CN105797741B - A kind of Copper-cladding Aluminum Bar type manganese dioxide-catalyst and preparation method thereof - Google Patents
A kind of Copper-cladding Aluminum Bar type manganese dioxide-catalyst and preparation method thereof Download PDFInfo
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- CN105797741B CN105797741B CN201610033716.0A CN201610033716A CN105797741B CN 105797741 B CN105797741 B CN 105797741B CN 201610033716 A CN201610033716 A CN 201610033716A CN 105797741 B CN105797741 B CN 105797741B
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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
- B01J23/84—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
- B01D53/46—Removing components of defined structure
- B01D53/72—Organic compounds not provided for in groups B01D53/48 - B01D53/70, e.g. hydrocarbons
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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
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/20—Metals or compounds thereof
- B01D2255/207—Transition metals
- B01D2255/2073—Manganese
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/20—Metals or compounds thereof
- B01D2255/207—Transition metals
- B01D2255/20761—Copper
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/702—Hydrocarbons
Abstract
The invention discloses a kind of preparation methods of Copper-cladding Aluminum Bar type manganese dioxide-catalyst, comprising the following steps: permanganate, Mn are added in a solventIIThese three raw materials of salt, copper powder obtain reaction solution, and acid is added makes reaction solution in highly acid, stir and carry out precipitation reaction and obtain the mixed solution containing precursor；Mixed solution after above-mentioned precipitation reaction is added in reaction kettle and carries out hydro-thermal reaction, then through over cleaning, filtering and dry filter residue to get arriving Copper-cladding Aluminum Bar type manganese dioxide-catalyst material.Preparation method of the invention can control the doping of copper, doping reaction sufficiently and can greatly increase the doping of copper.Catalyst prepared by the present invention is Copper-cladding Aluminum Bar manganese dioxide-catalyst material, realizes the doping of lattice copper, considerably increases the activity of its cartalytic decomposition effect.
Description
Technical field
The present invention relates to a kind of functional form inorganic material and preparation method thereof more particularly to a kind of catalysis oxidation Formaldehyde decompositions
Copper-cladding Aluminum Bar type manganese dioxide-catalyst material and preparation method thereof.
Background technique
With the development of science and technology with the progress of human civilization, interior decoration has begun in fashion.And during interior decoration
The pollutants such as produced pollution object formaldehyde are a kind of poisonous and harmful elements, are present in the indoor environment meeting that can be polluted for a long time
Seriously threaten the health of the mankind.
At present there are many method that solves the problems, such as formaldehyde pollution, wherein transition metal oxide especially manganese dioxide by
In cheap and the pollutants such as formaldehyde capable of being effectively catalytically decomposed and have been favored by people.However it is being applied to catalytic decomposition
During pollutant, since the limitation of manganese dioxide self performance causes it to be difficult to reach ideal catalytic degradation effect.
The study found that being doped when using some other metals to manganese dioxide, it is micro- to make it into manganese dioxide
In the lattice for seeing structure, when reapplying in cartalytic decomposition effect, have higher catalytic activity and catalysis faster anti-
Answer rate.So multiple catalysts material all uses doping type manganese dioxide, and doping metals type, doping and doping level
Etc. factors affect the catalytic efficiency of final material.
A kind of preparation method of catalyst for eliminating formaldehyde in air by low-temperature catalytic oxidation is disclosed in 101497042 B of CN,
The catalyst is by manganese oxide, noble metal platinum and auxiliary agent rare earth oxide, alkali or alkaline earth oxide composition, for formaldehyde
It can be at room temperature for carbon dioxide and water by formaldehyde complete oxidation with high catalytic oxidation activity.In this catalyst
The additive and auxiliary agent of type complexity, and the doping only simply mixed without reaching chemical bond level are used；And its
In used noble metal be even more to be difficult to apply because at high cost.It is disclosed in 104001502 A of CN under a kind of room temperature high humility
The preparation method of the cerium Mn catalyst of ozone decomposition is prepared the doping type manganese dioxide containing cerium dopping using precipitation reaction and is urged
Agent CeMnaOx, obtained can effectively ozone decomposition manganese cerium catalyst.Manganese cerium catalyst is in cerium prepared by this method
Doping is not high and doping is also difficult to control.
Summary of the invention
For above-mentioned related problem, the object of the present invention is to provide a kind of doping types of catalysis oxidation Formaldehyde decomposition to urge
The synthetic method of agent material, this preparation method can control the doping of copper, doping reaction sufficiently and can greatly increase copper
Doping.The material is Copper-cladding Aluminum Bar manganese dioxide-catalyst material, realizes the doping of lattice copper, considerably increases its catalysis
The activity of decomposition reaction.
