CN108910900A - A method of iron oxide and silica nano material are prepared simultaneously from iron tailings - Google Patents
A method of iron oxide and silica nano material are prepared simultaneously from iron tailings Download PDFInfo
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- CN108910900A CN108910900A CN201810791602.1A CN201810791602A CN108910900A CN 108910900 A CN108910900 A CN 108910900A CN 201810791602 A CN201810791602 A CN 201810791602A CN 108910900 A CN108910900 A CN 108910900A
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 174
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 145
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 87
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 72
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000000843 powder Substances 0.000 claims abstract description 27
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 26
- 239000010703 silicon Substances 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 239000003513 alkali Substances 0.000 claims abstract description 19
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002245 particle Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 66
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 46
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 25
- 230000004913 activation Effects 0.000 claims description 18
- 238000002604 ultrasonography Methods 0.000 claims description 17
- 230000004927 fusion Effects 0.000 claims description 16
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 16
- 239000000706 filtrate Substances 0.000 claims description 14
- 230000001376 precipitating effect Effects 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- 239000000908 ammonium hydroxide Substances 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 4
- 239000011858 nanopowder Substances 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 229910052681 coesite Inorganic materials 0.000 claims description 3
- 229910052593 corundum Inorganic materials 0.000 claims description 3
- 229910052906 cristobalite Inorganic materials 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 229910052682 stishovite Inorganic materials 0.000 claims description 3
- 229910052905 tridymite Inorganic materials 0.000 claims description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 24
- 238000002360 preparation method Methods 0.000 abstract description 8
- 239000002910 solid waste Substances 0.000 abstract description 5
- 238000005554 pickling Methods 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 abstract description 2
- 238000012805 post-processing Methods 0.000 abstract 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 11
- 239000000463 material Substances 0.000 description 8
- 239000007787 solid Substances 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 241000209094 Oryza Species 0.000 description 4
- 235000007164 Oryza sativa Nutrition 0.000 description 4
- 239000003086 colorant Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 235000009566 rice Nutrition 0.000 description 4
- 239000013049 sediment Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- 241000186216 Corynebacterium Species 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 229940067573 brown iron oxide Drugs 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 235000019795 sodium metasilicate Nutrition 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 235000021419 vinegar Nutrition 0.000 description 1
- 239000000052 vinegar Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
-
- 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
-
- 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]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/11—Powder tap density
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Nanotechnology (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Composite Materials (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Compounds Of Iron (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a kind of methods for preparing iron oxide and silica nano material simultaneously from iron tailings.It includes the following steps：（1）Mine tailing heat treatment；（2）Pickling mentions iron；（3）Alkali soluble mentions silicon；（4）Prepare silica nano material；（5）Prepare ferric oxide powder；（6）Product post-processing.Silica nano material prepared by the present invention has uniform lesser partial size, particle diameter distribution, higher purity and lesser density after tested；The ferric oxide powder of preparation has the characteristics that lesser particle, color are uniform and widely used, and the invention comprehensively utilizes the element in iron tailings, the ferric oxide powder and silica nano material of preparation have a very wide range of applications space.The present invention is low in cost using iron tailings as raw material, and can largely handle the solid waste, and preparation flow is simple, and reaction requires low, is easy to industrialize.
Description
Technical field
The invention belongs to technical field of inorganic material, and in particular to one kind prepares iron oxide from iron tailings and silica is received
The method of rice material.
Background technique
Iron tailings is a kind of solid waste, is that Mining Development especially metallic ore exploitation causes the important next of environmental pollution
Source.Processing tailing not only needs to occupy a large amount of soils, very big injury is caused to the ecological environment of surrounding, and to put into various
Processing and maintenance cost.In China, iron tailings ratio shared in industrial solid castoff is higher and higher, and due to iron tailings
Structural behaviour is complicated, and type is more, keeps it very low in the utilization rate in China, currently, the comprehensive utilization ratio of China's iron tailings is only
It is 7%, far below the utilization rate of developed country 60%.Synthetical recovery and the utilization for carrying out resource of tailings, can not only make full use of
Mineral resources expand mineral resource utilization range；It is also the important means of pollution administration, protecting ecology；It can also save a large amount of
Soil and fund.According to incompletely statistics, the iron tailings of the accumulative stockpiling in China at present has been up to 5 × 109T or so, and
With the continuous improvement of iron ore production capacity, iron tailings volume of cargo in storage is just with 5 × 108The rate of t/a increases.
