CN108911599B - Method for simultaneously preparing iron oxide and silicon dioxide aerogel pad from iron tailings - Google Patents
Method for simultaneously preparing iron oxide and silicon dioxide aerogel pad from iron tailings Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 223
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 116
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 111
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 33
- 239000004964 aerogel Substances 0.000 title abstract description 30
- 235000012239 silicon dioxide Nutrition 0.000 title abstract description 27
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 51
- 239000004965 Silica aerogel Substances 0.000 claims abstract description 50
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000003365 glass fiber Substances 0.000 claims abstract description 38
- 239000000843 powder Substances 0.000 claims abstract description 31
- 230000032683 aging Effects 0.000 claims abstract description 28
- 239000002994 raw material Substances 0.000 claims abstract description 27
- 238000001035 drying Methods 0.000 claims abstract description 25
- 238000001914 filtration Methods 0.000 claims abstract description 25
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 23
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 23
- 238000002156 mixing Methods 0.000 claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 23
- 238000012986 modification Methods 0.000 claims abstract description 20
- 230000004048 modification Effects 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 239000000706 filtrate Substances 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 15
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 12
- 238000001879 gelation Methods 0.000 claims abstract description 10
- 238000002844 melting Methods 0.000 claims abstract description 9
- 230000008018 melting Effects 0.000 claims abstract description 9
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 9
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003729 cation exchange resin Substances 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 7
- 150000002505 iron Chemical class 0.000 claims abstract description 5
- 230000003213 activating effect Effects 0.000 claims abstract description 3
- 238000000227 grinding Methods 0.000 claims abstract description 3
- 239000011858 nanopowder Substances 0.000 claims abstract description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 64
- 239000000243 solution Substances 0.000 claims description 63
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 44
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 41
- 229910052710 silicon Inorganic materials 0.000 claims description 41
- 239000010703 silicon Substances 0.000 claims description 41
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims description 36
- 239000005051 trimethylchlorosilane Substances 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 16
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 10
- 239000000084 colloidal system Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 8
- 239000002244 precipitate Substances 0.000 claims description 6
- 239000003513 alkali 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
- 229910052593 corundum Inorganic materials 0.000 claims description 3
- 230000004927 fusion Effects 0.000 claims description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 3
- 229910052681 coesite Inorganic materials 0.000 claims description 2
- 229910052906 cristobalite Inorganic materials 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 229910052682 stishovite Inorganic materials 0.000 claims description 2
- 229910052905 tridymite Inorganic materials 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 abstract description 4
- 239000002910 solid waste Substances 0.000 abstract description 4
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 abstract 1
- 239000000499 gel Substances 0.000 description 45
- 238000002360 preparation method Methods 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
- 229910010272 inorganic material Inorganic materials 0.000 description 3
- 239000011147 inorganic material Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 229910002808 Si–O–Si Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000012774 insulation material Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000006261 foam material Substances 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000009270 solid waste treatment Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000352 supercritical drying Methods 0.000 description 1
- 239000011240 wet gel Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/005—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing gelatineous or gel forming binders, e.g. gelatineous Al(OH)3, sol-gel binders
-
- 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
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- 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]
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/20—Mortars, concrete or artificial stone characterised by specific physical values for the density
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- Inorganic Chemistry (AREA)
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- Ceramic Engineering (AREA)
- Physics & Mathematics (AREA)
- Structural Engineering (AREA)
- Dispersion Chemistry (AREA)
- Materials Engineering (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
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- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a method for simultaneously preparing iron oxide and silicon dioxide aerogel cushions from iron tailings. The method comprises the steps of taking iron tailings as raw materials, sequentially grinding and crushing, roasting at high temperature and activating, mixing activated iron tailing powder with hydrochloric acid, stirring and reacting to obtain filter residues and filtrate; mixing and roasting filter residues and sodium hydroxide particles, then melting the mixture into water for heating reaction, passing through cation exchange resin, adjusting the mixture to be neutral by using an ammonia water solution, immersing the mixture into a glass fiber felt, repeatedly extruding the glass fiber felt to uniformly distribute silica sol into the glass fiber felt, standing for gelation to obtain a gel pad, and then aging, solvent exchange and surface modification are carried out to obtain a hydrophobic silica aerogel pad; adjusting pH of the filtrate to alkalescence with ammonia water, standing, filtering, and drying to obtain ferric oxide nanopowder. The whole process has the advantages of cheap and easily-obtained raw materials, low requirement on equipment, mild reaction conditions, capability of treating a large amount of solid waste such as iron tailings and high application value.
