CN106179396A - A kind of composite catalyst of ozone decomposition and preparation method thereof - Google Patents
A kind of composite catalyst of ozone decomposition and preparation method thereof Download PDFInfo
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- CN106179396A CN106179396A CN201610543720.1A CN201610543720A CN106179396A CN 106179396 A CN106179396 A CN 106179396A CN 201610543720 A CN201610543720 A CN 201610543720A CN 106179396 A CN106179396 A CN 106179396A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B01J23/84—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 arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8671—Removing components of defined structure not provided for in B01D53/8603 - B01D53/8668
- B01D53/8675—Ozone
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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Abstract
The preparation method of the composite catalyst of a kind of ozone decomposition, said method comprising the steps of: by permanganate, MnIISalt and CuIISalt the most each dissolves and obtains three kinds of saline solution；It is mixed and stirred for these three saline solution rapidly carrying out redox reaction, is then passed through filtering, cleaning the filtering residue obtaining composite oxides；Described filtering residue addition water is mixed, forms filtering residue and the suspension of water, described suspension is carried out Ultrafine Grinding process, be fully ground after described suspension again through freeze drying process, i.e. obtain the composite catalyst of described ozone decomposition.The method synthesis step of the present invention is few, and synthesis condition is simple, and it is simple that Ultrafine Grinding processes technique, and dispersion effect is good, and the various material mixing and dopings in the composite catalyst prepared are abundant, significantly improve catalytic effect.
Description
Technical field
The present invention relates to the preparation method of a kind of environmental protection and material for air purification, particularly relate to what a kind of catalysis ozone decomposed
Composite catalyst and preparation method thereof.
Background technology
Ozone (O3) a kind of light blue gas having off-odor, be primarily present in away from earth surface 20-35 kilometer is smelly
In oxygen layer, keep out the ultraviolet direct irradiation earth.Under normal circumstances, suck the most useful to human body, but suck excess to people
Body health has certain harm.In GB, in regulation room air, ozone concentration must not exceed 0.08mg/m3, the Gao Yun of ozone
Being permitted concentration is 0.16mg/m3, once exceed this concentration, human body can be damaged.The ozone of excessive concentrations can stimulate breathing
Road, causes the infringement of the aspects such as throat, trachea and lung, can cause visual deterioration, cause fetal anomaly youngster, nerve when situation is serious
The phenomenons such as poisoning.
Owing to having strong oxidizing property, ozone is normally used in the industries such as food, health care and water process playing sterilization
Effect.But, it is difficult to fully erased after usage and is directly discharged to our work and the region of life；It addition, come
Atmospheric environment has been entered into from what the ozone of other equipment such as photocopier, the aspect such as electrion of nature was all difficult to avoid that
In.It addition, popularizing rapidly along with air clearing product, the application of electrostatic precipitation product is more extensive, but at high pressure
Electrostatic precipitation module work during, voltage is the highest, its produce ozone the most, if be not acted upon, excess smelly
Oxygen the most inevitably enters in air, and too much ozone enters in air not only to produce offending odor impact ring
Border, the most seriously damages the health of human body.Ozone owing to producing is difficult to process, and also limit electrostatic precipitation air purifier
Application.
At present, the method having multiple removal ozone pollution, the most representational mainly have medicinal liquid absorption process, solid absorption
Method, photocatalytic method and constant temperature catalyzing method.Its herb liquid absorption method is to use liquid to absorb, it is difficult to be widely applied to smelly in air
The removal of oxygen；Solid absorption method is typically to utilize inorganic porous material to carry out physical absorption, to reach to remove the purpose of ozone, so
And the adsorption capacity of its material is limited, reach saturated after can not be continuing with but also exist and discharge secondary pollution
Risk, is not the very wise move solving ozone pollution problem；Photocatalytic method is typically with the material having catalyticing decomposition action to ozone
Material, owing to it needs the catalytic condition of light, it is difficult to is applied in the environment such as indoor；Constant temperature catalyzing method exists mainly by catalyst
Need not any additional condition catalysis ozone under room temperature decompose to reach the purpose removed, be a kind of permanently effective and practical
Method.