Ferric oxide powder is a kind of important raw material of industry, for painting, the coloring of rubber, plastics, building etc., is
Inorganic pigment is used as rust resisting pigment in coatings industry.It is also precision instrument, the polishing agent of optical glass and manufacture magnetic material
The raw material etc. of ferrite component.
Nano silica is a kind of inorganic chemical industry material, due to being ultrafine nanometer, size range in 1 ~ 100nm, because
This such as has to anti-ultraviolet optical property with many unique properties, can improve anti-aging other materials, intensity and resistance to
Chemical property etc., purposes is very extensive.The preparation of nano silica mainly divides physical method and chemical method at present, wherein changing
Method includes chemical vapor deposition (CVD) method, liquid phase method, ion-exchange, the precipitation method and collosol and gel (Sol-Gel) method again
Deng main production method is still using silicon tetrachloride as the vapor phase method of raw material, using sodium metasilicate and inorganic acid as the precipitation method of raw material
With the sol-gal process with silicic acid vinegar etc. for raw material.These methods are there is energy consumption height, and the problems such as silicon source is at high cost keeps it cheap
Production is faced with many problems.
Background in view of the above technology does not have also and prepares ferric oxide powder and silica nano material by raw material of iron tailings
Play-by-play, the present invention prepares ferric oxide powder and cheap silicon source while largely processing this waste of iron tailings,
And can be reacted to obtain the silica nano material that partial size is small, content is high under normal pressure, there is very big realistic meaning.
Summary of the invention
In view of the deficiencies of the prior art, iron oxide is prepared simultaneously from iron tailings the present invention provides one kind and silica is received
The method of rice material, the method that it prepares oxide-based nanomaterial simultaneously as raw material using iron tailings have low in cost, raw material
From a wealth of sources, daily low energy consumption, reaction condition is mild, is easy to industrialize and largely handle the advantage of solid waste；And it makes
The silica nano material obtained has biggish specific surface area, lesser partial size and higher content.
A kind of method preparing iron oxide and silica nano material simultaneously from iron tailings, it is characterised in that packet
Include following steps：
1）Iron tailings is ground and is sieved with 100 mesh sieve, obtain it is levigate after iron tailings；
2）By step 1）It is levigate after iron tailings be put into Muffle furnace and be heated to 850-950 DEG C and activated, keep the temperature 4.5-5.5
Hour, the iron tailings powder after activation is made；
3）By step 2）In activation after iron tailings powder and mixed in hydrochloric acid and be stirred to react, filter after reaction, filter residue into
Row drying, filtrate container collection；
4）By step 3）In filter residue and sodium hydrate particle be mixed and stirred for uniformly, being put into Muffle furnace 450-550 DEG C and keeping
1.5-2.5 hours, the iron tailings after alkali fusion reaction is made；
5）By step 4）Iron tailings after middle alkali fusion reaction incorporates in water, and heating stirring reaction is obtained by filtration thick after reaction
Silicon solution；
6）By step 5）In thick silicon solution obtained under ultrasound environments with salt acid for adjusting pH to 6.5-7.5, there are a large amount of precipitatings,
It is filtered after standing, residue collection；
7）To step 6）In filter residue be added hydrochloric acid stirring after filter and dry again, be made silica nano material；
8）By step 3）In filtrate adjust pH to 6.5-7.5 with ammonium hydroxide under ultrasound environments, there is a large amount of precipitatings, mistake after standing
It filters, uses container collection after filter residue and drying；
9）By step 8）Filter residue after middle drying is put into Muffle furnace, roasting temperature 2 hours of 600 DEG C -700 DEG C, finally
Ferric oxide nano powder is made.
The method that the slave iron tailings prepares iron oxide and silica nano material simultaneously, it is characterised in that step 1）
In iron tailings component mass fraction be SiO2 45.43%、CaO 13.81%、MgO 13.10%、Al2O3 11.35%、Fe2O3
10.13%, surplus is impurity.
