CN110813312A - Magnetic nano composite material and preparation method and application thereof - Google Patents
Magnetic nano composite material and preparation method and application thereof Download PDFInfo
- Publication number
- CN110813312A CN110813312A CN201911090109.8A CN201911090109A CN110813312A CN 110813312 A CN110813312 A CN 110813312A CN 201911090109 A CN201911090109 A CN 201911090109A CN 110813312 A CN110813312 A CN 110813312A
- Authority
- CN
- China
- Prior art keywords
- magnetic
- magnetic core
- mesoporous layer
- water
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 50
- 239000000463 material Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 108
- 238000006243 chemical reaction Methods 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910000510 noble metal Inorganic materials 0.000 claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 44
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 26
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 20
- 239000002904 solvent Substances 0.000 claims description 17
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 10
- 239000002202 Polyethylene glycol Substances 0.000 claims description 10
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 10
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 10
- 229920001223 polyethylene glycol Polymers 0.000 claims description 10
- SZEMGTQCPRNXEG-UHFFFAOYSA-M trimethyl(octadecyl)azanium;bromide Chemical compound [Br-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C SZEMGTQCPRNXEG-UHFFFAOYSA-M 0.000 claims description 10
- 239000012279 sodium borohydride Substances 0.000 claims description 9
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 9
- 238000011068 loading method Methods 0.000 claims description 8
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical group Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 claims description 8
- 239000011148 porous material Substances 0.000 claims description 8
- 238000000354 decomposition reaction Methods 0.000 claims description 6
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 5
- 239000003638 chemical reducing agent Substances 0.000 claims description 5
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 5
- 150000003057 platinum Chemical class 0.000 claims description 5
- 239000001632 sodium acetate Substances 0.000 claims description 5
- 235000017281 sodium acetate Nutrition 0.000 claims description 5
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000011162 core material Substances 0.000 claims description 4
- 239000000696 magnetic material Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 229910000859 α-Fe Inorganic materials 0.000 claims description 4
- 229910016516 CuFe2O4 Inorganic materials 0.000 claims description 2
- 229910017163 MnFe2O4 Inorganic materials 0.000 claims description 2
- 229910003264 NiFe2O4 Inorganic materials 0.000 claims description 2
- 229910001308 Zinc ferrite Inorganic materials 0.000 claims description 2
- DXKGMXNZSJMWAF-UHFFFAOYSA-N copper;oxido(oxo)iron Chemical compound [Cu+2].[O-][Fe]=O.[O-][Fe]=O DXKGMXNZSJMWAF-UHFFFAOYSA-N 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- NQNBVCBUOCNRFZ-UHFFFAOYSA-N nickel ferrite Chemical compound [Ni]=O.O=[Fe]O[Fe]=O NQNBVCBUOCNRFZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 8
- 239000003054 catalyst Substances 0.000 abstract description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 5
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 abstract description 5
- 239000001569 carbon dioxide Substances 0.000 abstract description 4
- 239000013067 intermediate product Substances 0.000 abstract description 2
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 15
- 238000001179 sorption measurement Methods 0.000 description 13
- 238000004140 cleaning Methods 0.000 description 10
- 239000002105 nanoparticle Substances 0.000 description 10
- 238000003756 stirring Methods 0.000 description 10
- 239000011258 core-shell material Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 6
- 229940040526 anhydrous sodium acetate Drugs 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 229940044631 ferric chloride hexahydrate Drugs 0.000 description 5
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- 229940032296 ferric chloride Drugs 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 206010007269 Carcinogenicity Diseases 0.000 description 1
- BDAGIHXWWSANSR-UHFFFAOYSA-N Formic acid Chemical compound OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 1
- 241000282412 Homo Species 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 239000012494 Quartz wool Substances 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 206010043275 Teratogenicity Diseases 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 231100000260 carcinogenicity Toxicity 0.000 description 1
- 230000007670 carcinogenicity Effects 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000002734 clay mineral Chemical class 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 231100000211 teratogenicity Toxicity 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
Images
Classifications
-
- 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
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8906—Iron and noble metals
-
- 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
-
- B01J35/23—
-
- B01J35/33—
-
- B01J35/397—
-
- B01J35/399—
-
- B01J35/615—
-
- B01J35/647—
-
- 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
- B01D2257/704—Solvents not covered by groups B01D2257/702 - B01D2257/7027
-
- 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
- B01D2257/708—Volatile organic compounds V.O.C.'s
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Environmental & Geological Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a magnetic nano composite material and a preparation method and application thereof. The magnetic nano composite material comprises a magnetic core and a mesoporous layer wrapped on the surface of the magnetic core, wherein noble metal is loaded on the mesoporous layer, the magnetic nano composite material has high conversion rate and selectivity on formaldehyde, secondary pollution caused by intermediate products generated in the reaction process is avoided, formaldehyde can be completely catalytically converted into carbon dioxide and water at room temperature, the catalyst can be recycled through an external magnetic field, and the cost is reduced. The preparation method is simple, and can control the cost at a very low level.