CN 103127942 A discloses a kind of ozone decomposition catalyst and preparation method thereof, with ferrum copper composite oxides
Being main active component, gold, for helping active component, uses Precipitation method to prepare iron/copper-gold composite catalyst, this catalyst pair
Ozone decomposed in room air has higher catalysis activity and stability.On the high side yet with noble metal, it is difficult to
To being widely applied.CN 102513106 B discloses a kind of room-temperature efficient ozone decomposition catalyst and preparation method thereof, its
The middle employing sedimentation method, with potassium carbonate and/or potassium bicarbonate as precipitant, with potassium chlorate as oxidant, precipitation and make activity group
Point, it is subsequently adding N, N-diethyl ethanamine, in a kettle. crystallization under the conditions of 180 DEG C-220 DEG C, through high-temperature roasting technique
Prepare.This preparation technology is numerous and diverse, and the hazardous agents of use is more, is unfavorable for that realizing safe produces, therefore is difficult to carry out industrialization
Produce；And easily cause reunion in last high-temperature roasting technique, reduce the catalysis activity of catalyst.
Summary of the invention
For above-mentioned involved problem, it is an object of the invention to provide a kind of catalysis ozone and decompose the system of composite catalyst
Preparation Method, this preparation method is safe and simple, and has polymolecularity, can efficient catalytic ozone decomposition.This material is dioxy
Change manganese and the catalytic composite material of copper oxide, and various compounding ingredients achieves the compound of lattice level, has the highest urging
Change activity；This composite catalyst has polymolecularity and sufficiently small particle diameter, and the catalytic reaction for ozone provides enough skies
Between.
To achieve these goals, the present invention is that to adopt the following technical scheme that a kind of catalysis ozone of realization decomposes compound
The synthetic method of catalyst, uses manganese and copper to carry out effective being combined and obtains Copper-cladding Aluminum Bar composite oxides, first pass through in solution
Oxidation-reduction method obtains described manganese dioxide and copper oxide composite, then by the above-mentioned composite catalyst of Ultrafine Grinding PROCESS FOR TREATMENT
Obtain the catalytic composite material that dispersion is the highest.
The preparation technology of the catalytic composite material of this ozone decomposition mainly includes the preparation of metal salt solution and oxide
Redox reaction and Ultrafine Grinding dispersing technology in technique, solution, specific as follows: catalysis ozone of the present invention decomposes compound
Catalyst material, it is prepared via a method which: by permanganate, MnIISalt and CuIISalt each dissolves and obtains saline solution；By this
Three kinds of solution are mixed and stirred for rapidly carrying out redox reaction, obtain composite oxides precipitation, are then passed through filtering, cleaning
To filtering residue；Finally described filtering residue addition water is mixed, form filtering residue and the suspension of water, described suspension is carried out ultra-fine
Mill processes, and is fully ground after suspension again through freeze drying process, i.e. obtains high degree of dispersion compound of molecular level mixing
Oxide catalyst.
As preferably, described permanganate can select potassium permanganate；
As preferably, described MnIISalt can select in manganese sulfate, manganese nitrate, manganese carbonate, manganese chloride any one or
Multiple；
As preferably, described CuIISalt can select one or more in copper sulfate, copper nitrate and copper chloride.
As preferably, described permanganate solution compound concentration is 10-30wt%, preferably 10-25wt%；
As preferably, described MnIISaline solution compound concentration is 5-30wt%, preferably 10-20wt%；
As preferably, described CuIISaline solution compound concentration is 3-30wt%, preferably 8-20wt%；
As preferably, described MnIISalt, permanganate and CuIIThe molar ratio of salt is 1:(2.1-4): (0.05-
1), wherein optimum ratio is 1:(2.2-3.5): (0.2-1).
As preferably, the temperature range of described redox reaction is-10-99 DEG C, preferably 10-90 DEG C；
As preferably, the time range of described redox reaction is 0.5-30h, preferably 0.5-20h；
As preferably, during described Ultrafine Grinding processes, spherolite footpath is 0.2-0.5mm, and rotating speed is 1000-2100r/min:
As preferably, in described suspension, solid content is 5wt%-50wt%；
As preferably, the described sufficient time is 30-600min, the most preferably 60-480min；
As preferably, described suspension lyophilization temperature is less than room temperature；
As preferably, described suspension sublimation drying is 5-48h；
Compared with prior art, have the advantage that
1, the synthesis step of catalytic composite material is few, and each raw material is co-precipitated by redox reaction, it is achieved that
Being combined on molecular level；
2, the synthesis condition of catalytic composite material is simple；
3, Ultrafine Grinding processes technique simply, and dispersion effect is good；
4, the various material mixing and dopings in composite catalyst are abundant, significantly improve catalytic effect.