The method that the slave iron tailings prepares iron oxide and silica nano material simultaneously, it is characterised in that step 3）
In concentration of hydrochloric acid be 1-3mol/L, preferably 2mol/L, activation mine tailing and mass ratio be 1:1.6-2.
The method that the slave iron tailings prepares iron oxide and silica nano material simultaneously, it is characterised in that step 4）
In filter residue and sodium hydroxide mass ratio be 1:1.4-2.
The method that the slave iron tailings prepares iron oxide and silica nano material simultaneously, it is characterised in that step 5）
In alkali soluble reaction after iron tailings press 1:The solid-to-liquid ratio of 4-6 is added to the water, and is stirred to react at a temperature of 60 DEG C -85 DEG C, passes through
Filter obtains thick silicon solution.
The method that the slave iron tailings prepares iron oxide and silica nano material simultaneously, it is characterised in that step 7）
Middle concentration of hydrochloric acid is 1-3mol/L, preferably 2mol/L, and the volume ratio of filter residue and hydrochloric acid is 1:1.5-2.
The method that the slave iron tailings prepares iron oxide and silica nano material simultaneously, it is characterised in that step 8）
Middle ammonia concn is 1-2mol/L.
The method that the slave iron tailings prepares iron oxide and silica nano material simultaneously, it is characterised in that obtain
The content of silica nano material is 99%, and partial size is less than 100nm, tap density 0.344-0.372g/cm3；Brown iron oxide
The tap density of body is 1.068-1.132 g/cm3, partial size is less than 50nm.
By using above-mentioned technology, compared with prior art, the present invention is had the advantages that：
1）The present invention has carried out a series of comprehensive utilization using this solid waste of iron tailings as raw material, to it, both alleviates
Environmental pressure, and develop a kind of cheap silicon source and prepare silica nano material, and rationally recycled ferro element therein with
Reach the comprehensive utilization of next step；
2）The present invention is made after thick silicon solution the adjusting pH under ultrasound environments and is allowed to precipitate, and greatly reduces silica dioxide granule
Partial size, while its specific surface area is increased, so that silica nano material obtained is had higher quality, appearance is white powder
End, partial size 20-100nm, dioxide-containing silica are greater than 99%, there is preferable dispersibility and chemical stability；
3）The present invention is made after thick silica and removes wherein a small amount of metal ion with acid, further improves final silica
The purity of nano material；
4）Silica nano material produced by the present invention after tested, shows that dioxide-containing silica is 99%, and partial size is less than 100nm,
Tap density is 0.368g/cm3。
Detailed description of the invention
Fig. 1 is implementation flow chart of the present invention；
Fig. 2 is SiO made from present example 12The SEM of nano material schemes；
Fig. 3 is SiO made from present example 12The Fourier of nano material is infrared（FTIR）Analysis chart；
Fig. 4 is the SEM figure of ferric oxide powder made from present example 1.
Specific embodiment
With specific embodiment, technical scheme is described further below, but protection scope of the present invention is unlimited
In this：
Embodiment 1 prepares oxide-based nanomaterial
As shown in Figure 1, the embodiment of the present invention 1 prepares oxide-based nanomaterial by raw material of iron tailings, include the following steps：
（1）Raw material includes at least North China's iron tailings（SiO245.43%、CaO 13.81%、MgO 13.10%、Al2O3
11.35%、Fe2O310.13%, surplus is impurity, and the iron tailings content in following instance is same as Example 1）, sodium hydroxide,
Hydrochloric acid, concentrated ammonia liquor；
（2）Iron tailings after will be levigate is heated to 850 DEG C in high temperature furnace, is kept for temperature 4.5 hours, the tailing after activation is made
Powder；
（3）By the mine tailing and 2mol/L hydrochloric acid by volume 1 after activation:1.6 are mixed and stirred for reacting for 2 hours, filtering
It obtains filter residue to be dried, filtrate container collection；
（4）By filter residue and solid sodium hydroxide particle in mass ratio 1:1.4 are mixed and stirred for uniformly, 450 DEG C of guarantors in Muffle furnace
Iron tailings after holding obtained alkali fusion reaction in 1.5 hours；