To achieve the goals above, the present invention is a kind of formaldehyde through catalytic oxidation material for adopting the following technical scheme that realization
Synthesis carries out Effective Doping to manganese dioxide using copper.Before being obtained first by the redox reaction in strongly acidic solution
Body, then doping type catalyst material is obtained by the hydro-thermal reaction of high temperature and pressure.
This doping type catalyst material preparation process mainly includes redox reaction and activation in strongly acidic solution
Doping and oxidation reaction technique in reaction process and reaction kettle, it is specific as follows: permanganate, Mn being added in a solventIISalt, copper
These three raw materials of powder obtain reaction solution, and acid, which is added, makes reaction solution in acidity, stirs and carries out precipitation reaction and obtains containing preceding body
The mixed solution of body；Mixed solution after above-mentioned precipitation reaction is added in reaction kettle and carries out hydro-thermal reaction, is then passed through
Cleaning filters and dries filter residue to get Copper-cladding Aluminum Bar type manganese dioxide-catalyst is arrived.
Preferably, the reaction dissolvent can select pure water；
Preferably, the MnIISalt can select manganese sulfate, manganese nitrate, manganese carbonate, in manganese chloride any one or
It is a variety of；
Preferably, the described acid can select sulfuric acid, hydrochloric acid, any one or more in nitric acid；
Preferably, the pH of the reaction solution is 1-4；
Preferably, the mass ratio of the gross mass of thrown raw material and solvent is 9: 10-50 in the precipitation reaction；
Preferably, the MnIIThe molar ratio of salt, potassium permanganate and copper powder is 1: (1.2-3): (0.01-1)；
Preferably, the precipitation reaction temperature is 0-90 DEG C；
Preferably, the precipitation reaction time is 1-30h；
Preferably, the temperature range of hydro-thermal reaction is 100-180 DEG C in the reaction kettle；
Preferably, the time of hydro-thermal reaction is 1-20h in the reaction kettle；
Preferably, the filter residue and drying temperature is 120-200 DEG C；
Preferably, the filter residue and drying time is 2-30h；
Compared with prior art, the present invention has the advantage that
1, use copper powder for copper source, doping ratio is controllable；
2, active copper ion can be obtained in the reaction condition of highly acid, so that reaction efficiency is higher；
3, the reaction under high-temperature and high-pressure conditions is so that doping level is high；
Detailed description of the invention
Fig. 1 is the doping type catalyst material synthesis process flow diagram of the catalysis oxidation Formaldehyde decomposition.
Fig. 2 is the energy spectrum diagram of the doping type catalyst material of the catalysis oxidation Formaldehyde decomposition in embodiment 1.
Fig. 3 is the energy spectrum diagram of the doping type catalyst material of the catalysis oxidation Formaldehyde decomposition in embodiment 2.
Specific embodiment
Embodiment 1
Six water manganese nitrate of 14.35g, 15.8g potassium permanganate and 0.96g copper powder are added into 400g pure water, nitre is added in stirring
The pH to 2.0 of acid-conditioning solution.Continue stirring to be allowed to after reacting 30h at 0 DEG C, mixed solution and the intermediate of internal generation are produced
Object is fully transferred in reaction kettle, then aforesaid reaction vessel is placed under the conditions of 200 DEG C and reacts 1h, is taken after reacting and completing cooling
Out, it cleans, filter and dry gained filter residue is to get arriving Copper-cladding Aluminum Bar manganese dioxide-catalyst material.
It is tested by power spectrum, the content for obtaining each component in the present embodiment product is shown in Table 1, and energy spectrum diagram in detail is as schemed
Shown in 2, show that synthesized Copper-cladding Aluminum Bar manganese dioxide-catalyst material is rod-like nano grade material, and copper is successfully doped into
In the lattice of manganese dioxide.
It prepares the glass tube of a 2mm, in-between position installation sand core conduct support, and bottom and is connected to formaldehyde
The air pump of device is connected, top is connected with gas chromatographic detection instrument, using above-mentioned glass tube as the catalytic performance test of material
Device evaluates the catalytic degradation performance of the material PARA FORMALDEHYDE PRILLS(91,95) of above-mentioned preparation.The Copper-cladding Aluminum Bar manganese dioxide of the above-mentioned preparation of 1.00g is taken to urge
Agent material is put on the sand core in glass tube and is assessed, and sets and generates content of formaldehyde in formaldehyde generator as 120ppm's
Air is transported via air pump to being reacted in glass tube with above-mentioned material, and the tail gas after reaction is entered along glass tube
In gas chromatographic detection instrument, wherein the solubility of removing residue formaldehyde can be then detected.Testing result shows to prepare in the present embodiment
Copper-cladding Aluminum Bar manganese dioxide-catalyst material at room temperature the formaldehyde of 120ppm is carried out that primary efficiency is catalytically decomposed be
92%.