Description
Technical Field
The invention belongs to the technical field of composite material preparation, particularly relates to a magnetic nano composite material, a preparation method and application thereof, and particularly relates to a magnetic core-shell structure nano composite material for catalyzing formaldehyde decomposition and a preparation method thereof.
Background
With the gradual improvement of living standard of people, the home decoration and arrangement of people are gradually increased, and the building decoration and arrangement materials are also the main sources of formaldehyde pollution in indoor environment. Formaldehyde is a highly toxic substance for humans and animals. The world health organization confirms that formaldehyde has carcinogenicity and teratogenicity, and the definition limit of formaldehyde in a room is less than 0.1mg/m3. The harm degree of formaldehyde to human bodies is positively correlated with the concentration of formaldehyde contacted with human bodies and the time of contacting the formaldehyde, and the larger the sum of the formaldehyde contacted with human bodies is, the longer the time is, the greater the harm to the human bodies is.
At present, a simple, convenient and fast means for reducing the indoor formaldehyde content is needed, and the indoor formaldehyde purification method mainly comprises the following methods: a photocatalytic method and an adsorption method, wherein the photocatalytic method mainly irradiates formaldehyde adsorbed on a catalyst by ultraviolet light with the wavelength of less than 380nm, so that the formaldehyde is oxidized and decomposed into water and carbon dioxide under the action of light. However, byproducts such as CO, HCOOH and the like are easy to exist in the reaction process of photocatalytic oxidation of formaldehyde, and secondary pollution is easy to cause. And the method needs to be carried out under the condition of ultraviolet light, has harsh requirements and high energy consumption, and is not suitable for popularization in common houses.
The adsorption method is to adsorb formaldehyde in the indoor air to the surface by using a substance with strong adsorption capacity through a physical adsorption method, so as to reduce the concentration of the formaldehyde in the indoor environment and purify the indoor air. Generally speaking, the higher the specific surface area, the higher the surface energy of the material, and the stronger the adsorption capacity, and the commonly used adsorption materials are gamma-alumina, activated carbon, modified metal oxides, clay minerals, etc. The adsorption method has better formaldehyde removal efficiency, can automatically adsorb and reduce the concentration of formaldehyde in the indoor environment, and is simple and convenient to operate. The method has the defects that the adsorption method does not convert and eliminate the pollutants, but only absorbs the pollutants into the adsorption material by the adsorption method, and when the adsorption material is saturated, the adsorption method cannot continuously adsorb the formaldehyde. And secondly, the adsorption method is greatly influenced by environmental conditions, and adsorbed formaldehyde is desorbed under certain conditions and enters the indoor environment again to cause secondary pollution.
Disclosure of Invention
Therefore, the invention aims to overcome the defects that the conversion rate and selectivity of formaldehyde decomposition are required to be improved in the existing formaldehyde removal method, and further provides a magnetic nano composite material, and a preparation method and application thereof.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
the magnetic nano composite material provided by the invention comprises a magnetic core and a mesoporous layer wrapped on the surface of the magnetic core, wherein noble metal is loaded on the mesoporous layer.
Further, the loading amount of the noble metal on the mesoporous layer is 0.25 wt% to 0.35 wt%.
Further, the mesoporous layer has a specific surface area of 220m3/g-280m3(ii)/g, the average pore diameter is 2-4 nm.
