CN106964349A - Ozone catalytic oxidation catalyst, its preparation method and application - Google Patents
Ozone catalytic oxidation catalyst, its preparation method and application Download PDFInfo
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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
- B01J23/745—Iron
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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
- B01J37/0205—Impregnation in several steps
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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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- 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
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/088—Decomposition of a metal salt
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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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- 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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/343—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the pharmaceutical industry, e.g. containing antibiotics
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a kind of preparation method of ozone catalytic oxidation catalyst, the preparation method of the catalyst comprises the following steps：A, the γ Al by a diameter of 3mm 5mm2O3Cleaned, dried with deionized water, high-temperature roasting must pre-process γ Al2O3；B, will pretreatment γ Al2O33 6h are impregnated in NaOH solution, filtering is taken out, is washed with distilled water to PH and no longer changes, in 100 120 DEG C of drying in oven, then it is immersed in again in ferric nitrate and copper nitrate mixed solution, the concentration of ferric nitrate and copper nitrate mixed solution is 0.75 1.25mol/L, obtains catalyst precursors；C, catalyst precursors are dried, high-temperature roasting obtains ozone catalytic oxidation catalyst.The preparation technology of ozone catalytic oxidation catalyst of the present invention is simple, and cost is low, it is easy to large-scale industrial production.The ozone catalytic oxidation catalyst that method produced according to the present invention is obtained is applied to processing antibiotic industrial waste water.
Description
Technical field
The invention belongs to water treatment field, specifically, it is related to a kind of preparation method of ozone catalytic oxidation catalyst, together
When the invention further relates to the catalyst obtained with the preparation method and the catalyst in processing antibiotic industrial waste water
Using.
Background technology
At present, discharged volume of industrial waste water increasingly increases, and complicated component, and huge harm is caused to environment and the mankind,
Antibiotic waste water is one of generally acknowledged pollution sources, and organic matter ammonia nitrogen and sulfate isoconcentration are high in antibiotic production wastewater, and contain
There is the Biostatic material such as antibiotic, waste component is complicated, and biodegradability is poor, salinity is high, toxicity is big, COD (chemical oxygen demands
Amount) high, colourity depth, greatly, wastewater treatment difficulty is big, and traditional secondary biochemical treatment has been difficult to meet for the pH value amount fluctuation of waste water
New discharge standard requirement, thus high-level oxidation technology arises at the historic moment, and is developed rapidly.
Ozone has strong oxidizing property, organic matter that can be in direct oxidation water, secondary pollution is not produced, in Water purification neck
Domain has a wide range of applications.But also there are many problems, ozone is unstable in water, and mass-transfer efficiency is low, cause the reality of ozone
Utilization rate is not high, adds processing cost, and ozone oxidation selectivity is high, and the reaction rate to some organic pollutions is low, goes
Except rate is low, salinity is low, influences its industrial application.O3 catalytic oxidation be produced using ozone under catalyst action it is more
Intermediate product such as hydroxyl radical free radical (OH) the oxidation Decomposition organic pollutants for having Strong oxdiative ability, these intermediate products
Oxidability is extremely strong, react non-selectivity, can Quick Oxidation ozone decomposition can not aoxidize high stability, difficult degradation it is organic
Thing, the technology is novel ozone oxidized method developed in recent years.
Different according to catalyst form, O3 catalytic oxidation is broadly divided into two classes：Homogeneous catalysis ozone oxidation and heterogeneous
O3 catalytic oxidation.Heterogeneous catalytic ozonation technology produces the higher hydroxyl radical free radical of oxidisability using various catalyst,
Larger molecular organicses in water can be decomposed into small-molecule substance, or even be mineralized into CO2And H2O.The technology can not only be realized and urged
The separation of agent and waste water, and catalyst can multiple Reusability, reduce cost.The catalyst developed at present has technique
Complexity, stability is poor, the low shortcoming for the treatment of effeciency, limits the development of the technology.
The content of the invention
It is an object of the invention to provide a kind of preparation method of ozone catalytic oxidation catalyst.