Embodiment 2
1.98g tetrahydrate manganese chloride, 4.74g potassium permanganate and 0.64g copper powder are added into 370g pure water, stirring adds
The pH to 4.0 of sulfuric acid regulation solution.Continue stirring to be allowed to after reacting 1h at 90 DEG C, by mixed solution and the internal centre generated
Product is fully transferred in reaction kettle, then aforesaid reaction vessel is placed under the conditions of 150 DEG C and reacts 10h, completes cooling wait react
After take out, clean, filter and dry gained filter residue to get to Copper-cladding Aluminum Bar manganese dioxide-catalyst material.
It is tested by power spectrum, the content for obtaining each component in the present embodiment product is shown in Table 1, and energy spectrum diagram in detail is as schemed
Shown in 3, show that synthesized Copper-cladding Aluminum Bar manganese dioxide-catalyst material is rod-like nano grade material, and copper is successfully doped into
In the lattice of manganese dioxide.
For catalytic performance test with embodiment 1, testing result shows that the ultra-dispersed composite catalyst prepared in the present embodiment exists
Under room temperature the formaldehyde of 120ppm is carried out that primary efficiency is catalytically decomposed to be 90%.
Embodiment 3
Tetra- water manganese sulfate of 22.3g, 18.96g potassium permanganate and 3.2g copper powder are added into 400g pure water, stirring adds
The pH to 1.0 of hydrochloric acid conditioning solution.Continue stirring to be allowed to after reacting 15h at room temperature, by mixed solution and internal generation
Intermediate product be fully transferred in reaction kettle, then aforesaid reaction vessel is placed under the conditions of 100 DEG C and reacts 20h, wait react
At being taken out after cooling, cleans, filters and dry gained filter residue to get Copper-cladding Aluminum Bar manganese dioxide-catalyst material is arrived.
For catalytic performance test with embodiment 1, testing result shows that the ultra-dispersed composite catalyst prepared in the present embodiment exists
Under room temperature the formaldehyde of 120ppm is carried out that primary efficiency is catalytically decomposed to be 89%.
Embodiment 4
Tetra- water manganese sulfate of 11.15g, 13.43g potassium permanganate and 2.24g copper powder are added into 500g pure water, stirs, then plus
Enter the pH to 3.0 of hydrochloric acid and sulfuric acid regulation solution.Continue stirring to be allowed to after reacting 4h at 60 DEG C, by mixed solution and internal life
At intermediate product be fully transferred in reaction kettle, then aforesaid reaction vessel is placed under the conditions of 120 DEG C and reacts 12h, wait react
It is taken out after completing cooling, clean, filter and dries gained filter residue to get Copper-cladding Aluminum Bar manganese dioxide-catalyst material is arrived.
For catalytic performance test with embodiment 1, testing result shows that the ultra-dispersed composite catalyst prepared in the present embodiment exists
Under room temperature the formaldehyde of 120ppm is carried out that primary efficiency is catalytically decomposed to be 91%.
Comparative example 1
Six water manganese nitrate of 14.35g, 15.8g potassium permanganate and 3.75g cupric sulfate pentahydrate, stirring are added into 400g pure water
It is allowed to after reacting 30h at 0 DEG C, mixed solution and the internal intermediate product generated is fully transferred in reaction kettle, then will be upper
It states under the conditions of reaction kettle is placed in 200 DEG C and reacts 1h, taken out after reacting and completing cooling, clean, filter and dry gained filter residue,
Obtain doping type manganese dioxide-catalyst material.
Through catalytic performance test with embodiment 1, testing result shows that the ultra-dispersed composite catalyst prepared in comparative example 1 exists
Under room temperature the formaldehyde of 120ppm is carried out that primary efficiency is catalytically decomposed to be 79%.
By embodiment 1 with comparative example 1 as can be seen that the present invention uses copper powder anti-as raw material and in acid condition
It answers, active copper ion can be obtained, so that copper is effectively doped in the lattice of manganese dioxide, to substantially increase multiple
Close the catalytic efficiency of catalyst.
Table 1: elemental constituent content detail in product
Above embodiments are merely to illustrate the present invention, and not limitation of the present invention, the common skill in relation to technical field
Art personnel can also make a variety of changes and modification without departing from the spirit and scope of the present invention, therefore all etc.
Same technical solution also belongs to scope of the invention, and scope of patent protection of the invention should be defined by the claims.