（5）Iron tailings after alkali fusion is reacted is soluble in water, is 1 by solid-to-liquid ratio:4 are stirred to react 24 hours at 60 DEG C, pass through
Filter obtains thick silicon solution；
（6）Thick silicon solution obtained is adjusted to pH=6.5 or so with hydrochloric acid under ultrasound environments, a large amount of precipitatings occurs, stands 1
It is filtered after hour, filter residue container collection；
（7）It is by volume 1 into filter residue:1.5 be added 2mol/L hydrochloric acid stir 2 hours, wash again later three times, filtering simultaneously
It is dry, silica nano material is made, appearance is white powder, partial size 60nm, dioxide-containing silica 99.3%；
（8）By step（3）In filtrate be adjusted to pH=6.5 with 2mol/L ammonium hydroxide under ultrasound environments, it is heavy to there are a large amount of brown colors
It forms sediment, is filtered after standing 1 hour, use container collection after residue washing is dry；
（9）Filter residue after drying is put into Muffle furnace, roasting temperature 2 hours of 600 DEG C, ferric oxide nano is finally made
Powder.And measured performance parameter is entered to resulting iron oxide and silica nano material, it is specific as follows：
1）The scanning electron microscope of silica nano material prepared by embodiment 1（SEM）Analysis
Fig. 2 is the morphology of silica nano material.It can be seen from the figure that the silica nano material of preparation
For graininess, particle diameter distribution is uniform, about 80nm, belongs to nano material scope.
2）The Fourier of silica nano material prepared by embodiment 1 is infrared（FTIR）Analysis
Fig. 3 is that the Fourier of silica nano material is infrared（FTIR）Analysis chart.It can be seen from the figure that in wave number
1085cm-1Locating strong and wide peak is Si-O-Si vibration peak；In 3446 cm of wave number-1The flexible vibration of the antisymmetry that the broad peak at place is-OH
Dynamic peak, it was demonstrated that resulting materials are hydrated SiO 2 nano material.
3）The scanning electron microscope of ferric oxide powder prepared by embodiment 1（SEM）Analysis
Fig. 4 is the microscopic appearance of ferric oxide powder.It can be seen from the figure that the ferric oxide powder of preparation is corynebacterium, partial size point
Cloth is uniform, is less than 50nm, belongs to nano material scope.
Embodiment 2 prepares oxide-based nanomaterial
The embodiment of the present invention 2 prepares oxide-based nanomaterial by raw material of iron tailings, includes the following steps：
（1）Raw material includes at least North China's iron tailings, sodium hydroxide, hydrochloric acid, concentrated ammonia liquor.
（2）Iron tailings after will be levigate is heated to 950 DEG C in high temperature furnace, is kept for temperature 5.5 hours, after activation is made
Mine tailing；
（3）By the mine tailing and 2mol/L hydrochloric acid by volume 1 after activation:2 are mixed and stirred for reacting for 2 hours, filter to take
It obtains filter residue to be dried, filtrate container collection；
（4）By filter residue and solid sodium hydroxide in mass ratio 1:2 are mixed and stirred for uniformly, and 550 DEG C of holdings 2.5 are small in Muffle furnace
When be made alkali fusion reaction after iron tailings；
（5）Iron tailings after alkali fusion is reacted is soluble in water, is 1 by solid-to-liquid ratio:6 are stirred to react 24 hours at 85 DEG C, pass through
Filter obtains thick silicon solution；
（6）Thick silicon solution obtained is adjusted to pH=7.5 or so with hydrochloric acid under ultrasound environments, a large amount of precipitatings occurs, stands 1
It is filtered after hour, filter residue container collection；
（7）It is by volume 1 into filter residue:2 be added 2mol/L hydrochloric acid stir 4 hours, wash again later three times, filter and do
It is dry, silica nano material is made, appearance is white powder, partial size 30nm, dioxide-containing silica 99.5%；
（8）By step（3）In filtrate be adjusted to pH=7.5 with 2mol/L ammonium hydroxide under ultrasound environments, it is heavy to there are a large amount of brown colors
It forms sediment, is filtered after standing 1 hour, use container collection after residue washing is dry；
（9）Filter residue after drying is put into Muffle furnace, roasting temperature 2 hours of 700 DEG C, ferric oxide nano is finally made
Powder.And measured performance parameter is entered to resulting iron oxide and silica nano material, iron oxide and silica are received
Rice material property parameter measurement is the same as embodiment 1.