A kind of preparation method of ozone catalytic oxidation catalyst, comprises the following steps：
A, the γ-Al by a diameter of 3mm-5mm2O3Cleaned with deionized water, dry, high-temperature roasting, must pre-process γ-
Al2O3；
B, will pretreatment γ-Al2O33-6h is impregnated in NaOH solution, filtering is taken out, is washed with distilled water to PH and no longer sends out
Changing, in 100-120 DEG C of drying in oven, is then immersed in ferric nitrate and copper nitrate mixed solution, ferric nitrate and nitre again
The concentration of sour copper mixed solution is 0.75-1.25mol/L, obtains catalyst precursors；
C, catalyst precursors are dried, high-temperature roasting obtains ozone catalytic oxidation catalyst.
Further, the Drying Technology Parameter in step a is：1-2h, high-temperature roasting technique are dried in 100-120 DEG C of baking oven
Parameter is：500-700 DEG C of Muffle kiln roasting 4-7h.
Further, the amount ratio of the material of ferric nitrate and copper nitrate is 0.5~1 in step b.
Further, γ-Al are pre-processed in step b2O3Ratio with mixed solution is 10-30g：300mL.
Further, γ-Al are pre-processed in step b2O3The time being immersed in mixed solution is 12-24h.
Further, the Drying Technology Parameter in step c is：1-2h, high-temperature roasting technique are dried in 100-120 DEG C of baking oven
Parameter is：500-700 DEG C of Muffle kiln roasting 4-7h.
The preparation method of ozone catalytic oxidation catalyst of the present invention has the advantages that：
1st, the preparation technology of ozone catalytic oxidation catalyst of the present invention is simple, and cost is low, it is easy to large-scale industrial production, choosing
With diameter 3mm-5mm γ-Al2O3It is used as carrier, γ-Al2O3There is the ability of certain O3 catalytic oxidation, waste water simultaneously
COD removal effects are good, and the 3mm-5mm selected γ-Al2O3It can reclaim and use, save cost recovery.
2nd, will pretreatment γ-Al2O33-6h is impregnated in NaOH aqueous slkalis, catalyst surface increase there are more alkalescence
Group, basic group has the ability for promoting ozone to produce hydroxyl radical free radical.
3rd, after the ferric nitrate and copper nitrate mixed solution after step b dippings are by filtering, filtrate subsequently adds solute to finger
Determine reusable after concentration, saved cost.
4th, load two kinds of metal active compositions of iron oxide and cupric oxide, easily occur electronics transmittance process, with compared with
High redox catalytic activity, promotes ozone decomposed, the hydroxyl radical free radical with extremely strong oxidisability is produced, so as to significantly carry
The high discomposing effect to Organic substance in water, the catalyst prepared is reusable, and catalytic activity is stable.
5th, the high-temperature roasting technological parameter in step a, c of the present invention is：500-700 DEG C of Muffle kiln roasting 4-7h；Through height
Volatile component is removed in temperature roasting, retains certain chemical composition, catalyst is had stable catalytic performance.In addition, step
In rapid c when sintering temperature is low, nitrate is decomposed into fine oxide crystal grain not exclusively, improves temperature and is conducive to decomposing during roasting
The progress of reaction, but temperature is too high can cause the sintering of crystal grain, and specific surface area of catalyst is reduced, catalyst activity reduction, this hair
The sintering temperature of bright 500-700 DEG C of selection.
6th, the amount ratio of the material of ferric nitrate and copper nitrate of the present invention is 0.5~1, and catalyst has more preferable catalytic activity,
And catalyst is reusable, performance is more stable.
The quality of the ozone catalytic oxidation catalyst carried metal obtained according to above-mentioned preparation method is 5%-10%.
Catalyst prepared by the inventive method is reusable, and metal ion amount of precipitation is extremely low, and catalytic activity is stable, has
Higher stability and repetition applicability.
The ozone catalytic oxidation catalyst obtained according to above-mentioned preparation method is applied to processing antibiotic industrial waste water.