Description
Technical Field
The invention belongs to the field of inorganic materials, and particularly relates to a method for simultaneously preparing iron oxide and a silicon dioxide aerogel cushion from iron tailings.
Background
The total development scale of mineral resources in China is in the front of the world, and the outstanding characteristics of iron ore resources in China are low grade and more symbiotic associated ores, so that a large amount of iron tailings can be generated in the ore dressing process, and 2.5-3.0t of tailings are discharged when 1t of iron concentrate is produced. The iron tailings not only occupy a large amount of land, but also pollute soil, water, air and the like, destroy the ecological environment and have great influence.
At present, the comprehensive utilization rate of the iron tailings is low and is less than 20%, most of the iron tailings are used as building fillers, and high-end products are few, mainly because the preparation process is complex, the reaction conditions are harsh and the like, so that the iron tailings cannot be produced in large quantities.
The iron oxide micropowder is an important industrial raw material, has the advantages of light resistance, chemical corrosion resistance, no toxicity and the like, has good dispersibility, tinting strength and ultraviolet absorption capability, and can be used in a plurality of fields such as buildings, coatings, iron metallurgy and the like.
The silicon dioxide aerogel is an inorganic material with high porosity, has the characteristic that common inorganic materials are not easy to burn, has stronger heat preservation performance of organic foam materials, and is a high-quality heat insulation material. However, due to the characteristic that the material is easy to crack, the application space of the material is limited, and a heat insulation material with good heat insulation and heat preservation performance and good mechanical performance is urgently needed.
Aiming at the technical background, the iron tailings are used as raw materials, the iron element can be collected to the maximum extent by preparing the iron oxide powder and the silica aerogel pad at the same time, the silica aerogel pad which has strong heat insulation performance and is not easy to crack is also prepared, and when the iron tailings are treated in a large quantity, a material with good heat insulation performance can be produced, so that the method has great significance.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for simultaneously preparing iron oxide powder and a silicon dioxide aerogel pad by using iron tailings as raw materials, the method can treat a large amount of solid waste of the iron tailings, the reaction condition is mild, the industrialization is easy, and the prepared silicon dioxide aerogel pad and the prepared iron oxide powder are widely applied.
The method for simultaneously preparing the iron oxide and the silicon dioxide aerogel cushion from the iron tailings is characterized by mainly comprising the following steps of:
1) grinding and crushing the iron tailings and sieving the iron tailings with a 100-mesh sieve to obtain finely ground iron tailings;
2) placing the finely ground iron tailings obtained in the step 1) into a muffle furnace, heating to 850-950 ℃, activating, preserving heat for 4.5-5.5 hours, cooling to normal temperature to obtain activated iron tailing powder, mixing the activated iron tailing powder with hydrochloric acid, stirring for reaction, filtering after the reaction is finished, drying filter residues, and collecting filtrate by using a container;
3) mixing the filter residue dried in the step 2) with sodium hydroxide particles, uniformly stirring, keeping the mixture in a muffle furnace at the temperature of 500-600 ℃ for 1.5-2.5 hours, melting the obtained iron tailings after the alkali fusion reaction into water for heating reaction, and filtering to obtain a crude silicon solution after the reaction is finished;
4) passing the crude silicon solution prepared in the step 3) through cation exchange resin, adjusting the pH value to 6.5-7.5 by using an ammonia water solution, immersing a glass fiber felt when the crude silicon solution is not gelled, repeatedly extruding the glass fiber felt to uniformly distribute silica sol into the glass fiber felt, and standing for gelation to obtain a gel pad;
5) aging the gel: adding the gel aging liquid into the gel pad prepared in the step 4), standing and aging at room temperature to obtain an aged gel pad;
6) solvent exchange: immersing the gel pad aged in the step 5) into n-hexane for 22-26 hours to displace water in the gel to obtain a colloid;
7) surface modification: immersing the colloid prepared in the step 6) into the modified solution, standing for 12-24 hours at room temperature, and finally drying the prepared gel at 90-120 ℃ under normal pressure for 6-8 hours to obtain a hydrophobic silica aerogel pad prepared by taking iron tailings as a raw material;
8) adjusting the pH of the filtrate obtained in the step 2) to 7-8 by using ammonia water under an ultrasonic environment, allowing a large amount of precipitate to appear, standing, filtering, drying filter residue, putting the filter residue into a muffle furnace, and roasting at the temperature of 600-700 ℃ for 1.5-2.5 hours to finally obtain the iron oxide nano powder.