Embodiment 3 prepares oxide-based nanomaterial
The embodiment of the present invention 3 prepares oxide-based nanomaterial by raw material of iron tailings, includes the following steps：
（1）Raw material includes at least North China's iron tailings, sodium hydroxide, hydrochloric acid, concentrated ammonia liquor；
（2）Iron tailings after will be levigate is heated to 900 DEG C in high temperature furnace, is kept for temperature 5 hours, the tailing after activation is made
Powder；
（3）By the mine tailing and 2mol/L hydrochloric acid by volume 1 after activation:1.8 are mixed and stirred for reacting for 2 hours, filtering
It obtains filter residue to be dried, filtrate container collection；
（4）By filter residue and solid sodium hydroxide in mass ratio 1:1.6 are mixed and stirred for uniformly, keep 2.5 for 500 DEG C in Muffle furnace
Iron tailings after hour obtained alkali fusion reaction；
（5）Iron tailings after alkali fusion is reacted is soluble in water, is 1 by solid-to-liquid ratio:5 are stirred to react 24 hours at 80 DEG C, pass through
Filter obtains thick silicon solution；
（6）Thick silicon solution obtained is adjusted to pH=7 or so with hydrochloric acid under ultrasound environments, a large amount of precipitatings occurs, it is small to stand 1
When after filter, filter residue container collection；
（7）It is by volume 1 into filter residue:1.8 be added 2mol/L hydrochloric acid stir 4 hours, wash again later three times, filtering simultaneously
It is dry, silica nano material is made, appearance is white powder, partial size 9nm, dioxide-containing silica 99.1%；
（8）By step（3）In filtrate be adjusted to pH=7 with 2mol/L ammonium hydroxide under ultrasound environments, it is heavy to there are a large amount of brown colors
It forms sediment, is filtered after standing 1 hour, use container collection after residue washing is dry；
（9）Filter residue after drying is put into Muffle furnace, roasting temperature 2 hours of 650 DEG C, ferric oxide nano is finally made
Powder.And measured performance parameter is entered to resulting iron oxide and silica nano material, iron oxide and silica are received
Rice material property parameter measurement is the same as embodiment 1.
Embodiment 3 prepares oxide-based nanomaterial
The embodiment of the present invention 3 prepares oxide-based nanomaterial by raw material of iron tailings, includes the following steps：
（1）Raw material includes at least North China's iron tailings, sodium hydroxide, hydrochloric acid, concentrated ammonia liquor；
（2）Iron tailings after will be levigate is heated to 920 DEG C in high temperature furnace, is kept for temperature 5 hours, the tailing after activation is made
Powder；
（3）By the mine tailing and 2mol/L hydrochloric acid by volume 1 after activation:1.6 are mixed and stirred for reacting for 2 hours, filtering
It obtains filter residue to be dried, filtrate container collection；
（4）By filter residue and solid sodium hydroxide in mass ratio 1:1.7 are mixed and stirred for uniformly, and 520 DEG C of holdings 2 are small in Muffle furnace
When be made alkali fusion reaction after iron tailings.
（5）Iron tailings after alkali fusion is reacted is soluble in water, is 1 by solid-to-liquid ratio:5 are stirred to react 24 hours at 85 DEG C,
Thick silicon solution is obtained by filtration.
（6）Thick silicon solution obtained is adjusted to pH=7 or so with hydrochloric acid under ultrasound environments, a large amount of precipitatings occurs, stands
It is filtered after 1 hour, filter residue container collection.
（7）It is by volume 1 into filter residue:1.6 be added 2mol/L hydrochloric acid stir 4 hours, wash again later three times, mistake
It filters and dries, silica nano material is made, appearance is white powder, partial size 40nm, dioxide-containing silica 99.6%
（8）By step（3）In filtrate be adjusted to pH=7.5 with 2mol/L ammonium hydroxide under ultrasound environments, it is heavy to there are a large amount of brown colors
It forms sediment, is filtered after standing 1 hour, use container collection after residue washing is dry.