Further, the dosage that the catalyst is applied to processing antibiotic industrial waste water is 7-10g/L.
Further, ozone volume flow is 1.5-2.5L/min, and ozone concentration is 55.3mg/L, and the reaction time is 0.5-
1.5h。
Ozone catalytic oxidation catalyst prepared by the present invention be applied to processing antibiotic industrial waste water, the catalyst of preparation with
Ozone molecule is cooperateed with, and produces the extremely strong hydroxyl radical free radical of oxidisability, being capable of fast degradation organic matter, raising COD clearances, reaction
Residence time is short, significantly reduces the operating cost of ozone, non-secondary pollution.
Embodiment
The invention discloses a kind of preparation method of ozone catalytic oxidation catalyst, comprise the following steps：
A, the γ-Al by a diameter of dmm2O3Cleaned with deionized water, in being dried in 105 DEG C of baking ovens after 1h, in temperature t1℃
Roasting 5h in Muffle furnace, taking-up is cooled to room temperature, must pre-process γ-Al2O3；
B, will pretreatment γ-Al2O34h is impregnated in the 1mol/L NaOH aqueous solution, filtering is taken out, is washed with distilled water to
PH no longer changes, and in 105 DEG C of drying in oven, is then immersed in again in ferric nitrate and copper nitrate mixed solution, ferric nitrate
Amount ratio with the material of copper nitrate is n1, the concentration of ferric nitrate and copper nitrate mixed solution is C1Mol/L, pretreatment γ-Al2O3
Ratio with mixed solution is n2, dip time is T, obtains catalyst precursors；
C, by catalyst precursors in 105 DEG C of baking ovens dry 1h after, in t2Roasting 5h, obtains ozone catalytic in Muffle furnace
Oxidation catalyst.
Embodiment 1-5：
According to the preparation method of above-mentioned ozone catalytic oxidation catalyst, each process parameters of embodiment 1-5 such as table 1 below institute
Show：
The process parameter table of table 1
Comparative example 1-14 have studied kind of carrier, mixed solution species and concentration, the influence of sintering temperature, each variable technique
Parameter value is as shown in following table 2-4, and its preparation method and other technological parameters are same as Example 3.
Comparative example 1-4：
The influence of the kind of carrier of table 2
Comparative example 5-10：
The influence of the mixed solution species of table 3 and concentration
Comparative example 11-14：
The influence of the sintering temperature of table 4
The quality of the carried metal of ozone catalytic oxidation catalyst prepared by above-described embodiment 1-5, comparative example 1-14 is calculated,
And the ozone catalytic oxidation catalyst for obtaining above-mentioned preparation method is applied to handle following antibiotic industrial waste water：1. normal two
The biochemical antibiotic industrial waste water I of level, waste water COD concentration is 800mg/L, PH=7, belongs to the industrial wastewater compared with difficult degradation；2. it is non-
Normal secondary biochemical antibiotic industrial waste water II, the waste water COD concentration is 1500mg/L, than normal secondary biochemical antibiotic waste water
More difficult degradation.Catalytic ozonation technical parameter：The dosage of catalyst is 10g/L, and ozone volume flow is 2.5L/min, smelly
Oxygen concentration is 55.3mg/L, and the reaction time is 1.5h, tests antibiotic industrial waste water COD clearances, experimental result such as table 5-8 institutes
Show.