Accompanying drawing explanation
Fig. 1 is the composite catalyst synthesis process flow diagram of ozone decomposition.
Fig. 2 is the transmission electron microscope picture of the composite catalyst of this ozone decomposition.
Detailed description of the invention
Embodiment 1
Being completely dissolved in 100mL pure water by 19.8g manganese chloride tetrahydrate, 34.76g potassium permanganate is completely dissolved in 200mL
In pure water, then 0.25g copper sulphate pentahydrate is dissolved in 50mL pure water, above-mentioned three kinds of solution are fully dissolved stand-by.The most mixed
Closing and state three kinds of solution & stir, after above-mentioned mixed solution is stirred at room temperature reaction 10h, sucking filtration cleans, and obtains combined oxidation
Thing filtering residue.Filtering residue obtained above is joined in Ultrafine Grinding equipment, adds 19g water and obtain the suspension that solid content is 50%,
Selecting the zirconia ball of 0.2mm, the rotating speed arranging Ultrafine Grinding is 2100r/min milled processed 10h.Suspension after grinding
High degree of dispersion composite catalyst powder is obtained after lyophilization 20h under the conditions of-50 DEG C.
Test (see Fig. 2) through SEM, show that the composite catalyst of synthesized ozone decomposition is nanometer materials, its particle diameter
In the range of 20-S0nm.
The divided catalytic ozone decomposition composite catalyst material taking the above-mentioned preparation of 1.00g is placed in the glass tubing of a diameter of 2mm
Catalytic decomposition Performance Evaluation is carried out on interior core.The bottom of glass tubing and air pump (being connected to the gas outlet of ozonator) phase
Even, top is connected with ultraviolet spectrophotometer on-line detector.It is the sky of 100ppm when producing ozone content in ozonator
Being discharged by its gas outlet after gas, ozone-containing air addition is 800mL/min, then with compound in air pump is transported to glass tubing
Catalysis material reacts, and is spilled over to connected ultraviolet spectrophotometer from glass tubing top, by detecting the most again
The content of ozone in tail gas measured by instrument.Testing result shows, in the present embodiment, the high degree of dispersion composite catalyst of preparation is in room temperature
Under the conditions of the ozone of 100ppm is carried out catalytic decomposition efficiency is 90%.
Embodiment 2
Being completely dissolved in 100mL pure water by 7.8g tetra-water manganese sulfate, it is pure that 22.1g potassium permanganate is completely dissolved in 100mL
In water, then 6.03g copper chloride dihydrate is dissolved in 95mL pure water, above-mentioned three kinds of solution are fully dissolved stand-by.Quickly mixing
Above-mentioned three kinds of solution & stir, after above-mentioned mixed solution stirs at 0 DEG C reaction 30h, sucking filtration cleans, and obtains composite oxides
Filtering residue.Filtering residue obtained above is joined in Ultrafine Grinding equipment, adds 36.4g water and obtain the suspension that solid content is 30%,
Selecting the alumina balls of 0.3mm, the rotating speed arranging Ultrafine Grinding is 1500r/min milled processed 6h.Will grind after suspension-
The composite catalyst powder of ozone decomposition is obtained after lyophilization 15h under the conditions of 20 DEG C.
Catalytic performance is tested with embodiment 1, and testing result shows the high degree of dispersion composite catalyst of preparation in the present embodiment
Ozone to 100ppm carries out catalytic decomposition efficiency at ambient temperature is 92%.
Embodiment 3
Being completely dissolved in 130mL pure water by 14.35g six water manganese nitrate, 22.1g potassium permanganate is completely dissolved in 200mL
In pure water, 8.45g nitrate trihydrate copper is completely dissolved in 85mL pure water, above-mentioned three kinds of solution are fully dissolved stand-by.Quickly
Mixing above-mentioned three kinds of solution & stir, after above-mentioned mixed solution stirs at 40 DEG C reaction 5h, sucking filtration cleans, and obtains composite oxygen
Compound filtering residue.Filtering residue obtained above is joined in Ultrafine Grinding equipment, add 187.4g water obtain solid content be 10% outstanding
Turbid liquid, selects the alumina balls of 0.4mm, and the rotating speed arranging Ultrafine Grinding is 1800r/min milled processed 1h.Will grind after suspended
Liquid obtains the composite catalyst powder of ozone decomposition under the conditions of 0 DEG C after lyophilization 30h.
