CN106732792A - One kind treatment Coal Chemical Industry high-salt wastewater catalyst and preparation method thereof - Google Patents
One kind treatment Coal Chemical Industry high-salt wastewater catalyst and preparation method thereof Download PDFInfo
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- CN106732792A CN106732792A CN201611166477.2A CN201611166477A CN106732792A CN 106732792 A CN106732792 A CN 106732792A CN 201611166477 A CN201611166477 A CN 201611166477A CN 106732792 A CN106732792 A CN 106732792A
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/32—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of manganese, technetium or rhenium
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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
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Abstract
The invention discloses one kind treatment Coal Chemical Industry high-salt wastewater catalyst and preparation method thereof.The method comprises the following steps:(1) adhesive is added in alumina powder, catalyst kernel is obtained through granulation;(2) alumina powder, metal salt solution, pore creating material and adhesive are added in the catalyst kernel, obtains being formed outside the catalyst kernel shaping of catalyst spheroid of integument through granulation;(3) the shaping of catalyst spheroid is dried and is calcined;(4) surface of the shaping of catalyst spheroid to being obtained after the roasting carries out hydrophobically modified, you can obtain the treatment Coal Chemical Industry high-salt wastewater catalyst.Catalyst of the present invention be with Multimetal oxide as main active component, surface there is the catalyst of hydrophobic property, can effectively prevent the Cl in strong brine high‑、SO4 2‑Deng Anion-adsorption, the removal efficiency of catalysis activity and organic matter is improved.
Description
Technical field
The invention belongs to field of catalyst preparation, more particularly to a kind for the treatment of Coal Chemical Industry high-salt wastewater catalyst and
Its preparation method.
Background technology
Modern Coal-based Chemical refers mainly to coal gas, coal liquifaction, coal-to-olefin, coal-ethylene glycol etc., and Modern Coal-based Chemical is to realize
The important channel that Coal Clean is efficiently utilized, is the important directions of country's encouragement.But because Coal Chemical Engineering Project is mainly distributed on west
Northern ecologically fragile areas, water resources shortage, and without receiving sewage body, therefore waste water requirement " nearly zero " discharge.The treatment of high-salt wastewater
Disposal is waste water " one of key restriction factors of nearly zero " discharge.Coal Chemical Industry high-salt wastewater mostlys come from film concentration or heat is dense
The strong brine that compression process is produced, its total dissolved solid (TDS) differs larger, and generally 1%~8%, what is had is even as high as
More than 20%, COD (COD) is 100~2000mg/L, and predominantly hardly degraded organic substance.COD high may cause film
Pollution, evaporation and crystal process Organic Pollution, limit waste water further concentration or recycling.For such waste water
Treatment, because salinity is to the inhibitory action of microorganism, biochemical process is typically hard to work.Active carbon adsorption is to organic matter removal
Effect is significant, but charcoal absorption finite capacity, regenerate difficulty after adsorption saturation, cause operating cost higher.Multiphase ozone is urged
Change oxidizing process by producing the hydroxyl radical free radical of strong oxidizing property, the organic pollution to difficult degradation in water, high stability carries out oxygen
Change degraded, do not produce secondary pollution, one of key technology as organic pollutant removal in high-salt wastewater.
Correlative study shows that surface soda acid position and the surface hydroxyl groups of metal oxide are considered as the work of ozone decomposed
Property site.In strong brine high, due to Cl-、SO4 2-、CO3 2-、PO4 3-Deng the absorption of anion, avtive spot is occupied so that smelly
VPO catalysts activity decrease.Existing ozone catalyst is for organic matter removal effect on driving birds is not good in Coal Chemical Industry high-salt wastewater.
The content of the invention
It is an object of the invention to provide one kind treatment Coal Chemical Industry high-salt wastewater catalyst and preparation method thereof, the method is led to
The metal active constituent for changing catalyst is crossed, regulates and controls Surface acid-base properties, and obtain using the method such as surfactant-modified
Hydrophobic surface, will weaken Cl-、SO4 2-Deng Anion-adsorption effect, so that ozone catalyst shows in high-salt wastewater
COD removal efficiency high.
A kind of preparation method for the treatment of Coal Chemical Industry high-salt wastewater catalyst that the present invention is provided, comprises the following steps:
(1) adhesive is added in alumina powder, catalyst kernel is obtained through granulation;
(2) alumina powder, metal salt solution, pore creating material and adhesive are added in the catalyst kernel, through granulation
Obtain being formed outside the catalyst kernel shaping of catalyst spheroid of integument;
(3) the shaping of catalyst spheroid is dried and is calcined;
(4) surface of the shaping of catalyst spheroid to being obtained after the roasting carries out hydrophobically modified, you can obtain the place
Reason Coal Chemical Industry high-salt wastewater catalyst.