（9）Filter residue after drying is put into Muffle furnace, roasting temperature 2 hours of 680 DEG C, iron oxide is finally made
Nano-powder.And measured performance parameter, iron oxide and titanium dioxide are entered to resulting iron oxide and silica nano material
Silicon nano material measured performance parameter is the same as embodiment 1.
Comparative example 1 prepares oxide-based nanomaterial
Comparative example 1 of the present invention prepares oxide-based nanomaterial by raw material of iron tailings, includes the following steps：
（1）Raw material includes at least North China's iron tailings, sodium hydroxide, hydrochloric acid, concentrated ammonia liquor；
（2）Iron tailings after will be levigate is heated to 900 DEG C in high temperature furnace, is kept for temperature 5 hours, the tailing after activation is made
Powder；
（3）By the mine tailing and 2mol/L hydrochloric acid by volume 1 after activation:1.6 are mixed and stirred for reacting for 2 hours, filtering
It obtains filter residue to be dried, filtrate container collection；
（4）By filter residue and solid sodium hydroxide in mass ratio 1:1.4 are mixed and stirred for uniformly, and 500 DEG C of holdings 2 are small in Muffle furnace
When be made alkali fusion reaction after iron tailings；
（5）Iron tailings after alkali fusion is reacted is soluble in water, is 1 by solid-to-liquid ratio:4 are stirred to react 24 hours at 60 DEG C, pass through
Filter obtains thick silicon solution；
（6）Thick silicon solution obtained is adjusted to pH=7 or so with hydrochloric acid, a large amount of precipitatings occurs, is filtered after standing 1 hour, filter residue
Use container collection；
（7）It is by volume 1 into filter residue:1 be added 2mol/L hydrochloric acid stir 2 hours, wash again later three times, filter and do
It is dry, silica nano material is made.
Comparative example 2 prepares oxide-based nanomaterial
Comparative example 2 of the present invention prepares oxide-based nanomaterial by raw material of iron tailings, includes the following steps：
（1）Raw material includes at least North China's iron tailings, sodium hydroxide, hydrochloric acid, concentrated ammonia liquor；（2）Iron tailings after will be levigate exists
It is heated to 900 DEG C in high temperature furnace, is kept for temperature 5 hours, the mine tailing after activation is made；
（3）By the mine tailing and 2mol/L hydrochloric acid by volume 1 after activation:2 are mixed and stirred for reacting for 2 hours, filter to take
It obtains filter residue to be dried, filtrate container collection；
（4）By filter residue and solid sodium hydroxide in mass ratio 1:2 are mixed and stirred for uniformly, are kept for 2 hours for 500 DEG C in Muffle furnace
Iron tailings after alkali fusion reaction is made；
（5）Iron tailings after alkali fusion is reacted is soluble in water, is 1 by solid-to-liquid ratio:6 are stirred to react 24 hours at 85 DEG C, pass through
Filter obtains thick silicon solution；
（6）Thick silicon solution obtained is adjusted to pH=6 or so with hydrochloric acid under ultrasound environments, a large amount of precipitatings occurs, it is small to stand 1
When after filter, residue washing three times, filter and dry, silica nano material is made.
Table 1 is the performance parameter summary sheet of present example products obtained therefrom
By two above comparative example, comparative example 1 is in step 6）In thick silicon solution when adjusting pH not under ultrasound environments into
Row, compared with original method, in scanning electron microscope（SEM）Down it can be seen that silica dioxide granule obtained is reunited in comparative example 1,
Partial size greatly increases, it was demonstrated that adjusts the precipitating that pH is generated under ultrasound environments, has smaller partial size and bigger specific surface area.
Comparative example 2 is in step（6）In not to thick silica carry out pickling operation, it is glimmering by X-ray compared with original method
Light spectrum analysis（XRF）, it can be seen that the content of silica nano material obtained is lower in comparative example 2, and only 67%, and
The content of silica nano material obtained has reached 99% in example 2, it was demonstrated that carries out pickling operation to thick silica
Technique be very important.
It can be gone out by table 1, its tap density of the product that 1-4 of the embodiment of the present invention is obtained is less than comparative example 1 and 2, and purity is big
It is big to improve.