Catalytic performance is tested with embodiment 1, and testing result shows the high degree of dispersion composite catalyst of preparation in the present embodiment
Ozone to 100ppm carries out catalytic decomposition efficiency at ambient temperature is 93%.
Embodiment 4
Being completely dissolved in 150mL pure water by 15g tetra-water manganese sulfate, 26.9g potassium permanganate is completely dissolved in 200mL pure water
In, 5g copper sulphate pentahydrate is completely dissolved in 50mL pure water, above-mentioned three kinds of solution are fully dissolved stand-by.Quickly mixing is above-mentioned
Three kinds of solution & stir, after above-mentioned mixed solution stirs at 30 DEG C reaction 20h, sucking filtration cleans, and obtains composite oxides filter
Slag.Filtering residue obtained above is joined in Ultrafine Grinding equipment, add 407g water and obtain the suspension that solid content is 5%, select
The zirconia ball of 0.5mm, the rotating speed arranging Ultrafine Grinding is 1200r/min milled processed 1h.Suspension after grinding is at 2 DEG C of bars
The composite catalyst powder of ozone decomposition is obtained after lyophilization 5h under part.
Catalytic performance is tested with embodiment 1, and testing result shows the high degree of dispersion composite catalyst of preparation in the present embodiment
Ozone to 100ppm carries out catalytic decomposition efficiency at ambient temperature is 91%.
Embodiment 5
Being completely dissolved in 150mL pure water by 14.35g tetra-water manganese sulfate, 23.7g potassium permanganate is completely dissolved in 200mL
In pure water, 7.5g copper sulphate pentahydrate is completely dissolved in 50mL pure water, above-mentioned three kinds of solution are fully dissolved stand-by.The most mixed
Closing and state three kinds of solution & stir, after above-mentioned mixed solution stirs at 50 DEG C reaction 2h, sucking filtration cleans, and obtains combined oxidation
Thing filtering residue.Filtering residue obtained above is joined in Ultrafine Grinding equipment, adds 69g water and obtain the suspension that solid content is 25%,
Selecting the zirconia ball of 0.2mm, the rotating speed arranging Ultrafine Grinding is 1500r/min milled processed 2h.Suspension after grinding is 5
The composite catalyst powder of ozone decomposition is obtained after lyophilization 8h under the conditions of DEG C.
Catalytic performance is tested with embodiment 1, and testing result shows the high degree of dispersion composite catalyst of preparation in the present embodiment
Ozone to 100ppm carries out catalytic decomposition efficiency at ambient temperature is 94%.
Comparative example 1
Being completely dissolved in 100mL pure water by 19.8g manganese chloride tetrahydrate, 34.76g potassium permanganate is completely dissolved in 200mL
In pure water, then 0.25g copper sulphate pentahydrate is dissolved in 50mL pure water, above-mentioned three kinds of solution are fully dissolved stand-by.The most mixed
Closing and state three kinds of solution & stir, after above-mentioned mixed solution is stirred at room temperature reaction 10h, sucking filtration cleans, and obtains combined oxidation
Thing filtering residue.Filtering residue obtained above is joined in general milling equipment, add 19g water obtain solid content be 50% suspended
Liquid, selects the zirconia ball of 0.2mm, uses general milling to process 10h.Suspension after grinding is freezing under the conditions of-50 DEG C
Obtain catalysis ozone after being dried 20h and decompose composite powder.
Catalytic performance is tested with embodiment 1, and testing result shows that in this comparative example, the composite catalyst of preparation is at room temperature bar
Under part, ozone to 100ppm carries out catalytic decomposition efficiency is 45%.
By above-described embodiment and comparative example 1 it can be seen that through Ultrafine Grinding process composite catalyst ozone is urged
Change capacity of decomposition and be noticeably greater than the composite catalyst not processed through Ultrafine Grinding.This is possibly due in Ultrafine Grinding processing procedure
In, each oxide obtains sufficiently dispersion in the milled processed of high speed high energy, merges into each other, thus has been greatly reinforced multiple
Close the catalytic decomposition ability of catalyst.
Above content is only presently preferred embodiments of the present invention, for those of ordinary skill in the art, according to the present invention's
Thought, the most all will change, and this specification content should not be construed as the present invention
Restriction.