Above-mentioned preparation method, in step (1), the aluminum oxide can be (20~100) with the mass ratio of described adhesive:
1, concretely 20:1.Described adhesive can be at least one in water, Ludox and Alumina gel.
The diameter of the catalyst kernel can be 2~4mm, concretely 2~3mm, 3~4mm, 2mm, 3mm or 4mm.
Above-mentioned preparation method, in step (2), the catalyst kernel, the alumina powder, the pore creating material and institute
The part by weight for stating adhesive is (50%~70%):(20%~30%):(5%~10%):(1%~5%), concretely
(60%~70%):(20%~30%):5%:5%th, 60%:30%:5%:5% or 70%:20%:5%:5%.It is described to make
Hole agent can be at least one in polyethylene glycol, polyvinyl alcohol, urea and carbon black.Described adhesive can be water, Ludox and aluminium
At least one in colloidal sol.
Above-mentioned preparation method, in step (2), the mass volume ratio of the catalyst kernel and the metal salt solution can
It is 1g:(0.1~1) mL, concretely 1g:(0.5~1) mL, 1g:0.5mL or 1g:1mL.
The metal salt solution contains manganese salt and following at least one slaine:Cerium salt, magnesium salts and pink salt, can specifically contain
There are manganese salt and the following slaine of any one:Cerium salt, magnesium salts and pink salt.The manganese salt and following at least one slaine:Cerium
The mol ratio of salt, magnesium salts and pink salt can be (1~10):1, concretely (4~10):1st, (5~10):1st, (4~5):1、4:1、
5:1 or 10:1.The molar concentration of manganese salt can be 0.1~2.0mol/L in the metal salt solution, concretely 1.0mol/L.Institute
It is the slaine for being dissolvable in water water to state slaine, including but not limited to nitrate, sulfate, acetate or chlorate.
Above-mentioned preparation method, in step (2), the diameter of the shaping of catalyst spheroid can be 4~8mm, concretely 4
~6mm, 6~8mm, 4mm, 6mm or 8mm.
Above-mentioned preparation method, in step (3), the dry temperature can be 80~150 DEG C (such as 100 DEG C), and the time is 4
~12 hours (such as 12 hours);The temperature of the roasting is 500~900 DEG C (such as 600 DEG C), and the time is for (such as 4 is small within 2~8 hours
When).
Above-mentioned preparation method, in step (4), the surface modifier that the hydrophobically modified is used can for surfactant and
At least one in silane coupler.The surfactant concretely lauryl sodium sulfate, stearic acid or perfluoro caprylic acid;
The silane coupler concretely 3- methacryloxypropyl trimethoxy silanes.The method of the hydrophobically modified is this
Conventional method known to art personnel, such as impregnated in the organic solution of the surface modifier and/or water-soluble by catalyst
In liquid, the hydrophobically modified of catalyst is capable of achieving after drying.The catalyst is in the organic solution and/or the aqueous solution
Mass concentration can be 3%~5%, concretely 3% or 5%.
Invention further provides the treatment Coal Chemical Industry high-salt wastewater catalysis that a kind of above-mentioned preparation method is prepared
Agent.The hardly degraded organic substance that the catalyst can be used in catalytic ozonation removal Coal Chemical Industry high-salt wastewater, removal efficiency is high.
The present invention has the advantages that:
(1) it with Multimetal oxide is main activearm that the salt tolerant ozone catalytic oxidation catalyst prepared in the present invention is
Point, surface there is the catalyst of hydrophobic property, can effectively prevent the Cl in strong brine high-、SO4 2-Deng Anion-adsorption, raising is urged
Change the removal efficiency of activity and organic matter.
(2) present invention is dissolved in water by the slaine with ozone catalytic activity, is rolled together with alumina powder powder stock
Dynamic granulation, dry, roasting, in high-temperature sintering process, slaine decomposes the metal oxide for obtaining has micron or nanometer chi
It is very little, it is uniformly distributed in alumina support, adhesive strength is high, and catalysis activity and stability are strong, easily realizes large-scale industry
Metaplasia is produced.
Catalyst of the invention is mainly used in catalytic ozonation removal Coal Chemical Industry high-salt wastewater (TDS is 1%~8%)
Persistent organic pollutants.