Further, the size of the magnetic core is 200nm-250 nm;
the thickness of the mesoporous layer is 30nm-50 nm.
Furthermore, the magnetic core is made of a ferrite magnetic material; preferably, the ferrite magnetic material is Fe3O4、MnFe2O4、NiFe2O4、CuFe2O4、ZnFe2O4At least one of;
the mesoporous layer is made of silicon dioxide and/or titanium dioxide; the noble metal is at least one of platinum, palladium and gold.
In addition, the invention also provides a preparation method of the magnetic nano composite material, which comprises the following steps: preparing a magnetic core; wrapping a mesoporous layer on the magnetic core; and (3) soaking the magnetic core wrapped with the mesoporous layer in a salt solution of noble metal to prepare the magnetic nano composite material.
Further, the magnetic core is Fe3O4The preparation method comprises the following steps of:
dissolving ferric chloride, sodium acetate and polyethylene glycol in a first solvent to carry out a first reaction to prepare Fe3O4A magnetic core;
mixing Fe3O4Dispersing the magnetic core in a second solvent, adding ammonia water, octadecyl trimethyl ammonium bromide and tetraethyl orthosilicate, and sequentially performing second reaction and calcination to prepare the magnetic core wrapping the mesoporous layer;
and dispersing the magnetic core wrapped with the mesoporous layer into a third solvent, adding soluble platinum salt and a reducing agent, and carrying out a third reaction to obtain the magnetic nano composite material.
Further, the first solvent is ethylene glycol; the ratio of the ferric chloride, the sodium acetate, the polyethylene glycol and the first solvent is (1.35-13.5) g: (1-10) g: (1-10) g: (40-250) mL; the temperature of the first reaction is 180-220 ℃, and the time is 7-8 h;
the second solvent comprises ethanol and water, and the volume ratio of the ethanol to the water is (80-400): (20-100), said Fe3O4The proportion of the magnetic core, ethanol, water, ammonia water, octadecyl trimethyl ammonium bromide and tetraethyl orthosilicate is (0.1-1) g: (80-400) ml: (20-100) ml: (1-20) ml: (0.2-4) g: (0.2-4) ml; the temperature of the second reaction is 20-30 ℃, and the time is 5-8 h; the calcining temperature is 280-320 ℃, and the time is 5-7 h.
Further, the third solvent comprises ethanol and water, and the volume ratio of the ethanol to the water is (50-400): (20-120), the soluble platinum salt is platinum chloride, and the reducing agent is sodium borohydride;
said Fe3O4The proportion of the magnetic core, ethanol, water, platinum chloride and sodium borohydride is (0.1-1) g: (50-400) ml: (20-120) ml: (10-100) mg: (10-100) mg; the temperature of the third reaction is 20-30 ℃, and the time is 10-14 h.
In addition, the invention also provides application of the magnetic nano composite material in catalyzing formaldehyde decomposition.
Compared with the prior art, the invention has the following beneficial effects:
(1) the magnetic nano composite material provided by the invention comprises a magnetic core and a mesoporous layer wrapped on the surface of the magnetic core, wherein noble metal is loaded on the mesoporous layer, the magnetic nano composite material has high conversion rate and selectivity on formaldehyde, secondary pollution caused by intermediate products generated in the reaction process is avoided, formaldehyde can be completely catalytically converted into carbon dioxide and water at room temperature, the catalyst can be recycled through an external magnetic field, and the cost is reduced.
(2) The magnetic nano composite material provided by the invention can continuously decompose adsorbed formaldehyde, so that the service life is greatly prolonged; the mesoporous layer has a proper specific surface area and ordered mesoporous channels, and the noble metal can be effectively dispersed in the channels, so that the activity reduction caused by the agglomeration of the noble metal can be prevented. Thereby providing enough space for absorbing a large amount of formaldehyde to carry out catalytic reaction. The surface of the mesoporous layer and the inside of the pore channel are loaded with noble metal catalysts, so that good loading performance of the catalysts is ensured, and nano noble metal particles are prevented from falling off from the surface.
(3) The magnetic nano composite material provided by the invention takes simple and easily-obtained metal oxide and trace precious metal as raw materials, the preparation method is simple, and the cost can be controlled at a very low level.