The method for simultaneously preparing the iron oxide and the silicon dioxide aerogel cushion from the iron tailings is characterized in that the components of the iron tailings in the step 1) comprise SiO2、CaO、MgO、Al2O3、Fe2O3。
The method for simultaneously preparing the iron oxide and silicon dioxide aerogel pad from the iron tailings is characterized in that the hydrochloric acid concentration in the step 2) is 1-3mol/L, preferably 2mol/L, and the volume ratio of the activated tailing powder to the hydrochloric acid is 1: 1.5-2.1, preferably 1.6-1.8.
The method for simultaneously preparing the ferric oxide and the silicon dioxide aerogel pad from the iron tailings is characterized in that the mass ratio of the filter residue to the sodium hydroxide in the step 3) is 1:1.5-2, the iron tailings after the alkali dissolution reaction are stirred and reacted at the temperature of 60-90 ℃ according to the solid-to-liquid ratio of 1:3-7, and a crude silicon solution is obtained by filtering.
The method for simultaneously preparing the ferric oxide and the silicon dioxide aerogel pad from the iron tailings is characterized in that 2-4mol/L ammonia water solution is added into the crude silicon solution in the step 4) to adjust the pH value, and after the crude silicon solution is uniformly immersed into a glass fiber mat, the mat is hardened to obtain gel.
The method for simultaneously preparing the iron oxide and silicon dioxide aerogel pad from the iron tailings is characterized in that the aging solution in the step 5) is a mixed solution of absolute ethyl alcohol and tetraethoxysilane, and the volume ratio of the absolute ethyl alcohol to the tetraethoxysilane is 8-12: 1.
the method for simultaneously preparing the iron oxide and the silicon dioxide aerogel pad from the iron tailings is characterized in that in the step 7), the modification liquid is a mixed liquid of n-hexane and trimethylchlorosilane, and the volume ratio of the n-hexane to the trimethylchlorosilane is 8-12: 1, preferably 10: 1.
The method for simultaneously preparing the iron oxide and the silicon dioxide aerogel pad from the iron tailings is characterized in that the density of the obtained silicon dioxide aerogel pad is 0.162-0.173g/cm3(ii) a The tap density of the ferric oxide nano powder is 1.063-1.141 g/cm3The particle size is less than 50 nm.
By adopting the technology, compared with the prior art, the invention has the following beneficial effects:
1) according to the invention, solid wastes such as iron tailings and the like are used as raw materials, iron and silicon elements in the solid wastes are reasonably utilized, and the hydrophobic silica aerogel pad is prepared by utilizing a cheap silicon source in the iron tailings; meanwhile, iron in the iron tailings is recycled to prepare iron oxide, and the hydrophobic silica aerogel and the iron oxide are used for the next comprehensive utilization, so that the purpose of treating a large amount of iron tailings is realized, the environmental pressure is relieved, the environmental pollution is reduced, the recycling rate is improved, and the requirement of environmental protection is met;
2) the invention overcomes the characteristic of easy fragmentation of the silicon dioxide aerogel while maintaining the extremely high heat preservation and insulation effect of the silicon dioxide aerogel, and greatly improves the mechanical strength of the silicon dioxide aerogel;
3) the invention provides a normal pressure drying method with mild reaction and short preparation time, which is more beneficial to industrial production than the common supercritical drying method;
4) the invention can obtain the iron oxide powder which can be used as a coloring agent of paint rubber and the like and other industrial purposes while preparing the silicon dioxide aerogel cushion.