Specific embodiment
Experimental technique used in following embodiments is conventional method unless otherwise specified.
Material used, reagent etc. in following embodiments, unless otherwise specified, commercially obtain.
Embodiment 1, preparation treatment Coal Chemical Industry high-salt wastewater catalyst
Treatment Coal Chemical Industry high-salt wastewater catalyst is prepared in accordance with the following steps:
(1) amorphous aluminium powder is selected, the 5% of the quality of alumina powder Alumina gel adhesive is added, through making
Grain obtains the catalyst kernel of a diameter of 2mm;
(2) manganese nitrate and cerous nitrate in molar ratio 4:1 is made into the aqueous solution, and wherein manganese nitrate molar concentration is 1.0mol/
L;Metal salt solution, (catalyst kernel is 1g with the mass volume ratio of metal salt solution:1mL) with alumina powder, poly- second two
Alcohol and Alumina gel adhesive mix, and are added in comminutor, and (catalyst kernel, alumina powder are granulated together with catalyst kernel
The mass ratio of end, pore creating material and adhesive is 60%:30%:5%:5%, obtain forming integument outside catalyst kernel
The shaping of catalyst spheroid of a diameter of 4mm;
(3) shaping of catalyst spheroid is dried into 12h, 600 DEG C of roasting 4h at 100 DEG C;
(4) surface of fired shaping of catalyst spheroid is carried out using Surfactant SDS hydrophobic
It is modified to obtain processing Coal Chemical Industry high-salt wastewater catalyst.The step of hydrophobically modified, is as follows:Lauryl sodium sulfate is dissolved in nothing
Water-ethanol (concentration is 5%), is cleaned up after catalyst is impregnated into 1h with ethanol, is put into 105 DEG C of oven dryings.
The catalytic performance test of catalyst manufactured in the present embodiment is accomplished by the following way:
Certain coal liquifaction enterprise reverse osmosis concentrated water is processed using catalytic ozonation, TDS is 18800mg/L, and COD is 300mg/
L, ozone dosage 200mg/L, the reaction time is 60min, is added without ozone catalyst, and COD is reduced to 250mg/ by 300mg/L
L;The salt tolerant ozone catalyst prepared using embodiment 1, COD is reduced to 150mg/L by 300mg/L, and COD clearances reach
50%, COD clearance improve 33.3%.
Embodiment 2, preparation treatment Coal Chemical Industry high-salt wastewater catalyst
Treatment Coal Chemical Industry high-salt wastewater catalyst is prepared in accordance with the following steps:
(1) amorphous aluminium powder is selected, the 5% of the quality of alumina powder Alumina gel adhesive is added, through making
Grain obtains the catalyst kernel of a diameter of 3mm;
(2) manganese sulfate and magnesium sulfate in molar ratio 10:1 is made into the aqueous solution, and wherein manganese sulfate molar concentration is 1.0mol/
L, metal salt solution, (catalyst kernel is 1g with the mass volume ratio of metal salt solution:1mL) with alumina powder, poly- second two
Alcohol and Alumina gel adhesive mix, and are added in comminutor, and (catalyst kernel, alumina powder are granulated together with catalyst kernel
The mass ratio of end, pore creating material and adhesive is 70%:20%:5%:5%, obtain forming integument outside catalyst kernel
The shaping of catalyst spheroid of a diameter of 6mm;
(3) shaping of catalyst spheroid is dried into 12h, 600 DEG C of roasting 4h at 100 DEG C;
(4) using silane coupler 3- methacryloxypropyl trimethoxy silanes to fired shaping of catalyst
The surface of spheroid carries out hydrophobically modified, obtains processing Coal Chemical Industry high-salt wastewater catalyst.The step of hydrophobically modified, is as follows:By silicon
Alkane coupling agent and absolute ethyl alcohol, water by volume 3:4:93 it is well mixed after hydrolyze 24h, catalyst is impregnated clear with ethanol after 1h
Wash clean, is put into 105 DEG C of oven dryings.
The catalytic performance test of catalyst manufactured in the present embodiment is accomplished by the following way:
Certain coal gas enterprise strong brine high is processed using catalytic ozonation, TDS is 80000mg/L, and COD is 1500mg/
L, ozone dosage 500mg/L, the reaction time is 60min, is added without ozone catalyst, and COD is reduced to by 1500mg/L
1300mg/L;The salt tolerant ozone catalyst prepared using embodiment 2, COD is reduced to 1100mg/L, COD removals by 1500mg/L
Efficiency improves 13.3%.