(4) The preparation method of the magnetic nano composite material provided by the invention comprises the steps of dissolving ferric chloride, sodium acetate and polyethylene glycol in a first solvent, and carrying out a first reaction to prepare Fe3O4A magnetic core; mixing Fe3O4Dispersing the magnetic core in a second solvent, adding ammonia water, octadecyl trimethyl ammonium bromide and tetraethyl orthosilicate, and sequentially performing second reaction and calcination to prepare the magnetic core wrapping the mesoporous layer; will wrap up the mesoporous layerThe magnetic core is dispersed in a third solvent, soluble platinum salt and a reducing agent are added to carry out a third reaction, and the magnetic nano composite material is prepared. The preparation method is beneficial to preparing the magnetic nano composite material with uniform structure and uniform noble metal load.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 shows a magnetic nanocomposite (Fe) in an embodiment of the present invention3O4@SiO2-Pt);
FIG. 2 is a partially enlarged TEM image of the magnetic nanocomposite material of FIG. 1.
Detailed Description
The technical solutions of the present invention are described clearly and completely below, and it is obvious that the described embodiments are some, not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The embodiment provides a magnetic nanocomposite material and a preparation method thereof. The preparation method comprises the following steps:
(1) dissolving 1.35g of ferric chloride hexahydrate, 1.0g of anhydrous sodium acetate and 1.0g of polyethylene glycol into 40mL of ethylene glycol, then pouring the uniformly mixed solution into a reaction kettle to react for 8 hours at 200 ℃, and after the reaction is finished, magnetically separating and cleaning the product for several times to obtain ferroferric oxide nanoparticles;
(2) dispersing 0.1g of ferroferric oxide nano particles in 80mL of ethanol and 20mL of water, adding 1mL of ammonia water, 0.2g of octadecyl trimethyl ammonium bromide and 0.2mL of tetraethyl orthosilicate, mechanically stirring for 6 hours at room temperature, and after the reaction is finished, magnetically separating and cleaning the product for several times; then calcining the product at 300 ℃ for 6h to obtain a powdery substance, namely a nano composite material coated with nanoscale ordered mesoporous silica-a magnetic core coated with a mesoporous layer;
(3) finally, dispersing the magnetic core wrapping the mesoporous layer in 50mL of ethanol and 20mL of water, adding 10mg of platinum chloride, adding 10mg of sodium borohydride at room temperature, mechanically stirring for reaction for 12 hours at room temperature to finally obtain the magnetic core-shell structure nanocomposite, and testing to show that the TEM of the magnetic core-shell structure nanocomposite is 250nm in size as shown in figures 1 and 2; the thickness of the mesoporous layer is 30nm, and the specific surface area is 250m3(ii)/g, average pore diameter 3 nm; the loading of noble metal on the mesoporous layer was 0.3 wt%.
Example 2
The embodiment provides a magnetic nanocomposite material and a preparation method thereof. The preparation method comprises the following steps:
(1) dissolving 13.5g of ferric chloride hexahydrate, 10g of anhydrous sodium acetate and 10g of polyethylene glycol into 250mL of ethylene glycol, then pouring the uniformly mixed solution into a reaction kettle to react for 8 hours at 200 ℃, and after the reaction is finished, magnetically separating and cleaning the product for several times to obtain ferroferric oxide nanoparticles;
(2) dispersing 1g of ferroferric oxide nano particles in 400mL of ethanol and 100mL of water, adding 20mL of ammonia water, 4g of octadecyl trimethyl ammonium bromide and 4mL of tetraethyl orthosilicate, mechanically stirring for 6 hours at room temperature, and after the reaction is finished, magnetically separating and cleaning the product for several times; then calcining the product at 300 ℃ for 6h to obtain a powdery substance, namely a nano composite material coated with nanoscale ordered mesoporous silica-a magnetic core coated with a mesoporous layer;
(3) finally, dispersing the magnetic core wrapping the mesoporous layer in 400mL of ethanol and 120mL of water, adding 100mg of platinum chloride, adding 100mg of sodium borohydride at room temperature, mechanically stirring for reaction at room temperature for 12 hours to finally obtain the magnetic core-shell structure nanocomposite, wherein the size of the magnetic core is 200nm through testing; the thickness of the mesoporous layer is 50 nm/LSurface area of 280m3(ii)/g, average pore diameter of 2 nm; the loading of noble metal on the mesoporous layer was 0.35 wt%.