By above embodiments and comparative example it is found that the present invention provides one kind to prepare oxidate nano by raw material of iron tailings
The method of material, including：Iron tailings is comprehensively utilized, environmental pressure is alleviated；It is cheap as raw material preparation using iron tailings
Silicon source；The partial size that precipitating substantially reduces silica nano material is formed under ultrasound environments；Acid is carried out to thick silica
Wash the content that operation improves its silica.Ferric oxide powder and silica nano material preparation condition provided by the invention
Mildly, not high to equipment requirement, daily energy consumption is smaller, rationally utilizes solid waste, reduces cost, be easy to industrialize.
The foregoing is merely section Examples of the invention, are not intended to limit the invention.In every case according to the content of present invention institute
The equivalent changes and modifications done, all for protection scope of the present invention within.
Claims (8)
1. a kind of method for preparing iron oxide and silica nano material simultaneously from iron tailings, it is characterised in that including following step
Suddenly：
1）Iron tailings is ground and is sieved with 100 mesh sieve, obtain it is levigate after iron tailings；
2）By step 1）It is levigate after iron tailings be put into Muffle furnace and be heated to 850-950 DEG C and activated, keep the temperature 4.5-5.5
Hour, the iron tailings powder after activation is made；
3）By step 2）In activation after iron tailings powder and mixed in hydrochloric acid and be stirred to react, filter after reaction, filter residue into
Row drying, filtrate container collection；
4）By step 3）In filter residue and sodium hydrate particle be mixed and stirred for uniformly, being put into Muffle furnace 450-550 DEG C and keeping
1.5-2.5 hours, the iron tailings after alkali fusion reaction is made；
5）By step 4）Iron tailings after middle alkali fusion reaction incorporates in water, and heating stirring reaction is obtained by filtration thick after reaction
Silicon solution；
6）By step 5）In thick silicon solution obtained under ultrasound environments with salt acid for adjusting pH to 6.5-7.5, there are a large amount of precipitatings,
It is filtered after standing, residue collection；
7）To step 6）In filter residue be added hydrochloric acid stirring after filter and dry again, be made silica nano material；
8）By step 3）In filtrate adjust pH to 6.5-7.5 with ammonium hydroxide under ultrasound environments, there is a large amount of precipitatings, mistake after standing
It filters, uses container collection after filter residue and drying；
9）By step 8）Filter residue after middle drying is put into Muffle furnace, roasting temperature 2 hours of 600 DEG C -700 DEG C, finally
Ferric oxide nano powder is made.
2. the method according to claim 1 for preparing iron oxide and silica nano material simultaneously from iron tailings, special
Sign is step 1）In iron tailings component mass fraction be SiO2 45.43%、CaO 13.81%、MgO 13.10%、Al2O3
11.35%、Fe2O310.13%, surplus is impurity.
3. the method according to claim 1 for preparing iron oxide and silica nano material simultaneously from iron tailings, special
Sign is step 3）In concentration of hydrochloric acid be 1-3mol/L, preferably 2mol/L, activation mine tailing and mass ratio be 1:1.6-
2。
4. the method according to claim 1 for preparing iron oxide and silica nano material simultaneously from iron tailings, special
Sign is step 4）In filter residue and sodium hydroxide mass ratio be 1:1.4-2.
5. the method according to claim 1 for preparing iron oxide and silica nano material simultaneously from iron tailings, special
Sign is step 5）In alkali soluble reaction after iron tailings press 1:The solid-to-liquid ratio of 4-6 is added to the water, and stirs at a temperature of 60 DEG C -85 DEG C
Reaction is mixed, thick silicon solution is obtained by filtration.
6. the method according to claim 1 for preparing iron oxide and silica nano material simultaneously from iron tailings, special
Sign is step 7）Middle concentration of hydrochloric acid is 1-3mol/L, preferably 2mol/L, and the volume ratio of filter residue and hydrochloric acid is 1:1.5-2.
7. the method according to claim 1 for preparing iron oxide and silica nano material simultaneously from iron tailings, special
Sign is step 8）Middle ammonia concn is 1-2mol/L.
8. the method according to claim 1 for preparing iron oxide and silica nano material simultaneously from iron tailings, special
The content for levying the silica nano material being is 99%, and partial size is less than 100nm, tap density 0.344-0.372g/
cm3；The tap density of ferric oxide nano powder is 1.068-1.132 g/cm3, partial size is less than 50nm.
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