CN106540706B - A kind of support type ozone catalyst and its preparation method and application - Google Patents
A kind of support type ozone catalyst and its preparation method and application Download PDFInfo
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- CN106540706B CN106540706B CN201610947082.XA CN201610947082A CN106540706B CN 106540706 B CN106540706 B CN 106540706B CN 201610947082 A CN201610947082 A CN 201610947082A CN 106540706 B CN106540706 B CN 106540706B
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- ozone catalyst
- 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
- 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
- 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
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
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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
-
- 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
Abstract
The present invention discloses a kind of support type ozone catalyst and its preparation method and application.The preparation method of support type ozone catalytic agent carrier, the load of preparation and transition metal oxide and rare-earth oxide including catalyst carrier in catalyst support surface, the transition metal oxide and rare-earth oxide are loaded in catalyst support surface, wherein, transition metal oxide accounts for the 8%-13% of the ozone catalyst quality, and rare-earth oxide accounts for the 1%-3% of the ozone catalyst quality.Support type ozone catalyst being applied in sewage treatment made from the above method.Compared with prior art, the present invention can effectively improve the contact area of ozone catalyst and ozone, so that ozone be accelerated to decompose the oxidation rate and efficiency for generating hydroxyl radical free radical, and then accelerating dirty Organic substance in water.Ozone catalyst preparation is simple, reusable.
Description
Technical field
The invention belongs to sewage treatment fields, and in particular to a kind of support type ozone catalyst and preparation method thereof and answer
With.
Background technique
Catalytic ozonation technology is a kind of efficient advanced treatment of wastewater technology, is Industrial Waste Water Treatments field in recent years
Research hotspot.Compared with ozone is separately as oxidant, the hydroxyl radical free radical of ozone and catalyst interaction generation is to dirt
The oxidability of Organic substance in water is stronger, and oxidation rate faster, can almost aoxidize all pollutants.With homogeneous ozone catalytic
Oxidation technology is compared, and the catalyst in heterogeneous catalytic ozonation technology exists in solid form, is easily separated with solution, can weight
It is multiple to utilize, it is widely used in actual sewage processing.
The rate of hydroxyl radical free radical is generated in order to increase ozone and catalyst action, on the one hand a large amount of researchers are found
On the other hand the superior ozone catalysing material of performance prepares more preferable ideal catalyst carrier.Common ozone catalyst is
By metal or metal oxide supported in a series of porous materials such as zeolite, ceramics, silica gel, diatomite, active carbon, molecular sieve
Carrier surface, these carriers have reference area big, and catalyst life is high, the features such as being easily isolated and recycled.Catalyst is born
The contact area of ozone and catalyst can be increased by being loaded in these porous material surfaces, thus accelerate the generating rate of free radical,
And then accelerate the oxidation rate of dirty Organic substance in water.
For existing porous material catalyst carrier, the surface area that how to further increase it can be used for loading is to improve
The key of support type ozone catalyst catalytic rate.
Summary of the invention
In order to overcome the deficiencies of the prior art, present invention aims at: a kind of support type ozone catalyst preparation method is provided,
Titanium dioxide microballoon sphere is grown in molecular sieve surface and is used as catalyst carrier together with molecular sieve.
Another object of the present invention is: providing a kind of support type ozone catalyst made from the above method, increases load
Body can load area, improve catalyst and ozone contact area, accelerate the generating rate of free radical.While titanium dioxide is certainly
Body is also a kind of ozone catalyst, can be used to that catalysis is assisted to react.
Another object of the present invention is to: the application in sewage treatment of the support type ozone catalyst is provided.Into
And accelerate the oxidation rate of dirty Organic substance in water.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of preparation method of support type ozone catalyst, comprising the following steps:
(1) preparation of catalyst carrier
It weighs ammonium titanium fluoride and boric acid is soluble in water, stir, obtain precursor solution；Precursor solution is transferred to sealing
In reaction kettle, pretreated molecular sieve is immersed in precursor solution, hydro-thermal reaction.After the reaction was completed, product is taken out, clearly
It washes, calcines to get catalyst carrier is arrived；
(2) load of transition metal oxide and rare-earth oxide in catalyst support surface
Carrying transition metal oxide and rare-earth oxide in the catalyst carrier made from step (1), wherein mistake
Metal oxide accounts for the ozone catalyst quality 8% -13% is crossed, rare-earth oxide accounts for the ozone catalyst quality
1% -3%.
