CN106082353B - A kind of preparation method of ferric oxide nano piece - Google Patents
A kind of preparation method of ferric oxide nano piece Download PDFInfo
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- CN106082353B CN106082353B CN201610408147.3A CN201610408147A CN106082353B CN 106082353 B CN106082353 B CN 106082353B CN 201610408147 A CN201610408147 A CN 201610408147A CN 106082353 B CN106082353 B CN 106082353B
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 238000001556 precipitation Methods 0.000 claims abstract description 27
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000000926 separation method Methods 0.000 claims abstract description 13
- 239000007787 solid Substances 0.000 claims abstract description 12
- 230000008569 process Effects 0.000 claims abstract description 7
- 229910021577 Iron(II) chloride Inorganic materials 0.000 claims abstract description 6
- 239000008156 Ringer's lactate solution Substances 0.000 claims abstract description 6
- 238000002242 deionisation method Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 238000010792 warming Methods 0.000 claims abstract description 6
- JVTAAEKCZFNVCJ-UHFFFAOYSA-M Lactate Chemical compound CC(O)C([O-])=O JVTAAEKCZFNVCJ-UHFFFAOYSA-M 0.000 claims abstract description 5
- 229940001447 lactate Drugs 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims 1
- 239000003344 environmental pollutant Substances 0.000 abstract 1
- 231100000719 pollutant Toxicity 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 description 7
- 239000011229 interlayer Substances 0.000 description 6
- 238000011282 treatment Methods 0.000 description 6
- 150000001450 anions Chemical class 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 239000005416 organic matter Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 239000012855 volatile organic compound Substances 0.000 description 5
- 239000002351 wastewater Substances 0.000 description 5
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229960001545 hydrotalcite Drugs 0.000 description 3
- 229910001701 hydrotalcite Inorganic materials 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229960000907 methylthioninium chloride Drugs 0.000 description 3
- -1 stirs 20min Substances 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- NGSFWBMYFKHRBD-DKWTVANSSA-M sodium;(2s)-2-hydroxypropanoate Chemical compound [Na+].C[C@H](O)C([O-])=O NGSFWBMYFKHRBD-DKWTVANSSA-M 0.000 description 2
- IHICGCFKGWYHSF-UHFFFAOYSA-N C1=CC=CC=C1.CC1=CC=CC=C1.CC1=CC=CC=C1C Chemical compound C1=CC=CC=C1.CC1=CC=CC=C1.CC1=CC=CC=C1C IHICGCFKGWYHSF-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001449 anionic compounds Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000007084 catalytic combustion reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003933 environmental pollution control Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 229910001412 inorganic anion Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical group [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 150000002891 organic anions Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000003380 propellant Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 239000004449 solid propellant Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Manufacturing & Machinery (AREA)
- Compounds Of Iron (AREA)
- Catalysts (AREA)
Abstract
The present invention discloses a kind of preparation method of ferric oxide nano piece.In turn include the following steps：Take 500mL FeCl2Solution, it is placed in 70~80 DEG C of water-baths of constant temperature, 30% 2~4mL of (mass fraction) hydrogen peroxide and a certain amount of NaOH weak solutions is added dropwise simultaneously into solution, it is 12~13 to keep pH value, react 2~3h, it is transferred in autoclave, 150~180 DEG C is warming up in 1h, continues to react 4~8h, naturally cool to room temperature, the precipitation with layer structure is formed in this process, and precipitation separation, deionization is washed 2~3 times；The solid that precipitation is obtained is added in the sodium lactate solution that concentration is 2~4mol/L, and solid-to-liquid ratio is 1：10~1：50,4~5h is stirred, precipitation separation, the solid of acquisition is being washed with deionized after 2~3 times, calcined at a temperature of 400~450 DEG C, removes lactate therein, you can obtain a kind of ferric oxide nano piece.The structure is conducive to adsorbing and being catalyzed pollutant.
Description
Technical field
The present invention relates to the exploitation of novel environmental pollution control material, more particularly to a kind of preparation side of ferric oxide nano piece
Method.
Background technology
VOCs treatment refers to the place that the organic exhaust gas produced in industrial processes is adsorbed, filtered, purified
Science and engineering is made.Usual VOCs treatment has benzene homologues VOCs treatments such as formaldehyde VOCs treatment, benzene toluene dimethylbenzene etc.
Deng.Organic exhaust gas be usually present it is inflammable and explosive, poisonous and harmful, water insoluble, be dissolved in the big spy of organic solvent, intractability
Point.Organic exhaust gas active-carbon adsorption treatment method, Production by Catalytic Combustion Process, catalysis oxidation are generally used in VOCs treatment
A variety of principles such as method, acid-base neutralization method, plasma method.Catalysis oxidation is a kind of both economical effective method.But need through
Ji is adapted to blanket catalyst.