Drawings
FIG. 1 is a flow chart of an embodiment of the present invention;
FIG. 2 is an SEM image of a silica aerogel pad made according to example 1 of the present invention;
FIG. 3 is a graph of Fourier Infrared (FTIR) analysis of a silica aerogel mat made in accordance with example 1 of the present invention;
FIG. 4 is an SEM photograph of an iron oxide powder obtained in example 1 of the present invention;
FIG. 5 is a schematic representation of a silica aerogel blanket made in accordance with example 1 of the present invention.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples, but the scope of the present invention is not limited thereto:
example 1 preparation of iron oxide powder and silica aerogel pad
As shown in fig. 1, the preparation method of the iron oxide powder and the silica aerogel pad using the iron tailings as the raw material in the embodiment 1 of the present invention includes the following steps:
(1) the raw material at least comprises iron tailings (SiO) in North China245.43%、CaO 13.81%、MgO 13.10%、Al2O311.35%、Fe2O310.13 percent, and the balance being impurities), sodium hydroxide, hydrochloric acid, concentrated ammonia water, glass fiber felt, normal hexane, trimethylchlorosilane and absolute ethyl alcohol;
(2) sieving the milled iron tailings with a 100-mesh sieve, then placing the iron tailings into a muffle furnace, heating the iron tailings to 850 ℃, keeping the temperature for 4.5 hours, cooling the iron tailings to the normal temperature, mixing the iron tailings with 2mol/L hydrochloric acid according to the volume ratio of 1:1.5, stirring the mixture for 2 hours, filtering the mixture to obtain filter residues, drying the filter residues, and collecting the filtrate by using a container;
(3) mixing the filter residue and sodium hydroxide according to the mass ratio of 1:1.5, uniformly stirring, heating to 500 ℃, keeping for 1.5 hours, taking out, melting into water, stirring and reacting at 60 ℃ for 24 hours according to the solid-liquid ratio of 1:3, and filtering to obtain a crude silicon solution;
(4) passing the crude silicon solution through cation exchange resin, then adjusting the pH value to be =6.5 by using 2mol/L ammonia water solution, immersing the crude silicon solution into a glass fiber felt when the crude silicon solution is not gelled, repeatedly extruding the glass fiber felt to uniformly distribute silica sol into the glass fiber felt, and standing for gelation;
(5) aging the gel: immersing the prepared gel pad into gel aging solution (anhydrous ethanol and tetraethoxysilane are mixed according to the volume of 10: 1), standing at room temperature for 20 hours and aging;
(6) solvent exchange: soaking the aged gel pad into n-hexane for 22 hours for solvent exchange, and displacing water in the gel pad;
(7) surface modification: immersing the prepared colloid into a modification solution (n-hexane and trimethylchlorosilane are mixed according to the volume ratio of 10: 1), standing for 12 hours at room temperature, and finally drying the prepared gel at 90 ℃ under normal pressure for 6 hours to finally obtain a hydrophobic silica aerogel pad prepared by taking iron tailings as a raw material, wherein a physical diagram of the hydrophobic silica aerogel pad is shown in fig. 5;
(8) and (3) adjusting the iron-containing filtrate obtained in the step (2) to pH =7 by using ammonia water in an ultrasonic environment, allowing a large amount of precipitate to appear, standing for 2 hours, filtering, drying filter residues, putting the filter residues into a muffle furnace, and roasting at the temperature of 600 ℃ for 1.5 hours to finally obtain the iron oxide nano powder. And the performance parameters of the obtained iron oxide and silicon dioxide aerogel cushion are measured, and the method comprises the following specific steps:
1) scanning Electron Microscope (SEM) analysis of aerogel blanket prepared in example 1
FIG. 2 is a microstructure of a silica aerogel blanket under a scanning electron microscope. As can be seen from fig. 2, the porous silica aerogel is attached to the glass fiber to fix the glass fiber filaments together, so that the defect that the silica aerogel is soft and fragile is overcome, and the porous silica aerogel belongs to a typical composite aerogel structure;
2) fourier Infrared (FTIR) analysis of the aerogel prepared in example 1
FIG. 3 is a Fourier transform infrared spectrum of a silica aerogel. FromAs can be seen in fig. 3: at 1090 cm-1The strong and wide peak is a Si-O-Si vibration peak; the silica aerogel is proved to be a three-dimensional network structure consisting of Si-O-Si;
3) scanning Electron Microscope (SEM) analysis of the iron oxide powder prepared in example 1
FIG. 4 shows the microstructure of iron oxide powder under an electron scanning microscope. As can be seen from the figure, the prepared iron oxide powder is short rod-shaped particles, has uniform particle size distribution of less than 50nm, and belongs to the field of nano materials.