In step (1): ammonium titanium fluoride, boric acid, water additive amount mass ratio be (2-4): 1:(32-40)；Hydro-thermal reaction
Process conditions are as follows: at 40-80 DEG C react 6-10 h；The process conditions of calcining are as follows: calcine 40-80 at 400-600 DEG C
min。
In step (2): the substance withdrawl syndrome ratio of ferric nitrate, nickel nitrate and cerous nitrate is (8-12): (1- in maceration extract
2): 1；Dip time is 8-16 hours；Dry process conditions are as follows: the dry 60-120 min at 100-120 DEG C；The work of calcining
Skill condition are as follows: calcined 3-5 hours at 300-400 DEG C.
Transition metal oxide described in step (2) is iron oxide and nickel oxide, and the rare-earth oxide is
Cerium oxide.
A kind of support type ozone catalyst, which is characterized in that be prepared according to any of the above-described the method.
The present invention provides a kind of application of support type ozone catalyst in sewage treatment.
Compared with prior art, the present invention can effectively improve the contact area of ozone catalyst and ozone, to accelerate smelly
Oxygen solution generates hydroxyl radical free radical, and then accelerates the oxidation rate and efficiency of dirty Organic substance in water.Ozone catalyst preparation letter
It is single, it is reusable.The invention has the following advantages that
(1) titanium dioxide microballoon sphere is grown in molecular sieve surface and is used as catalyst carrier together with molecular sieve by the present invention, is increased
Added carrier can load area, improve the contact area of catalyst and ozone, accelerate the generating rate of free radical, and then accelerate
The oxidation rate of dirty Organic substance in water.
(2) titanium dioxide microballoon sphere of molecular sieve surface growth is also ozone catalyst, can be used to that catalysis is assisted to react.
Detailed description of the invention
In the titanium dioxide microballoon sphere of molecular sieve surface growth in Fig. 1 present invention.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1:
A kind of preparation method of support type ozone catalyst, is made up of following steps:
(1) it weighs ammonium titanium fluoride and boric acid is soluble in water, stir, obtain precursor solution.Ammonium titanium fluoride, boric acid, water
The mass ratio of additive amount is 3:1:36.
(2) precursor solution is transferred in sealing reaction kettle, pretreated molecular sieve is immersed in precursor solution,
The hydro-thermal reaction 8h at 60 DEG C.
(3) after the reaction was completed, product is taken out, is rinsed with deionized water, surface residue is removed, is calcined at 500 DEG C
60min to get arrive catalyst carrier.Catalyst carrier obtained is detected, Fig. 1 shows the two of molecular sieve surface growth
The SEM of titania microsphere schemes, and Cong Tuzhong is it can be found that the diameter that titanium dioxide microballoon sphere is made is 1-2 μm.
(4) carrier obtained being dipped in maceration extract, maceration extract is the mixed liquor of ferric nitrate, nickel nitrate and cerous nitrate,
Corresponding substance withdrawl syndrome ratio is 10:1.5:1；Dipping takes out after 12 hours, the dry 80min at 105 DEG C, then is placed in 350
4h is calcined at DEG C to get purpose product support type ozone catalyst is arrived.
(5) ozone catalyst prepared by is 83.6 % to the degradation rate of the COD of certain waste water from pesticide factory
Embodiment 2:
A kind of preparation method of support type ozone catalyst, is made up of following steps:
(1) it weighs ammonium titanium fluoride and boric acid is soluble in water, stir, obtain precursor solution.Ammonium titanium fluoride, boric acid, water
The mass ratio of additive amount is 2:1:32.
(2) precursor solution is transferred in sealing reaction kettle, pretreated molecular sieve is immersed in precursor solution,
The hydro-thermal reaction 10h at 40 DEG C.
(3) after the reaction was completed, product is taken out, is rinsed with deionized water, surface residue is removed, is calcined at 400 DEG C
80min to get arrive catalyst carrier.