Claims (10)
1. a preparation method for the composite catalyst of ozone decomposition, said method comprising the steps of: by permanganate, MnII
Salt and CuIISalt the most each dissolves and obtains three kinds of saline solution；It is mixed and stirred for these three saline solution rapidly carrying out oxidoreduction
Reaction, is then passed through filtering, cleaning the filtering residue obtaining composite oxides；Described filtering residue addition water is mixed, forms filtering residue
With the suspension of water, described suspension is carried out Ultrafine Grinding process, be fully ground after described suspension again through lyophilization work
Skill, i.e. obtains the composite catalyst of described ozone decomposition.
The preparation method of the composite catalyst of ozone decomposition the most according to claim 1, described permanganate selects height
Potassium manganate.
The preparation method of the composite catalyst of ozone decomposition the most according to claim 1 and 2, described MnIISulfur selected by salt
Any one or more in acid manganese, manganese nitrate, manganese carbonate, manganese chloride.
4. according to the preparation method of the composite catalyst of the ozone decomposition described in any one of claim 1-3, described CuIISalt can
To select one or more in copper sulfate, copper nitrate and copper chloride.
5. according to the preparation method of the composite catalyst of the ozone decomposition described in any one of claim 1-4, described permanganic acid
Saline solution compound concentration is 10-30wt%, preferably 10-25wt%.
6. according to the preparation method of the composite catalyst of the ozone decomposition described in any one of claim 1-5, described MnIISalt is molten
Liquid compound concentration is 5-30wt%, preferably 10-20wt%.
7. according to the preparation method of the composite catalyst of the ozone decomposition described in any one of claim 1-6, described CuIISalt is molten
Liquid compound concentration is 3-30wt%, preferably 8-20wt%.
8. according to the preparation method of the composite catalyst of the ozone decomposition described in any one of claim 1-7, described MnIISalt,
Permanganate and CuIIThe mol ratio of salt is 1: (2.1-4): (0.05-1), and wherein optimum ratio is 1: (2.2-3.5): (0.2-
1)。
9., according to the preparation method of the composite catalyst of the ozone decomposition described in any one of claim 1-8, described oxidation is also
The temperature range of former reaction is-10-99 DEG C, preferably 10-90 DEG C.
10., according to the preparation method of the composite catalyst of the ozone decomposition described in any one of claim 1-9, described oxidation is also
The time range of former reaction is 0.5-30h, preferably 0.5-20h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107456978A (en) * | 2017-09-01 | 2017-12-12 | 深圳市高斯宝电气技术有限公司 | A kind of ozone decomposition catalyst and preparation method thereof |
| CN109772159A (en) * | 2019-03-14 | 2019-05-21 | 中山大学 | A kind of amorphous state manganese oxide catalyst and its preparation method and application |
| CN111744498A (en) * | 2020-05-25 | 2020-10-09 | 广州广钢气体能源股份有限公司 | Manganese-copper composite oxide catalyst and preparation method and application thereof |
| CN112108152A (en) * | 2020-09-23 | 2020-12-22 | 上海化工研究院有限公司 | Catalyst for fish meal odor treatment and preparation method and application thereof |
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| CN102600861A (en) * | 2012-03-26 | 2012-07-25 | 中国科学院生态环境研究中心 | Manganese-based composite oxide catalyst for catalytically decomposing ozone, and preparation method of manganese-based composite oxide catalyst |
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| CN107456978A (en) * | 2017-09-01 | 2017-12-12 | 深圳市高斯宝电气技术有限公司 | A kind of ozone decomposition catalyst and preparation method thereof |
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| CN111744498A (en) * | 2020-05-25 | 2020-10-09 | 广州广钢气体能源股份有限公司 | Manganese-copper composite oxide catalyst and preparation method and application thereof |
| CN111744498B (en) * | 2020-05-25 | 2021-05-25 | 广州广钢气体能源股份有限公司 | Manganese-copper composite oxide catalyst and preparation method and application thereof |
| CN112108152A (en) * | 2020-09-23 | 2020-12-22 | 上海化工研究院有限公司 | Catalyst for fish meal odor treatment and preparation method and application thereof |
| CN112108152B (en) * | 2020-09-23 | 2023-01-24 | 上海化工研究院有限公司 | Catalyst for fish meal odor treatment and preparation method and application thereof |
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| CN106179396B (en) | 2019-02-15 |
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