Embodiment 3, preparation treatment Coal Chemical Industry high-salt wastewater catalyst
Treatment Coal Chemical Industry high-salt wastewater catalyst is prepared in accordance with the following steps:
(1) amorphous aluminium powder is selected, the 5% of the quality of alumina powder Alumina gel adhesive is added, through making
Grain obtains the catalyst kernel of a diameter of 3mm;
(2) manganese acetate and butter of tin in molar ratio 5:1 is made into the aqueous solution, and wherein manganese acetate molar concentration is
1.0mol/L, metal salt solution, (catalyst kernel is 1g with the mass volume ratio of metal salt solution:0.5mL) and alumina powder
The mixing of end, polyethylene glycol and Alumina gel adhesive, is added in comminutor, granulated together with catalyst kernel (catalyst kernel,
The mass ratio of alumina powder, pore creating material and adhesive is 70%:20%:5%:5%, obtain being formed outside catalyst kernel
The shaping of catalyst spheroid of a diameter of 6mm of integument;
(3) shaping of catalyst spheroid is dried into 12h, 600 DEG C of roasting 4h at 100 DEG C;
(4) hydrophobically modified is carried out to the surface of the shaping of catalyst spheroid after fired using surfactant stearic acid,
Obtain processing Coal Chemical Industry high-salt wastewater catalyst.The step of hydrophobically modified, is as follows:Stearic acid is dissolved in into acetone, and (concentration is
5%) cleaned up with acetone after catalyst, is impregnated into 1h, be put into 105 DEG C of oven dryings.
The catalytic performance test of salt tolerant ozone catalyst manufactured in the present embodiment is accomplished by the following way:
Certain coal-to-olefin enterprise strong brine high is processed using catalytic ozonation, TDS is 42800mg/L, and COD is 500mg/
L, ozone dosage 500mg/L, the reaction time is 60min, is added without ozone catalyst, and COD is reduced to 350mg/ by 500mg/L
L;The catalyst prepared using embodiment 3, COD is reduced to 200mg/L by 500mg/L, and COD removal efficiency improves 30.0%.
Above-described embodiment is the present invention preferably implementation method, but embodiments of the present invention are not by above-described embodiment
Limitation, others are any to should be equivalent substitute mode without departing from the change made under Spirit Essence of the invention and principle,
It is included in the present invention.
Claims (10)
1. a kind of preparation method for processing Coal Chemical Industry high-salt wastewater catalyst, comprises the following steps:
(1) adhesive is added in alumina powder, catalyst kernel is obtained through granulation;
(2) alumina powder, metal salt solution, pore creating material and adhesive are added in the catalyst kernel, is obtained through granulation
The shaping of catalyst spheroid of integument is formed outside the catalyst kernel;
(3) the shaping of catalyst spheroid is dried and is calcined;
(4) surface of the shaping of catalyst spheroid to being obtained after the roasting carries out hydrophobically modified, you can obtain the treatment coal
Chemical industry high-salt wastewater catalyst.
2. preparation method according to claim 1, it is characterised in that:In step (1), the matter of the aluminum oxide and adhesive
Amount is than being (20~100):1;Described adhesive is at least one in water, Ludox and Alumina gel.
3. preparation method according to claim 1 and 2, it is characterised in that:In step (1), the catalyst kernel it is straight
Footpath is 2~4mm.
4. the preparation method according to any one of claim 1-3, it is characterised in that:In step (2), in the catalyst
The part by weight of core, the alumina powder, the pore creating material and described adhesive is (50%~70%):(20%~
30%):(5%~10%):(1%~5%);The pore creating material be polyethylene glycol, polyvinyl alcohol, urea and carbon black at least
It is a kind of;Described adhesive is at least one in water, Ludox and Alumina gel.
5. the preparation method according to any one of claim 1-4, it is characterised in that:In step (2), in the catalyst
The mass volume ratio of core and the metal salt solution is 1g:(0.1~1) mL;The metal salt solution contain manganese salt and it is following extremely
A kind of few slaine:Cerium salt, magnesium salts and pink salt;The manganese salt and following at least one slaine:Cerium salt, magnesium salts and pink salt
Mol ratio be (1~10):1;The molar concentration of manganese salt is 0.1~2.0mol/L in the metal salt solution.
6. the preparation method according to any one of claim 1-5, it is characterised in that:In step (2), the catalyst into
A diameter of 4~8mm of type spheroid.