Example 2 preparation of iron oxide powder and silica aerogel pad
The embodiment 2 of the invention takes iron tailings as raw materials to prepare iron oxide powder and silicon dioxide aerogel pads, and comprises the following steps:
(1) the raw materials at least comprise iron tailings in North China, sodium hydroxide, hydrochloric acid, concentrated ammonia water, glass fiber, normal hexane, trimethylchlorosilane and absolute ethyl alcohol;
(2) sieving the milled iron tailings with a 100-mesh sieve, then placing the iron tailings into a muffle furnace, heating the iron tailings to 950 ℃, keeping the temperature for 5.5 hours, cooling the iron tailings to normal temperature, mixing the iron tailings with 2mol/L hydrochloric acid according to the volume ratio of 1:2.1, stirring the mixture for 4 hours, filtering the mixture to obtain filter residues, drying the filter residues, and collecting the filtrate by using a container;
(3) mixing the filter residue and sodium hydroxide according to the mass ratio of 1:2, uniformly stirring, heating to 600 ℃, keeping for 2.5 hours, taking out, melting into water, stirring and reacting at 90 ℃ for 27 hours according to the solid-liquid ratio of 1:7, and filtering to obtain a crude silicon solution;
(4) passing the crude silicon solution through cation exchange resin, then adjusting the pH value to be =7.5 by using 2mol/L ammonia water solution, immersing the crude silicon solution into a glass fiber felt when the crude silicon solution is not gelled, repeatedly extruding the glass fiber felt to uniformly distribute silica sol into the glass fiber felt, and standing for gelation;
(5) aging the gel: immersing the prepared gel pad into gel aging solution (anhydrous ethanol and tetraethoxysilane are mixed according to the volume of 10: 1), standing at room temperature for 26 hours and aging;
(6) solvent exchange: immersing the aged gel pad into n-hexane for 26 hours for solvent exchange, and displacing water in the gel pad;
(7) surface modification: immersing the prepared colloid into a modification solution (mixing n-hexane and trimethylchlorosilane according to the volume ratio of 10: 1), standing for 24 hours at room temperature, and finally drying the prepared gel at 120 ℃ under normal pressure for 8 hours to finally obtain a hydrophobic silica aerogel pad prepared by taking iron tailings as a raw material;
(8) and (3) adjusting the iron-containing filtrate obtained in the step (2) to pH =8 by using ammonia water in an ultrasonic environment, allowing a large amount of precipitate to appear, standing for 2 hours, filtering, drying filter residues, putting the filter residues into a muffle furnace, and roasting at the temperature of 700 ℃ for 2.5 hours to obtain the iron oxide nano powder. And the performance parameters of the obtained iron oxide and silica aerogel pad are measured, and the performance parameters of the iron oxide and silica nano material are measured in the same way as in example 1.
