 1-9mm's
Spheric catalyst, but catalyst catalytic performance is often relatively low, it is impossible to while satisfaction had not only reduced cost but also had ensured catalyst performance
Energy.And CuO, CeO2, etc. prices costly, this not only to production add larger economic pressures, also constrain ozone
Catalytic oxidation technologies are in the popularization of sewage treatment field.
The content 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, at low cost, and catalyst has good catalytic performance in ozone oxidation catalytic reaction.
The present invention provides a kind of preparation methods of ozone oxidation catalyst, comprise the following steps：
(1) sepiolite powder, active component with water are mixed, prepares the spherical pellet that grain size is 1-9mm；Wherein, activearm
It is divided into zinc oxide；Preferably, the grain 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 grain size of sepiolite powder is 200-325 mesh.Physico-chemical property is selected to stablize, machinery
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, in step (1), pelletized using round as a ball moulding process.Round as a ball moulding process, have it is quick,
The advantages of simple and easy amplification.
Further, in step (1), pelletized, comprised the following steps using spheronizator：By sepiolite powder, activity
Component is added in the disk of spheronizator, sprays into spray water as adhesive to form spherical pellet.
Further, the rotating 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 remain to after high-temperature activation to keep original pattern, preferable mechanical strength, it is common load in commercial catalysts
Body, wherein, content of MgO is 21~25wt%, and basic anhydride MgO and ozone have stronger interaction force, beneficial to ozone
Dissolving in water, and ozone decomposed can be promoted to generate the 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 in more mild 60-90 DEG C of temperature range of condition, can promote the hydration reaction of sepiolite and water, pass through sepiolite
Glue continuous cropping with obtaining the sample of mechanical strength bigger, and can make sample that preferable spherical morphology be kept not crack.It lives through high temperature
After change, absorption water, constitution water inside removing sepiolite ball, hole increases after water is removed inside sepiolite so that catalyst
Ball has higher specific surface area, obtains the catalyst granules of mechanical strength >=80N.
The present invention is also claimed using the 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：
Cheap and high catalytic performance zinc oxide is used as active component, using sepiolite as carrier, by a step it is round as a ball into
The technique of type quickly mass produces ozone catalytic oxidation catalyst.
The present invention solves the problems, such as that ozone oxidation catalyst cost input and catalytic performance are low in sewage disposal.Chemical industry is former
ZnO powder price is 20000 yuan/ton to material in the market, hence it is evident that less 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
It loads in system of the zinc oxide for organic matter in catalyst catalytic ozonation degrading waste water, solubility of the ozone in waste water
More than the system in other two kinds of catalyst；So as to reduce the concentration of ozone in exhaust gas, the utilization ratio of ozone is improved and to useless
The removal rate of Organic substance in water.
Above description is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be practiced according to the content of specification, below with presently preferred embodiments of the present invention and coordinate attached drawing be described in detail as after.
Description of the drawings
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, the specific embodiment of the present invention is described in further detail.Implement below
Example is not limited to the scope of the present invention for illustrating the present invention.
Embodiment 1
(1) by the sepiolite of 325 mesh and zinc oxide mixing, mixture is obtained, wherein, 4-10% mass is contained in mixture
The zinc oxide of percentage.Round as a ball shaping is carried out using spheronizator.The round as a ball disk of 1-3m is chosen, it is past with 100kg/h charging rates
Mixture is continuously added in the rounding disk of unlatching, while water is sprayed into rounding disk according to 50kg/L rates, it is to be obtained a diameter of
During 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, by controlling 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 form of example, as can be seen from the table
1 sample mechanical strength of example is all higher than 80N, and the sample for illustrating to prepare using the technique has preferable mechanical strength.