The catalyst activity test data table of table 5
| Embodiment | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| The quality (%) of carried metal | 5 | 8 | 10 | 7 | 9 |
| COD clearances (waste water I) | 72.0% | 73.1% | 76.2% | 74.2% | 73.6% |
| COD clearances (waste water II) | 51.2% | 52.1% | 52.9% | 51.1% | 52.6% |
Influence tables of data of the kind of carrier of table 6 to catalyst activity
| Comparative example | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 |
| The quality (%) of carried metal | 9 | 6 | 5 | 7 |
| COD clearances (waste water I) | 61.5% | 60.2% | 67.5% | 64.2% |
| COD clearances (waste water II) | 45.1% | 48.6% | 40.0% | 46.7% |
The influence tables of data of the mixed solution species of table 7 and concentration to catalyst activity
Influence tables of data of the sintering temperature of table 8 to catalyst activity
| Comparative example | Comparative example 11 | Comparative example 12 | Comparative example 13 | Comparative example 14 |
| The quality (%) of carried metal | 6 | 6 | 5 | 7 |
| COD clearances (waste water I) | 69.5% | 66.2% | 68.2% | 69.9% |
| COD clearances (waste water II) | 51.0% | 48.2% | 47.9% | 50.1% |
Blank assay is set, catalyst is not put into, ozone volume flow, ozone concentration, reaction time technical parameter with it is upper
State that test data is identical, its COD clearance for handling normal secondary biochemical antibiotic industrial waste water I is 34.1%, and its processing is non-
The COD clearances of normal secondary biochemical antibiotic industrial waste water II are 19.2%, and the catalytic oxidation activity that ozone is used alone is remote
The ozone catalytic oxidation catalyst prepared far below the present invention.
Ozone catalytic oxidation catalyst prepared by above-described embodiment 1-5 is applied to handle improper secondary biochemical antibiotic
Industrial wastewater II, and test reuse ten times after iron ion and copper ion stripping quantity, the stability of catalyst testing.
The catalyst metal ion stripping quantity tables of data of table 9
As can be seen from Table 9, ozone catalytic oxidation catalyst handles improper secondary biochemical antibiotic industrial waste water II, the
First use and after reusing ten times, iron ion and copper ion stripping quantity≤0.7%, show preferable stability.
Claims (10)
1. a kind of preparation method of ozone catalytic oxidation catalyst, it is characterised in that the preparation method of the catalyst include with
Lower step：
A, the γ-Al by a diameter of 3mm-5mm2O3Cleaned, dried with deionized water, high-temperature roasting must pre-process γ-Al2O3；
B, will pretreatment γ-Al2O33-6h is impregnated in NaOH solution, filtering is taken out, is washed with distilled water to PH and no longer becomes
Change, in 100-120 DEG C of drying in oven, be then immersed in again in ferric nitrate and copper nitrate mixed solution, ferric nitrate and copper nitrate
The concentration of mixed solution is 0.75-1.25mol/L, obtains catalyst precursors；
C, catalyst precursors are dried, high-temperature roasting obtains ozone catalytic oxidation catalyst.
2. the preparation method of ozone catalytic oxidation catalyst according to claim 1, it is characterised in that dry in step a
Drying process parameter is：1-2h is dried in 100-120 DEG C of baking oven, high-temperature roasting technological parameter is：500-700 DEG C of Muffle kiln roasting
4-7h。
3. the preparation method of ozone catalytic oxidation catalyst according to claim 1, it is characterised in that nitric acid in step b
The amount ratio of the material of iron and copper nitrate is 0.5~1.
4. the preparation method of ozone catalytic oxidation catalyst according to claim 1, it is characterised in that locate in advance in step b
Manage γ-Al2O3Ratio with mixed solution is 10-30g：300mL.
5. the preparation method of ozone catalytic oxidation catalyst according to claim 4, it is characterised in that locate in advance in step b
Manage γ-Al2O3The time being immersed in mixed solution is 12-24h.
6. the preparation method of ozone catalytic oxidation catalyst according to claim 1, it is characterised in that dry in step c
Drying process parameter is：1-2h is dried in 100-120 DEG C of baking oven, high-temperature roasting technological parameter is：500-700 DEG C of Muffle kiln roasting
4-7h。
7. the ozone catalytic oxidation catalyst that the preparation method according to any one of claim 1-6 is obtained, its feature exists
In the quality of the ozone catalytic oxidation catalyst carried metal is 5%-10%.
8. a kind of application of ozone catalytic oxidation catalyst as described in claim 7, it is characterised in that the catalyst should
For handling antibiotic industrial waste water.