Example 3 preparation of iron oxide powder and silica aerogel pad
The embodiment 3 of the invention takes iron tailings as raw materials to prepare the iron oxide powder and the silicon dioxide aerogel cushion, and comprises the following steps:
(1) the raw materials at least comprise iron tailings in North China, sodium hydroxide, hydrochloric acid, concentrated ammonia water, glass fiber, normal hexane, trimethylchlorosilane and absolute ethyl alcohol;
(2) sieving the milled iron tailings with a 100-mesh sieve, then placing the iron tailings into a muffle furnace, heating the iron tailings to 900 ℃, keeping the temperature for 5 hours, cooling the iron tailings to the normal temperature, mixing the iron tailings with 2mol/L hydrochloric acid according to the volume ratio of 1:1.8, stirring the mixture for 4.5 hours, filtering the mixture to obtain filter residues, drying the filter residues, and collecting filtrate by using a container;
(3) mixing the filter residue and sodium hydroxide according to a mass ratio of 1:1.7, uniformly stirring, heating to 550 ℃, keeping for 2 hours, taking out, melting into water, stirring and reacting at 85 ℃ for 25 hours according to a solid-liquid ratio of 1:5, and filtering to obtain a crude silicon solution;
(4) passing the crude silicon solution through cation exchange resin, then adjusting the pH value to be =7 by using 2mol/L ammonia water solution, immersing the crude silicon solution into a glass fiber felt when the crude silicon solution is not gelled, repeatedly extruding the glass fiber felt to uniformly distribute silica sol into the glass fiber felt, and standing for gelation;
(5) aging the gel: immersing the prepared gel pad into gel aging solution (anhydrous ethanol and tetraethoxysilane are mixed according to the volume of 10: 1), standing at room temperature for 25 hours and aging;
(6) solvent exchange: soaking the aged gel pad into n-hexane for 24 hours for solvent exchange, and displacing water in the gel pad;
(7) surface modification: immersing the prepared colloid into a modification solution (mixing n-hexane and trimethylchlorosilane according to the volume ratio of 10: 1), standing for 14 hours at room temperature, and finally drying the prepared gel at 80 ℃ under normal pressure for 6 hours to finally obtain a hydrophobic silica aerogel pad prepared by taking iron tailings as a raw material;
(8) and (3) adjusting the iron-containing filtrate obtained in the step (2) to pH =7.5 by using ammonia water in an ultrasonic environment, allowing a large amount of precipitate to appear, standing for 2 hours, filtering, drying filter residues, putting the filter residues into a muffle furnace, and roasting at 650 ℃ for 2 hours to obtain the iron oxide nano powder. And the performance parameters of the obtained iron oxide and silica aerogel pad are measured, and the performance parameters of the iron oxide and silica nano material are measured in the same way as in example 1.
Example 3 preparation of iron oxide powder and silica aerogel pad
The embodiment 3 of the invention takes iron tailings as raw materials to prepare the iron oxide powder and the silicon dioxide aerogel cushion, and comprises the following steps:
(1) the raw materials at least comprise iron tailings in North China, sodium hydroxide, hydrochloric acid, concentrated ammonia water, glass fiber, normal hexane, trimethylchlorosilane and absolute ethyl alcohol;
(2) sieving the milled iron tailings with a 100-mesh sieve, then placing the iron tailings into a muffle furnace, heating the iron tailings to 920 ℃, keeping the temperature for 5 hours, cooling the iron tailings to normal temperature, mixing the iron tailings with 2mol/L hydrochloric acid according to the volume ratio of 1:1.7, stirring the mixture for 4.5 hours, filtering the mixture to obtain filter residues, drying the filter residues, and collecting the filtrate by using a container;
(3) mixing the filter residue and sodium hydroxide according to a mass ratio of 1:1.5, uniformly stirring, heating to 520 ℃, keeping for 2.5 hours, taking out, melting into water, stirring and reacting at 80 ℃ for 23 hours according to a solid-liquid ratio of 1:6, and filtering to obtain a crude silicon solution;
(4) passing the crude silicon solution through cation exchange resin, then adjusting the pH value to be =7.5 by using 2mol/L ammonia water solution, immersing the crude silicon solution into a glass fiber felt when the crude silicon solution is not gelled, repeatedly extruding the glass fiber felt to uniformly distribute silica sol into the glass fiber felt, and standing for gelation;
(5) aging the gel: immersing the prepared gel pad into gel aging solution (anhydrous ethanol and tetraethoxysilane are mixed according to the volume of 10: 1), standing at room temperature for 26 hours and aging;
(6) solvent exchange: soaking the aged gel pad into n-hexane for 22 hours for solvent exchange, and displacing water in the gel pad;
(7) surface modification: immersing the prepared colloid into a modification solution (mixing n-hexane and trimethylchlorosilane according to the volume ratio of 10: 1), standing for 16 hours at room temperature, and finally drying the prepared gel at 90 ℃ under normal pressure for 7 hours to finally obtain a hydrophobic silica aerogel pad prepared by taking iron tailings as a raw material;
(8) and (3) adjusting the pH of the iron-containing filtrate obtained in the step (2) to be 7.5 by using ammonia water in an ultrasonic environment, allowing a large amount of precipitates to appear, standing for 2 hours, filtering, drying filter residues, putting the filter residues into a muffle furnace, roasting at 680 ℃ for 2 hours, and finally obtaining the iron oxide nano powder. And the performance parameters of the obtained iron oxide and silica aerogel pad are measured, and the performance parameters of the iron oxide and silica nano material are measured in the same way as in example 1.