Example 3
The embodiment provides a magnetic nanocomposite material and a preparation method thereof. The preparation method comprises the following steps:
(1) dissolving 7g of ferric chloride hexahydrate, 6g of anhydrous sodium acetate and 6g of polyethylene glycol into 150mL of ethylene glycol, then pouring the uniformly mixed solution into a reaction kettle to react for 7 hours at 220 ℃, and after the reaction is finished, magnetically separating and cleaning the product for several times to obtain ferroferric oxide nanoparticles;
(2) dispersing 0.5g of ferroferric oxide nano particles in 240mL of ethanol and 60mL of water, adding 10mL of ammonia water, 2g of octadecyl trimethyl ammonium bromide and 2mL of tetraethyl orthosilicate, mechanically stirring for 5 hours at 30 ℃, and after the reaction is finished, magnetically separating and cleaning the product for several times; then calcining the product at 280 ℃ for 7h to obtain a powdery substance, namely a nano composite material coated with nanoscale ordered mesoporous silica-a magnetic core coated with a mesoporous layer;
(3) finally, dispersing the magnetic core wrapping the mesoporous layer in 230mL of ethanol and 70mL of water, adding 60mg of platinum chloride, adding 50mg of sodium borohydride at 20 ℃, mechanically stirring for reaction for 14h at 20 ℃, and finally obtaining the magnetic core-shell structure nanocomposite, wherein the size of the magnetic core is 220nm through testing; the thickness of the mesoporous layer is 40nm, and the specific surface area is 220m3(ii)/g, average pore diameter 4 nm; the loading of noble metal on the mesoporous layer was 0.25 wt%.
Example 4
The embodiment provides a magnetic nanocomposite material and a preparation method thereof. The preparation method comprises the following steps:
(1) dissolving 5g of ferric chloride hexahydrate, 8g of anhydrous sodium acetate and 3g of polyethylene glycol into 200mL of ethylene glycol, then pouring the uniformly mixed solution into a reaction kettle to react for 8 hours at 180 ℃, and after the reaction is finished, magnetically separating and cleaning the product for several times to obtain ferroferric oxide nanoparticles;
(2) dispersing 0.8g of ferroferric oxide nano particles in 180mL of ethanol and 80mL of water, adding 17mL of ammonia water, 1g of octadecyl trimethyl ammonium bromide and 3mL of tetraethyl orthosilicate, mechanically stirring for 8 hours at 20 ℃, and after the reaction is finished, magnetically separating and cleaning the product for several times; then calcining the product at 320 ℃ for 5 hours to obtain a powdery substance, namely a nano composite material coated with nanoscale ordered mesoporous silica-a magnetic core coated with a mesoporous layer;
(3) finally, dispersing the magnetic core wrapping the mesoporous layer in 350mL of ethanol and 50mL of water, adding 80mg of platinum chloride, adding 90mg of sodium borohydride at 30 ℃, mechanically stirring for reaction for 10 hours at 30 ℃, and finally obtaining the magnetic core-shell structure nanocomposite, wherein the size of the magnetic core is 240nm through testing; the thickness of the mesoporous layer is 38nm, and the specific surface area is 260m3(ii)/g, average pore diameter of 2 nm; the loading of noble metal on the mesoporous layer was 0.32 wt%.