Table 1 is the mechanical strength tables of data of 1 sample of test case five times
Embodiment 2
(1) by the sepiolite of 200 mesh and zinc oxide mixing, mixture is obtained, wherein, 4-10% mass is contained in mixture
The zinc oxide of percentage.Round as a ball shaping is carried out using spheronizator.The round as a ball disk of 1-3m is chosen, it is past with 100kg/h charging rates
Mixture is continuously added in the rounding disk of unlatching, while suitable water is sprayed into rounding disk according to 50kg/L rates, it is to be obtained
During the bead of a diameter 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, by controlling 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) by the sepiolite of 325 mesh and zinc oxide mixing, mixture is obtained, wherein, 4-10% mass is contained in mixture
The zinc oxide of percentage.Round as a ball shaping is carried out using spheronizator.The round as a ball disk of 1-3m is chosen, it is past with 100kg/h charging rates
Be continuously added to mixture in the rounding disk of unlatching, at the same spray into rounding disk according to 50kg/L rates water be then sprayed into it is suitable
During the bead of water, a diameter of 1-3mm to be obtained 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, by controlling 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 as control, prepare catalyst using copper oxide as active component, be as follows：
(1) by the sepiolite of 325 mesh and copper oxide mixing, mixture is obtained, wherein, 4-10% mass is contained in mixture
The copper oxide of percentage.Round as a ball shaping is carried out using spheronizator.The round as a ball disk of 1-3m is chosen, it is past with 100kg/h charging rates
Be continuously added to mixture in the rounding disk of unlatching, at the same spray into rounding disk according to 50kg/L rates water be then sprayed into it is suitable
During the bead of water, a diameter of 3-5mm to be obtained 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, by controlling 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 as control, prepare catalyst using ceria as active component, be as follows：
(1) by the sepiolite of 325 mesh and ceria mixing, mixture is obtained, wherein, 4-10% matter is contained in mixture
Measure the ceria of percentage.Round as a ball shaping 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 spray into water into rounding disk according to 50kg/L rates and be then sprayed into
During the bead of suitable water, a diameter of 3-5mm to be obtained 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, by controlling 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
Catalyst prepared in embodiment 1,4,5 is used for catalytic ozonation degradation of phenol as the useless of simulating pollution object
In water, specific implementation step is as follows：
Phenol is selected to be used as simulating pollution object, phenol concentration 250ppm.Into the phenol solution configured respectively
Above-mentioned catalyst is added in, the wherein mass volume ratio of catalyst and aqueous solution is 10g:1L.Open magnetic agitation or mechanical agitation
Reaction to ensure reaction vessel interior uniformly occurs, and is passed through ozone, and the dosage of ozone and the ratio of waste water are 0.5g:1L.
Reaction time is 1h.The phenol concentration in solution under different time is measured, the results are 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 prepared by method using the present invention
Go out the catalyst with good catalytic, and reduce production cost.And sepiolite is carrier loaded zinc oxide object
Change property to stablize, be insoluble in water, greatly reduce the loss of catalyst, extend the service life of catalyst.
Embodiment 7
Catalyst prepared in embodiment 1,4,5 is degraded into sodium oxalate as simulating pollution object for catalytic ozonation
In waste water, specific implementation step is as follows：
Sodium oxalate is selected to be used as simulating pollution object, oxalic acid na concn is 1.2kg/L.Toward the sodium oxalate water solution configured
In be separately added into above-mentioned catalyst, wherein the mass volume ratio of catalyst and aqueous solution is 10g:1L.Open magnetic agitation or machine
Reaction of the tool stirring to ensure 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 in solution under different time is measured, the results are shown in Table 1, from table
In can be seen that, the catalyst of example 1 to the removal rate of COD in solution better than check experiment (embodiment 4 and 5), embodiment 1,4,
Catalyst in 5 is respectively 43.0%, 38.4%, 33.8% to the removal rate of COD, illustrates prepared by method using the present invention
Go out the catalyst with good catalytic.
2 catalyst of table COD concentration in the experiment of catalytic ozonation sodium oxalate changes with time data
The above is only the preferred embodiment of the present invention, is not intended to limit 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 (10)
1. a kind of preparation method of ozone oxidation catalyst, which is characterized in that comprise the following steps：
(1) sepiolite, active component with water are mixed, prepares the spherical pellet that grain size is 1-9mm；Wherein, the active component
For zinc oxide；
(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), the grain size of sepiolite is 200-
325 mesh.
3. preparation method according to claim 1, it is characterised in that：In step (1), the sepiolite and zinc oxide
Mass ratio is 90-96:4-10.
4. preparation method according to claim 1, it is characterised in that：In step (1), the quality of the sepiolite and water
Than for 1.5-2.5：1.
5. preparation method according to claim 1, it is characterised in that：In step (1), carried out using round as a ball moulding process
Granulation.
6. preparation method according to claim 5, it is characterised in that：In step (1), pelletized using spheronizator,
Comprise the following steps：The sepiolite, active component are added in the disk of spheronizator, spray into spray water as adhesive with shape
The pellet of globulate.
7. preparation method according to claim 6, it is characterised in that：The rotating speed of the disk of the spheronizator is 20-
60rpm。
8. a kind of ozone oxidation catalyst prepared by preparation method according to any one of claim 1-7.
9. application of the ozone oxidation catalyst according to claim 8 in catalytic ozonation organic matter.
10. application according to claim 9, 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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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108906054A (en) * | 2018-07-21 | 2018-11-30 | 山东理工大学 | A kind of forming method using Fenton iron cement preparation ozone oxidation nbsCOD catalyst |
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