Nano-sized iron oxide has huge specific surface area, and skin effect is a kind of good catalyst significantly.Use nanoparticle
Activity, the selectivity for the catalyst that son is made all are higher than typical catalyst, and long lifespan is easy to operate.It will be made of nano-sized iron oxide
Into hollow beads, float on the wastewater surface containing organic matter.The degraded for carrying out organic matter using sunshine can accelerate at waste water
Reason process.It is exactly this method used that the U.S., Japan etc., which are revealed when the pollution caused is handled offshore oil,.Nano oxygen
Change the catalyst that iron has been directly used as high molecular polymer oxidation, reduction and synthesis, nano iron oxide catalyst can make oil
Rate of cleavage improves 1~5 times, and the burning velocity for the solid propellant being made using it as combustion catalyst can compared with conventional propellant
1~10 times is improved, this is highly beneficial to manufacture high-performance rocket and guided missile.Water can also be catalytically decomposed in nano-sized iron oxide, be made
Clean energy resource.
Hydrotalcite-based compound (LDHs) is the compound by interlayer anion and the accumulation of positively charged laminate.Neatly
Stone chemical structure of general formula is：[M2+ 1-xM3+x(OH)2]x+[(An-)x/n·mH2O], wherein M2+And M3+Respectively it is located at main layer board
On divalence and trivalent metal cation, such as Mg2+、Ni2+、Zn2+、Mn2+、Cu2+、Co2+、Pd2+、Fe2+Deng bivalent cation and Al3 +、Cr3+、Co3+、Fe3+Hydrotalcite can be formed Deng Tricationic；An–For interlayer anion, inorganic anion can be included,
Organic anion, complex anion, same many and heteropolyanion；X is M3+/(M2++M3+) molar ratio, about 4:1 arrives
2:1；M is the number of interlayer hydrone.Its structure is similar to shepardite Mg (OH)2, main body is formed by the shared seamed edge of octahedron
Laminate.Divalent metal M on laminate2+Can be golden by the close trivalent of ion half price in certain proportion
Belong to cation M3+Same order elements so that laminate is positively charged, the positive electricity on anion and laminate that interlayer presence can be exchanged
Lotus balances so that LDHs overall structure is in electroneutral.The anion of interlayer can be exchanged, by a series of modifications, hydrotalcite
Material can obtain the material of many kinds of different properties.
The content of the invention
The purpose of the present invention be for overcome the shortcomings of in the prior art iron oxide structure single there is provided a kind of ferric oxide nano
The preparation method of piece.
The technical solution adopted by the present invention is in turn include the following steps：
1) by FeCl2It is dissolved into water, is configured to the solution that concentration is 2~3mol/L, takes the 500mL solution, Xiang Qi
In 30% 2~4mL of (mass fraction) hydrogen peroxide and a certain amount of NaOH weak solutions are added dropwise simultaneously, it is 12~13 to keep pH value, instead
2~3h is answered, is transferred in autoclave, 150~180 DEG C are warming up in 1h, continues to react 4~8h, room temperature is naturally cooled to, at this
During formed with layer structure precipitation, precipitation separation, deionization wash 2~3 times；
2) solid for obtaining precipitation is added in the sodium lactate solution that concentration is 2~4mol/L, and solid-to-liquid ratio is 1：10~
1：50,4~5h is stirred, precipitation is separated, and the solid of acquisition is being washed with deionized after 2~3 times, in 400~450 DEG C of temperature
Degree is lower to be calcined, and removes lactate therein, you can obtain a kind of ferric oxide nano piece.
It is an advantage of the invention that：The ferric iron that part ferrous ion is generated by hydrogen peroxide oxidation, divalent ion and generation
Trivalent ion in the presence of alkali, produce co-precipitation, form lamella hydrotalcite structure, then enter lactate in piece Inter layer exchange,
Lactate is removed finally by high-temperature calcination, the relative lamellar structure scattered is formed.The structure is conducive to adsorbing and is catalyzed dirt
Contaminate thing.
Embodiment
3 embodiments of the present invention are provided further below：
Embodiment 1
By FeCl2It is dissolved into water, is configured to the solution that concentration is 2mol/L, the solution is placed in 80 DEG C of constant temperature by 500mL
In water-bath, while 30% (mass fraction) hydrogen peroxide 4mL and a certain amount of NaOH weak solutions is added dropwise, it is 13 to keep pH value, reaction
3h, is transferred in autoclave, and 180 DEG C are warming up in 1h, is continued to react 8h, is naturally cooled to room temperature, forms tool in this process
There is the precipitation of layer structure, precipitation separation, deionization is washed 3 times；It is 4mol/L's that the solid that precipitation is obtained, which is added to concentration,
In sodium lactate solution, solid-to-liquid ratio is 1：10,5h is stirred, precipitation separation, the solid of acquisition is being washed with deionized after 3 times,
Calcined at a temperature of 450 DEG C, that is, obtain a kind of ferric oxide nano piece.