Comparative example 1 preparation of iron oxide powder and silica aerogel pad
Comparative example 1 of the present invention, which uses iron tailings as a raw material to prepare an iron oxide powder and a silica aerogel pad, includes the following steps:
(1) the raw materials at least comprise iron tailings in North China, sodium hydroxide, hydrochloric acid, concentrated ammonia water, glass fiber, normal hexane, trimethylchlorosilane and absolute ethyl alcohol;
(2) sieving the milled iron tailings with a 100-mesh sieve, then placing the iron tailings into a muffle furnace to be heated to 900 ℃, keeping the temperature for 5 hours, cooling the iron tailings at normal temperature, mixing the iron tailings with 2mol/L hydrochloric acid according to the volume ratio of 1:1.5, stirring the mixture for 2 hours, filtering the mixture to obtain filter residues, drying the filter residues, and collecting the filtrate by using a container;
(3) mixing the filter residue and sodium hydroxide according to a mass ratio of 1:1.5, uniformly stirring, heating to 500 ℃, keeping for 1 hour, taking out, melting into water, stirring and reacting at 60 ℃ for 24 hours according to a solid-liquid ratio of 1:3, and filtering to obtain a crude silicon solution;
(4) adjusting the crude silicon solution to be near neutral by using 2mol/L hydrochloric acid, immersing the crude silicon solution into a glass fiber felt when the crude silicon solution is not gelled, repeatedly extruding the glass fiber felt to uniformly distribute silica sol into the glass fiber felt, and standing for gelation;
(5) aging the gel: immersing the prepared gel pad into gel aging solution (anhydrous ethanol and tetraethoxysilane are mixed according to the volume of 10: 1), standing at room temperature for 20 hours and aging;
(6) solvent exchange: soaking the aged gel pad into n-hexane for 20 hours for solvent exchange, and displacing water in the gel pad;
(7) surface modification: immersing the prepared colloid into a modification solution (mixing n-hexane and trimethylchlorosilane according to the volume ratio of 10: 1), standing for 20 hours at room temperature, and finally drying the prepared gel at 70 ℃ under normal pressure for 6 hours to finally obtain the hydrophobic silica aerogel pad prepared by taking the iron tailings as the raw material.