Example 5
The embodiment provides a magnetic nanocomposite material and a preparation method thereof. The preparation method comprises the following steps:
(1) dissolving 10g of ferric chloride hexahydrate, 4g of anhydrous sodium acetate and 6g of polyethylene glycol into 100mL of ethylene glycol, then pouring the uniformly mixed solution into a reaction kettle to react for 8 hours at 210 ℃, and after the reaction is finished, magnetically separating and cleaning the product for several times to obtain ferroferric oxide nanoparticles;
(2) dispersing 0.3g of ferroferric oxide nano particles in 300mL of ethanol and 40mL of water, adding 8mL of ammonia water, 3g of octadecyl trimethyl ammonium bromide and 1.8mL of tetraethyl orthosilicate, mechanically stirring for 8h at 24 ℃, and after the reaction is finished, magnetically separating and cleaning the product for several times; then calcining the product at 310 ℃ for 7h to obtain a powdery substance, namely a nano composite material coated with nanoscale ordered mesoporous silica-a magnetic core coated with a mesoporous layer;
(3) finally, dispersing the magnetic core wrapping the mesoporous layer in 150mL of ethanol and 100mL of water, adding 40mg of palladium chloride, adding 50mg of sodium borohydride at 30 ℃, mechanically stirring for reaction for 10 hours at 30 ℃, and finally obtaining the magnetic core-shell structure nanocomposite, wherein the size of the magnetic core is 210nm through testing; the thickness of the mesoporous layer is33nm and a specific surface area of 235m3(ii)/g, average pore diameter of 2.8 nm; the loading of noble metal on the mesoporous layer was 0.26 wt%.
Comparative example 1
The present comparative example provides a magnetic nanocomposite material and a method of making the same. The preparation method is the same as example 1, and only differs from the following steps: in this comparative example, step (2) in example 1 was not performed.
Test example 1
The magnetic nanocomposites prepared in examples 1-5 and comparative example 1 above were tested for catalytic performance by the following test methods: 0.3g of the magnetic nanocomposite prepared above was placed on quartz wool in a metal tube of 5mm diameter for catalytic decomposition activity evaluation, the bottom of the metal tube was connected to a formaldehyde generator, and the top was connected to an infrared spectrometer. The method comprises the following steps of blowing compressed air into a formaldehyde generator, mixing the air with formaldehyde to obtain air with the formaldehyde concentration of 100ppm, enabling the air containing the formaldehyde to enter a metal pipe filled with a catalyst from the bottom, and then enabling the air to enter an infrared spectrometer from the top to detect the concentrations of the formaldehyde and the carbon dioxide, wherein the test results are shown in the following table 1:
TABLE 1
| Conversion rate of formaldehyde decomposition | CO2Selectivity of (2) | |
| Example 1 | 98.5％ | 98.4％ |
| Example 2 | 97.8％ | 97.6％ |
| Example 3 | 98.1％ | 97.8％ |
| Example 4 | 97.5％ | 97.3％ |
| Example 5 | 93.0％ | 92.9％ |
| Comparative example 1 | 40.9％ | 35.9％ |
Note: the conversion of formaldehyde decomposition ═ total molar amount of formaldehyde-molar amount of undecomposed formaldehyde)/total molar amount of formaldehyde; CO 22Selectivity of (2) CO production2Molar amount of (a)/total molar amount of formaldehyde.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. A magnetic nano composite material comprises a magnetic inner core and a mesoporous layer wrapping the surface of the magnetic inner core, wherein noble metal is loaded on the mesoporous layer.
2. The magnetic nanocomposite of claim 1, wherein the loading of noble metal on the mesoporous layer is between 0.25 wt% and 0.35 wt%.
3. The magnetic nanocomposite material according to claim 1 or 2, wherein the mesoporous layer has a specific surface area of 220m3/g-280m3(ii)/g, the average pore diameter is 2-4 nm.
4. The magnetic nanocomposite material of any of claims 1-3, wherein the magnetic core has a size of 200nm to 250 nm;
the thickness of the mesoporous layer is 30nm-50 nm.
5. The magnetic nanocomposite material of claim 4, wherein the magnetic core is made of a ferrite magnetic material; preferably, the ferrite magnetic material is Fe3O4、MnFe2O4、NiFe2O4、CuFe2O4、ZnFe2O4At least one of;
the mesoporous layer is made of silicon dioxide and/or titanium dioxide; the noble metal is at least one of platinum, palladium and gold.
6. A method of preparing a magnetic nanocomposite material as claimed in any of claims 1 to 5, comprising the steps of: preparing a magnetic core; wrapping a mesoporous layer on the magnetic core; and (3) soaking the magnetic core wrapped with the mesoporous layer in a salt solution of noble metal to prepare the magnetic nano composite material.