1g ferric oxide nano pieces are taken, is added in the pending methylene blue waste water of 1.0L, adds 0.01 milliliter of quality
Fraction is 30% hydrogen peroxide, stirs 20min, and organic matter is decomposed, and precipitation separation, clearance 97.2%, supernatant can be arranged
Put.
Embodiment 2
By FeCl2It is dissolved into water, is configured to the solution that concentration is 3mol/L, the solution is placed in 70 DEG C of constant temperature by 500mL
In water-bath, while 30% (mass fraction) hydrogen peroxide 2mL and a certain amount of NaOH weak solutions is added dropwise, it is 12 to keep pH value, reaction
2h, is transferred in autoclave, and 150 DEG C are warming up in 1h, is continued to react 4h, is naturally cooled to room temperature, forms tool in this process
There is the precipitation of layer structure, precipitation separation, deionization is washed 2 times；2) solid for obtaining precipitation is added to concentration for 2mol/L
Sodium lactate solution in, solid-to-liquid ratio is 1：10, stir 4h, precipitation separation, the solid of acquisition be washed with deionized 2 times it
Afterwards, calcined at a temperature of 400 DEG C, that is, obtain a kind of ferric oxide nano piece.
1g ferric oxide nano pieces are taken, is added in the pending methylene blue waste water of 1.0L, adds 0.01 milliliter of quality
Fraction is 30% hydrogen peroxide, stirs 20min, and organic matter is decomposed, and precipitation separation, clearance 96.9%, supernatant can be arranged
Put.
Embodiment 3
By FeCl2It is dissolved into water, is configured to the solution that concentration is 2.5mol/L, the solution is placed in constant temperature 80 by 500mL
In DEG C water-bath, while 30% (mass fraction) hydrogen peroxide 3mL and a certain amount of NaOH weak solutions is added dropwise, it is 13 to keep pH value, instead
3h is answered, is transferred in autoclave, 180 DEG C are warming up in 1h, continues to react 8h, naturally cools to room temperature, formed in this process
Precipitation with layer structure, precipitation separation, deionization is washed 3 times；The solid that precipitation is obtained is added to concentration for 4mol/L
Sodium lactate solution in, solid-to-liquid ratio is 1：20, stir 5h, precipitation separation, the solid of acquisition be washed with deionized 3 times it
Afterwards, calcined at a temperature of 450 DEG C, that is, obtain a kind of ferric oxide nano piece.
1g ferric oxide nano pieces are taken, is added in the pending methylene blue waste water of 1.0L, adds 0.01 milliliter of quality
Fraction is 30% hydrogen peroxide, stirs 20min, and organic matter is decomposed, and precipitation separation, clearance 96.5%, supernatant can be arranged
Put.
Claims (1)
1. a kind of preparation method of ferric oxide nano piece, it is characterized in that in turn including the following steps：
1) by FeCl2It is dissolved into water, is configured to the solution that concentration is 2~3mol/L, takes the 500mL solution, drip simultaneously thereto
Plus hydrogen peroxide 2~4mL and a certain amount of NaOH weak solution of the mass fraction for 30%, it is 12~13 to keep pH value, reaction 2~
3h, is transferred in autoclave, and 150~180 DEG C are warming up in 1h, is continued to react 4~8h, room temperature is naturally cooled to, in the process
Middle to form the precipitation with layer structure, precipitation separation, deionization is washed 2~3 times；
2) solid for obtaining precipitation is added in the sodium lactate solution that concentration is 2~4mol/L, and solid-to-liquid ratio is 1：10~1：50,
4~5h is stirred, precipitation is separated, and the solid of acquisition is being washed with deionized after 2~3 times, at a temperature of 400~450 DEG C
Calcining, removes lactate therein, you can obtain a kind of ferric oxide nano piece.
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| CN106992295B (en) * | 2017-03-02 | 2019-09-10 | 浙江大学 | A kind of preparation method of monodisperse alpha-ferric oxide nanometer sheet |
| CN108186677B (en) * | 2018-01-05 | 2020-05-19 | 中国科学院上海硅酸盐研究所 | Degradable nano material capable of efficiently generating free radicals and preparation method and application thereof |
| CN107935055B (en) * | 2018-01-10 | 2020-01-31 | 合肥学院 | layered α -Fe with visible light absorption enhancement2O3Preparation method of nano round cake |
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| CN101062790A (en) * | 2007-04-20 | 2007-10-31 | 南京大学 | Simple preparation method of alpha-FeOOH and alpha-Fe2O3 nano stick |
| CN101591059A (en) * | 2009-07-10 | 2009-12-02 | 江南大学 | A kind of with the ozonization wastewater treatment method of alpha-FeOOH nano material as catalyzer |
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