(4) carrier obtained being dipped in maceration extract, maceration extract is the mixed liquor of ferric nitrate, nickel nitrate and cerous nitrate,
Corresponding substance withdrawl syndrome ratio is 8:1:1；Dipping takes out after 8 hours, dry 60min at 120 DEG C, then is placed at 400 DEG C and forges
3h is burnt to get purpose product support type ozone catalyst is arrived.
(5) ozone catalyst prepared by is 79.3 % to the degradation rate of the COD of certain waste water from pesticide factory
Embodiment 3:
A kind of preparation method of support type ozone catalyst, is made up of following steps:
(1) it weighs ammonium titanium fluoride and boric acid is soluble in water, stir, obtain precursor solution.Ammonium titanium fluoride, boric acid, water
The mass ratio of additive amount is 4:1:40.
(2) precursor solution is transferred in sealing reaction kettle, pretreated molecular sieve is immersed in precursor solution,
The hydro-thermal reaction 6h at 80 DEG C.
(3) after the reaction was completed, product is taken out, is rinsed with deionized water, surface residue is removed, is calcined at 600 DEG C
40min to get arrive catalyst carrier.
(4) carrier obtained being dipped in maceration extract, maceration extract is the mixed liquor of ferric nitrate, nickel nitrate and cerous nitrate,
Corresponding substance withdrawl syndrome ratio is 12:2:1；Dipping takes out after 16 hours, the dry 120min at 100 DEG C, then is placed in 300 DEG C
Lower calcining 5h to get arrive purpose product support type ozone catalyst.
(5) ozone catalyst prepared by is 81.7% to the degradation rate of the COD of certain waste water from pesticide factory
Embodiment 4:
A kind of preparation method of support type ozone catalyst, is made up of following steps:
(1) it weighs ammonium titanium fluoride and boric acid is soluble in water, stir, obtain precursor solution.Ammonium titanium fluoride, boric acid, water
The mass ratio of additive amount is 3:1:36.
(2) precursor solution is transferred in sealing reaction kettle, pretreated molecular sieve is immersed in precursor solution,
The hydro-thermal reaction 8h at 60 DEG C.
(3) after the reaction was completed, product is taken out, is rinsed with deionized water, surface residue is removed, is calcined at 500 DEG C
60min to get arrive catalyst carrier.
(4) carrier obtained being dipped in maceration extract, maceration extract is the mixed liquor of ferric nitrate, nickel nitrate and cerous nitrate,
Corresponding substance withdrawl syndrome ratio is 8:1:1；Dipping takes out after 8 hours, dry 60min at 120 DEG C, then is placed at 400 DEG C and forges
3h is burnt to get purpose product support type ozone catalyst is arrived.
(5) ozone catalyst prepared by is 78.8 % to the degradation rate of the COD of certain waste water from pesticide factory
Embodiment 5:
A kind of preparation method of support type ozone catalyst, is made up of following steps:
(1) it weighs ammonium titanium fluoride and boric acid is soluble in water, stir, obtain precursor solution.Ammonium titanium fluoride, boric acid, water
The mass ratio of additive amount is 2:1:32.
(2) precursor solution is transferred in sealing reaction kettle, pretreated molecular sieve is immersed in precursor solution,
The hydro-thermal reaction 10h at 40 DEG C.
(3) after the reaction was completed, product is taken out, is rinsed with deionized water, surface residue is removed, is calcined at 400 DEG C
80min to get arrive catalyst carrier.
(4) carrier obtained being dipped in maceration extract, maceration extract is the mixed liquor of ferric nitrate, nickel nitrate and cerous nitrate,
Corresponding substance withdrawl syndrome ratio is 12:2:1；Dipping takes out after 16 hours, the dry 120min at 100 DEG C, then is placed in 300 DEG C
Lower calcining 5h to get arrive purpose product support type ozone catalyst.
(5) ozone catalyst prepared by is 79.2% to the degradation rate of the COD of certain waste water from pesticide factory
Embodiment 6:
A kind of preparation method of support type ozone catalyst, is made up of following steps:
(1) it weighs ammonium titanium fluoride and boric acid is soluble in water, stir, obtain precursor solution.Ammonium titanium fluoride, boric acid, water
The mass ratio of additive amount is 4:1:40.