7. The method of claim 6, wherein the magnetic core is Fe3O4The preparation method comprises the following steps of:
dissolving ferric chloride, sodium acetate and polyethylene glycol in a first solvent to perform a first reactionTo obtain Fe3O4A magnetic core;
mixing Fe3O4Dispersing the magnetic core in a second solvent, adding ammonia water, octadecyl trimethyl ammonium bromide and tetraethyl orthosilicate, and sequentially performing second reaction and calcination to prepare the magnetic core wrapping the mesoporous layer;
and dispersing the magnetic core wrapped with the mesoporous layer into a third solvent, adding soluble platinum salt and a reducing agent, and carrying out a third reaction to obtain the magnetic nano composite material.
8. The method of claim 7, wherein the first solvent is ethylene glycol; the ratio of the ferric chloride, the sodium acetate, the polyethylene glycol and the first solvent is (1.35-13.5) g: (1-10) g: (1-10) g: (40-250) mL; the temperature of the first reaction is 180-220 ℃, and the time is 7-8 h;
the second solvent comprises ethanol and water, and the volume ratio of the ethanol to the water is (80-400): (20-100), said Fe3O4The proportion of the magnetic core, ethanol, water, ammonia water, octadecyl trimethyl ammonium bromide and tetraethyl orthosilicate is (0.1-1) g: (80-400) ml: (20-100) ml: (1-20) ml: (0.2-4) g: (0.2-4) ml; the temperature of the second reaction is 20-30 ℃, and the time is 5-8 h; the calcining temperature is 280-320 ℃, and the time is 5-7 h.
9. The method according to claim 7 or 8, wherein the third solvent comprises ethanol and water, and the volume ratio of the ethanol to the water is (50-400): (20-120), the soluble platinum salt is platinum chloride, and the reducing agent is sodium borohydride;
said Fe3O4The proportion of the magnetic core, ethanol, water, platinum chloride and sodium borohydride is (0.1-1) g: (50-400) ml: (20-120) ml: (10-100) mg: (10-100) mg; the temperature of the third reaction is 20-30 ℃, and the time is 10-14 h.
10. Use of the magnetic nanocomposite material of any one of claims 1 to 5 for catalyzing formaldehyde decomposition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911090109.8A CN110813312A (en) | 2019-11-08 | 2019-11-08 | Magnetic nano composite material and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911090109.8A CN110813312A (en) | 2019-11-08 | 2019-11-08 | Magnetic nano composite material and preparation method and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110813312A true CN110813312A (en) | 2020-02-21 |
Family
ID=69554007
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911090109.8A Pending CN110813312A (en) | 2019-11-08 | 2019-11-08 | Magnetic nano composite material and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110813312A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114100341A (en) * | 2020-08-31 | 2022-03-01 | 宁波方太厨具有限公司 | Formaldehyde eliminating agent and preparation method thereof |
| CN116371414A (en) * | 2023-04-04 | 2023-07-04 | 华中科技大学 | High-temperature stable reduction-resistant cerium oxide-nickel ferrite composite catalyst and preparation method and application thereof |
| CN116371414B (en) * | 2023-04-04 | 2024-05-10 | 华中科技大学 | High-temperature stable reduction-resistant cerium oxide-nickel ferrite composite catalyst and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106111208A (en) * | 2016-05-13 | 2016-11-16 | 宁波大学 | A kind of magnetic Nano microsphere/polypyrrole palladium composite material of core-shell structure and preparation method thereof |
| CN106311274A (en) * | 2016-07-29 | 2017-01-11 | 武汉工程大学 | Magnetic nanoparticles catalyst used for p-nitrophenol of catalysis hydrogenation and preparing method and application thereof |
| CN107096545A (en) * | 2017-04-27 | 2017-08-29 | 扬州大学 | A kind of preparation method of yolk eggshell structural composite material |
| CN110152683A (en) * | 2019-05-27 | 2019-08-23 | 西北工业大学 | One kind can rotation magnetic nano chain supported palladium nano-particle catalyst and preparation method thereof |
-
2019