9. the application of ozone catalytic oxidation catalyst according to claim 8, it is characterised in that the catalyst is applied to
The dosage for handling antibiotic industrial waste water is 7-10g/L.
10. the application of ozone catalytic oxidation catalyst according to claim 9, it is characterised in that ozone volume flow is
1.5-2.5L/min, ozone concentration is 55.3mg/L, and the reaction time is 0.5-1.5h.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108404913A (en) * | 2018-01-24 | 2018-08-17 | 大连理工大学 | A method of preparing the ozone catalyst for removing water removal moderate resistance life element using cheap material as carrier |
| CN110052269A (en) * | 2019-05-08 | 2019-07-26 | 科盛环保科技股份有限公司 | A kind of preparation method of depth-averaged model ozone catalytic oxidation catalyst |
| CN110052268A (en) * | 2019-05-22 | 2019-07-26 | 四川恒泰环境技术有限责任公司 | A kind of ozone catalytic oxidation catalyst and preparation method thereof |
| CN110270329A (en) * | 2019-06-18 | 2019-09-24 | 北京首创股份有限公司 | For handling the ozone catalyst and preparation method thereof of hardly degraded organic substance in water |
| CN111153487A (en) * | 2020-01-08 | 2020-05-15 | 杭州天创环境科技股份有限公司 | Method for efficiently removing refractory organic matters in clean sewage |
| CN111804300A (en) * | 2020-06-18 | 2020-10-23 | 中国城市建设研究院有限公司 | Ozone oxidation catalyst for advanced treatment of organic wastewater and preparation method thereof |
| CN112156789A (en) * | 2020-08-07 | 2021-01-01 | 光大水务（深圳）有限公司 | Sponge iron catalyst for catalyzing ozone oxidation to treat wastewater and preparation method thereof |
| CN113117684A (en) * | 2021-04-19 | 2021-07-16 | 河北德龙环境工程股份有限公司 | Preparation method of ternary oxide ozone catalyst for advanced wastewater treatment |
| CN113262787A (en) * | 2021-05-27 | 2021-08-17 | 煤炭科学技术研究院有限公司 | Preparation method of iron-based composite catalyst for catalytic ozonation treatment of coal chemical wastewater |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108404913A (en) * | 2018-01-24 | 2018-08-17 | 大连理工大学 | A method of preparing the ozone catalyst for removing water removal moderate resistance life element using cheap material as carrier |
| CN110052269A (en) * | 2019-05-08 | 2019-07-26 | 科盛环保科技股份有限公司 | A kind of preparation method of depth-averaged model ozone catalytic oxidation catalyst |
| CN110052268A (en) * | 2019-05-22 | 2019-07-26 | 四川恒泰环境技术有限责任公司 | A kind of ozone catalytic oxidation catalyst and preparation method thereof |
| CN110270329A (en) * | 2019-06-18 | 2019-09-24 | 北京首创股份有限公司 | For handling the ozone catalyst and preparation method thereof of hardly degraded organic substance in water |
| CN111153487A (en) * | 2020-01-08 | 2020-05-15 | 杭州天创环境科技股份有限公司 | Method for efficiently removing refractory organic matters in clean sewage |
| CN111804300A (en) * | 2020-06-18 | 2020-10-23 | 中国城市建设研究院有限公司 | Ozone oxidation catalyst for advanced treatment of organic wastewater and preparation method thereof |
| CN112156789A (en) * | 2020-08-07 | 2021-01-01 | 光大水务（深圳）有限公司 | Sponge iron catalyst for catalyzing ozone oxidation to treat wastewater and preparation method thereof |
| CN113117684A (en) * | 2021-04-19 | 2021-07-16 | 河北德龙环境工程股份有限公司 | Preparation method of ternary oxide ozone catalyst for advanced wastewater treatment |
| CN113262787A (en) * | 2021-05-27 | 2021-08-17 | 煤炭科学技术研究院有限公司 | Preparation method of iron-based composite catalyst for catalytic ozonation treatment of coal chemical wastewater |
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Application publication date: 20170721 |