7. the preparation method according to any one of claim 1-6, it is characterised in that:In step (3), the dry temperature
It is 80~150 DEG C to spend, and the time is 4~12 hours;The temperature of the roasting is 500~900 DEG C, and the time is 2~8 hours.
8. the preparation method according to any one of claim 1-7, it is characterised in that:In step (4), the hydrophobically modified
The surface modifier for using is at least one in surfactant and silane coupler.
9. preparation method according to claim 8, it is characterised in that:The surfactant be lauryl sodium sulfate,
Stearic acid or perfluoro caprylic acid;The silane coupler is 3- methacryloxypropyl trimethoxy silanes.
10. the treatment Coal Chemical Industry high-salt wastewater catalyst that the preparation method any one of claim 1-9 is prepared.
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108178283A (en) * | 2017-12-27 | 2018-06-19 | 苏州大学 | The method for removing organic matter in high-chloride wastewater |
CN108745419A (en) * | 2018-07-24 | 2018-11-06 | 大唐(北京)水务工程技术有限公司 | A kind of catalyst and preparation method thereof of O3 catalytic oxidation waste water |
CN109772358A (en) * | 2018-06-29 | 2019-05-21 | 光大水务(深圳)有限公司 | A kind of preparation method of catalyst pore creating material and the high porosity catalyst based on pore creating material |
CN109939695A (en) * | 2019-04-03 | 2019-06-28 | 宁夏大学 | A kind of support type O3The preparation of catalyst and its application in coal chemical industry high-salt wastewater COD removal |
CN110961118A (en) * | 2019-12-18 | 2020-04-07 | 煤炭科学技术研究院有限公司 | Coal gangue-based ozone oxidation catalyst and preparation method and application thereof |
CN111013571A (en) * | 2019-11-27 | 2020-04-17 | 萍乡煤科环保科技有限公司 | Preparation method of modified ozone catalyst suitable for high-salinity wastewater in coal chemical industry |
CN111468105A (en) * | 2020-04-23 | 2020-07-31 | 光大水务科技发展(南京)有限公司 | Multilayer structure catalyst for catalytic oxidation of nbsCOD by ozone and preparation method and application thereof |
CN113976118A (en) * | 2021-11-30 | 2022-01-28 | 昂星新型碳材料常州有限公司 | Ozone catalyst, preparation method and application thereof |
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Cited By (11)
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CN108178283A (en) * | 2017-12-27 | 2018-06-19 | 苏州大学 | The method for removing organic matter in high-chloride wastewater |
CN109772358A (en) * | 2018-06-29 | 2019-05-21 | 光大水务(深圳)有限公司 | A kind of preparation method of catalyst pore creating material and the high porosity catalyst based on pore creating material |
CN108745419A (en) * | 2018-07-24 | 2018-11-06 | 大唐(北京)水务工程技术有限公司 | A kind of catalyst and preparation method thereof of O3 catalytic oxidation waste water |
CN108745419B (en) * | 2018-07-24 | 2020-12-18 | 萍乡煤科环保科技有限公司 | Catalyst for catalyzing ozone to oxidize wastewater and preparation method thereof |
CN109939695A (en) * | 2019-04-03 | 2019-06-28 | 宁夏大学 | A kind of support type O3The preparation of catalyst and its application in coal chemical industry high-salt wastewater COD removal |
CN111013571A (en) * | 2019-11-27 | 2020-04-17 | 萍乡煤科环保科技有限公司 | Preparation method of modified ozone catalyst suitable for high-salinity wastewater in coal chemical industry |
CN110961118A (en) * | 2019-12-18 | 2020-04-07 | 煤炭科学技术研究院有限公司 | Coal gangue-based ozone oxidation catalyst and preparation method and application thereof |
CN110961118B (en) * | 2019-12-18 | 2023-02-24 | 煤炭科学技术研究院有限公司 | Coal gangue-based ozone oxidation catalyst and preparation method and application thereof |
CN111468105A (en) * | 2020-04-23 | 2020-07-31 | 光大水务科技发展(南京)有限公司 | Multilayer structure catalyst for catalytic oxidation of nbsCOD by ozone and preparation method and application thereof |
CN111468105B (en) * | 2020-04-23 | 2023-06-16 | 光大水务科技发展(南京)有限公司 | Multi-layer structure catalyst for catalytic oxidation of nbsCOD by ozone and preparation method and application thereof |
CN113976118A (en) * | 2021-11-30 | 2022-01-28 | 昂星新型碳材料常州有限公司 | Ozone catalyst, preparation method and application thereof |
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