- 2019-11-08 CN CN201911090109.8A patent/CN110813312A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106111208A (en) * | 2016-05-13 | 2016-11-16 | 宁波大学 | A kind of magnetic Nano microsphere/polypyrrole palladium composite material of core-shell structure and preparation method thereof |
| CN106311274A (en) * | 2016-07-29 | 2017-01-11 | 武汉工程大学 | Magnetic nanoparticles catalyst used for p-nitrophenol of catalysis hydrogenation and preparing method and application thereof |
| CN107096545A (en) * | 2017-04-27 | 2017-08-29 | 扬州大学 | A kind of preparation method of yolk eggshell structural composite material |
| CN110152683A (en) * | 2019-05-27 | 2019-08-23 | 西北工业大学 | One kind can rotation magnetic nano chain supported palladium nano-particle catalyst and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114100341A (en) * | 2020-08-31 | 2022-03-01 | 宁波方太厨具有限公司 | Formaldehyde eliminating agent and preparation method thereof |
| CN116371414A (en) * | 2023-04-04 | 2023-07-04 | 华中科技大学 | High-temperature stable reduction-resistant cerium oxide-nickel ferrite composite catalyst and preparation method and application thereof |
| CN116371414B (en) * | 2023-04-04 | 2024-05-10 | 华中科技大学 | High-temperature stable reduction-resistant cerium oxide-nickel ferrite composite catalyst and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Nie et al. | Room-temperature catalytic oxidation of formaldehyde on catalysts | |
| CN108514878B (en) | Monoatomic noble metal catalyst, preparation method thereof and application thereof in low-temperature catalytic oxidation of formaldehyde | |
| CN104338528A (en) | Preparation of room temperature formaldehyde catalyst | |
| WO2016041380A1 (en) | Supported catalyst suitable for purifying air at normal temperature | |
| CN105473221A (en) | Catalysts for oxidation of carbon monoxide and/or volatile organic compounds | |
| US5068217A (en) | Carrier catalysts for oxidizing carbon monoxide and process for their production | |
| CN107398272A (en) | A kind of formaldehyde room temperature catalysis composite carried catalyst and preparation method thereof | |
| CN109603820A (en) | The monatomic method for preparing catalyst of room temperature degradation of formaldehyde under a kind of Oxygen Condition | |
| CN107159202B (en) | Manganese-doped palladium supported catalyst and preparation method and application thereof | |
| CN105080529B (en) | Normal-temperature efficient removes VOCs catalysis materials | |
| CN102838168A (en) | Mesoporous manganese oxide nanometer material capable of removing ozone and formaldehyde in air at room temperature simultaneously | |
| CN103043773B (en) | A kind of Catalytic Wet Oxidation method of flue gas desulphurization waste solution | |
| Chen et al. | Defect engineering and synergistic effect in Co3O4 catalysts for efficient removal of formaldehyde at room temperature | |
| CN108067263B (en) | Catalyst with shell-core structure and preparation method and application thereof | |
| Li et al. | A review of Co 3 O 4-based catalysts for formaldehyde oxidation at low temperature: Effect parameters and reaction mechanism | |
| CN110813312A (en) | Magnetic nano composite material and preparation method and application thereof | |
| CN108067265B (en) | Preparation method of methane conversion catalyst | |
| Zhang et al. | NiCo-LDH@ MnO2 nanocages as advanced catalysts for efficient formaldehyde elimination | |
| CN101143335B (en) | Plasma reactor catalyst and its preparation method and use | |
| Li et al. | Well-dispersed CuFe doping nanoparticles with mixed valence in carbon aerogel as effective adsorbent for H2S removal at low temperature | |
| JPH11514291A (en) | Honeycomb catalyst carrier | |
| KR101436992B1 (en) | Chemicals and Devices to remove Ammonia and Hydrogen Peroxide Gas | |
| Ali et al. | Effect of Au precursor and support on the catalytic activity of the nano-Au-catalysts for propane complete oxidation | |
| CN108067286B (en) | Methane halogen oxidation catalyst and preparation method and application thereof | |
| CN108067262A (en) | A kind of preparation method of highly selective methane zirconyl oxyhalides catalyst |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200221 |
|
| RJ01 | Rejection of invention patent application after publication |