Claims (11)
1. a kind of preparation method of Copper-cladding Aluminum Bar type manganese dioxide-catalyst, comprising the following steps: in a solvent be added permanganate,
MnⅡThese three raw materials of salt, copper powder obtain reaction solution, and acid, which is added, makes reaction solution in acidity, and stirring carries out precipitation reaction and obtains
Mixed solution containing precursor；Mixed solution after above-mentioned precipitation reaction is added in reaction kettle and carries out hydro-thermal reaction,
Then through over cleaning, filtering and dry filter residue to get arriving Copper-cladding Aluminum Bar type manganese dioxide-catalyst；The acid selects sulfuric acid, salt
Acid, any one or more in nitric acid, the temperature range of hydro-thermal reaction is 100-180 DEG C in the reaction kettle, described
The time of hydro-thermal reaction is 1-20h in reaction kettle.
2. the preparation method of Copper-cladding Aluminum Bar type manganese dioxide-catalyst according to claim 1, wherein the solvent selects pure water.
3. the preparation method of Copper-cladding Aluminum Bar type manganese dioxide-catalyst according to claim 1, wherein the MnⅡSalt selects sulphur
Sour manganese, manganese nitrate, manganese carbonate, any one or more in manganese chloride.
4. the preparation method of Copper-cladding Aluminum Bar type manganese dioxide-catalyst according to claim 1, wherein the pH of the reaction solution is
1-4。
5. the preparation method of Copper-cladding Aluminum Bar type manganese dioxide-catalyst according to claim 1, wherein in the precipitation reaction
The gross mass of thrown raw material and the ratio of solvent quality are 9:10-50.
6. the preparation method of Copper-cladding Aluminum Bar type manganese dioxide-catalyst according to claim 1, wherein the MnⅡSalt, Gao Meng
The molar ratio of sour potassium and copper powder is 1:(1.2-3): (0.01-1).
7. the preparation method of Copper-cladding Aluminum Bar type manganese dioxide-catalyst according to claim 1, wherein the precipitation reaction temperature
Degree is 0-90 DEG C.
8. the preparation method of Copper-cladding Aluminum Bar type manganese dioxide-catalyst according to claim 1, wherein when the described precipitation reaction
Between be 1-30h.
9. the preparation method of Copper-cladding Aluminum Bar type manganese dioxide-catalyst according to claim 1, wherein the filter residue and drying temperature
Degree is 120-200 DEG C.
10. the preparation method of Copper-cladding Aluminum Bar type manganese dioxide-catalyst according to claim 1, wherein when the described filter residue and drying
Between be 2-30h.
11. a kind of Copper-cladding Aluminum Bar type manganese dioxide-catalyst, which is characterized in that the catalyst is according to claim 1 any one of -10
The preparation method preparation of Copper-cladding Aluminum Bar type manganese dioxide-catalyst described in claim.
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| CN105618081A (en) * | 2016-01-31 | 2016-06-01 | 内蒙古工业大学 | Rare earth metal La doped copper manganese catalyst and experiment method thereof |
| CN107768778A (en) * | 2016-08-19 | 2018-03-06 | 中国科学院上海高等研究院 | 3 D stereo manganese bioxide electrode material and its preparation method and application |
| CN106423191A (en) * | 2016-08-30 | 2017-02-22 | 宁波钛安新材料科技有限公司 | Health-care air-purifying composite catalyst material and preparation method thereof |
| CN106334565B (en) * | 2016-10-12 | 2020-06-09 | 友好净控科技（浙江）有限公司 | Air purification composite catalyst and preparation method thereof |
| CN109126771B (en) * | 2018-08-31 | 2021-09-14 | 西南交通大学 | Non-noble metal VOCs catalyst and preparation method thereof |
| CN110639551A (en) * | 2019-09-26 | 2020-01-03 | 复旦大学 | Monolithic catalyst for removing benzene series at low temperature and preparation method thereof |
| CN112619663A (en) * | 2020-09-10 | 2021-04-09 | 何俊 | Cobalt or copper doped birnessite catalyst, preparation method and application thereof |
| CN115851024A (en) * | 2022-12-16 | 2023-03-28 | 海啊科技股份有限公司 | Antibacterial and aldehyde-removing spray for automobile foot pads |
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| CN102626636A (en) * | 2012-03-22 | 2012-08-08 | 杭州中环化工设备有限公司 | Nanometer manganese dioxide-copper oxide composite catalyst and its application |
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| CN102626636A (en) * | 2012-03-22 | 2012-08-08 | 杭州中环化工设备有限公司 | Nanometer manganese dioxide-copper oxide composite catalyst and its application |
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