(2) precursor solution is transferred in sealing reaction kettle, pretreated molecular sieve is immersed in precursor solution,
The hydro-thermal reaction 6h at 80 DEG C.
(3) after the reaction was completed, product is taken out, is rinsed with deionized water, surface residue is removed, is calcined at 600 DEG C
40min to get arrive catalyst carrier.
(4) carrier obtained being dipped in maceration extract, maceration extract is the mixed liquor of ferric nitrate, nickel nitrate and cerous nitrate,
Corresponding substance withdrawl syndrome ratio is 10:1.5:1；Dipping takes out after 12 hours, the dry 80min at 105 DEG C, then is placed in 350
4h is calcined at DEG C to get purpose product support type ozone catalyst is arrived.
(5) ozone catalyst prepared by is 79.1% to the degradation rate of the COD of certain waste water from pesticide factory.
Claims (5)
1. a kind of preparation method of support type ozone catalyst, which comprises the following steps:
(1) preparation of catalyst carrier
It weighs ammonium titanium fluoride and boric acid is soluble in water, stir, obtain precursor solution；Precursor solution is transferred to sealing reaction
In kettle, pretreated molecular sieve is immersed in precursor solution, hydro-thermal reaction；After the reaction was completed, product is taken out, cleaning is forged
It burns to get catalyst carrier is arrived；
(2) load of transition metal oxide and rare-earth oxide in catalyst support surface
Carrying transition metal oxide and rare-earth oxide in the catalyst carrier made from step (1), specifically, will system
The carrier obtained is dipped in maceration extract, and maceration extract is the mixed liquor of ferric nitrate, nickel nitrate and cerous nitrate, and drying after dipping is calcined,
In, transition metal oxide accounts for the 8% -13% of the ozone catalyst quality, and rare-earth oxide accounts for the ozone catalytic
The 1% -3% of agent quality；Wherein,
In step (1): ammonium titanium fluoride, boric acid, water additive amount mass ratio be (2-4): 1:(32-40)；The work of hydro-thermal reaction
Skill condition are as follows: 6-10 h is reacted at 40-80 DEG C；The process conditions of calcining are as follows: 40-80 min is calcined at 400-600 DEG C.
2. a kind of preparation method of support type ozone catalyst according to claim 1, which is characterized in that step (2)
In: the substance withdrawl syndrome ratio of ferric nitrate, nickel nitrate and cerous nitrate is (8-12): (1-2): 1 in maceration extract；Dip time is 8-
16 hours；Dry process conditions are as follows: the dry 60-120 min at 100-120 DEG C；The process conditions of calcining are as follows: in 300-
It is calcined 3-5 hours at 400 DEG C.
3. a kind of preparation method of support type ozone catalyst according to claim 1, which is characterized in that step (2)
Described in transition metal oxide be iron oxide and nickel oxide, the rare-earth oxide be cerium oxide.
4. a kind of support type ozone catalyst, which is characterized in that be prepared according to claim 1 to 3 any the methods.
5. application of a kind of support type ozone catalyst in sewage treatment according to claim 4.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107597174B (en) * | 2017-10-18 | 2019-11-29 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of heterogeneous ozone catalyst and products thereof and application |
| CN107876045A (en) * | 2017-11-01 | 2018-04-06 | 南京理工大学 | A kind of TiO2(A B) load MnCe oxidizing and denitrating ozone catalyst and preparation method thereof, application |
| CN107876062A (en) * | 2017-11-06 | 2018-04-06 | 上海纳米技术及应用国家工程研究中心有限公司 | Ozone catalyst preparation method and products thereof and application |
| CN110975862A (en) * | 2019-11-22 | 2020-04-10 | 南京中衡元环保科技有限公司 | High-efficiency catalyst for ozone reactor and preparation method thereof |
| CN112264030B (en) * | 2020-11-21 | 2022-06-21 | 江西挺进环保科技股份有限公司 | Ozone catalytic treating agent for treating organic matters in wastewater and preparation method thereof |
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