Comparative example 2 preparation of iron oxide powder and silica aerogel pad
In comparative example 2 of the present invention, iron oxide powder and silica aerogel pad are prepared using iron tailings as raw materials, and the method comprises the following steps:
(1) the raw materials at least comprise iron tailings in North China, sodium hydroxide, hydrochloric acid, concentrated ammonia water, glass fiber, normal hexane, trimethylchlorosilane and absolute ethyl alcohol;
(2) sieving the milled iron tailings with a 100-mesh sieve, then placing the iron tailings into a muffle furnace to be heated to 900 ℃, keeping the temperature for 5 hours, cooling the iron tailings at normal temperature, mixing the iron tailings with 2mol/L hydrochloric acid according to the volume ratio of 1:2.1, stirring the mixture for 4 hours, filtering the mixture to obtain filter residues, drying the filter residues, and collecting the filtrate by using a container;
(3) mixing the filter residue and sodium hydroxide according to the mass ratio of 1:2, uniformly stirring, heating to 500 ℃, keeping for 3 hours, taking out, melting into water, stirring and reacting at 90 ℃ for 28 hours according to the solid-liquid ratio of 1:7, and filtering to obtain a crude silicon solution;
(4) passing the crude silicon solution through cation exchange resin, adjusting to be near neutral by using 2mol/L ammonia water solution, immersing the crude silicon solution into a glass fiber felt when the crude silicon solution is not gelled, repeatedly extruding the glass fiber felt to uniformly distribute silica sol into the glass fiber felt, and standing for gelation;
(5) aging the gel: immersing the prepared gel pad into gel aging solution (anhydrous ethanol and tetraethoxysilane are mixed according to the volume of 10: 1), standing at room temperature for 26 hours and aging;
(6) surface modification: immersing the prepared colloid into a modification solution (mixing n-hexane and trimethylchlorosilane according to the volume ratio of 10: 1), standing for 24 hours at room temperature, and finally drying the prepared gel at 80 ℃ under normal pressure for 8 hours to finally obtain the hydrophobic silica aerogel pad prepared by taking the iron tailings as the raw material.
Through the above two comparative examples, comparative example 1 does not perform a cation exchange operation on the crude silicon solution in step (4), and directly adjusts the pH to be neutral to wait for gelation, compared with the original method, the finally prepared silica aerogel cushion is soft, the glass fiber is exposed, and substantially no gel is formed in the preparation process; comparative example 2 the solvent exchange operation was not performed after the gel was aged in step (5), so that the mechanical strength of the silica aerogel mat was not high, mainly because water has a large surface tension and the pores were collapsed when the silica wet gel was dried, resulting in no formation of the silica aerogel mat.
As can be seen from the above examples and comparative examples, the present invention provides a method for simultaneously preparing iron oxide powder and silica aerogel mat using iron tailings as raw materials, comprising: recovering elements such as iron, silicon, aluminum and the like which are rich in the iron tailings; obtaining a cheap silicon source for preparing the silicon dioxide aerogel pad; after a series of aging, solvent exchange and surface modification, drying the prepared silicon dioxide aerogel pad under normal pressure; the prepared iron oxide powder also has wide application in the fields of paint, building and the like. The iron oxide powder and the silicon dioxide aerogel pad provided by the invention have the advantages of mild preparation conditions, short preparation period, large amount of solid waste treatment and easiness in industrialization.
The above description is only a few examples of the present invention, and is not intended to limit the present invention. But all equivalent changes and modifications made according to the contents of the present invention are within the scope of the present invention.
Claims (10)
1. A method for simultaneously preparing iron oxide and silica aerogel mats from iron tailings, characterized by comprising the steps of:
1) grinding and crushing the iron tailings and sieving the iron tailings with a 100-mesh sieve to obtain finely ground iron tailings;
2) placing the finely ground iron tailings obtained in the step 1) into a muffle furnace, heating to 850-950 ℃, activating, preserving heat for 4.5-5.5 hours, cooling to normal temperature to obtain activated iron tailing powder, mixing the activated iron tailing powder with hydrochloric acid, stirring for reaction, filtering after the reaction is finished, drying filter residues, and collecting filtrate by using a container;
3) mixing the filter residue dried in the step 2) with sodium hydroxide particles, uniformly stirring, keeping the mixture in a muffle furnace at the temperature of 500-600 ℃ for 1.5-2.5 hours, melting the obtained iron tailings after the alkali fusion reaction into water for heating reaction, and filtering to obtain a crude silicon solution after the reaction is finished;
4) passing the crude silicon solution prepared in the step 3) through cation exchange resin, adjusting the pH value to 6.5-7.5 by using an ammonia water solution, immersing a glass fiber felt when the crude silicon solution is not gelled, repeatedly extruding the glass fiber felt to uniformly distribute silica sol into the glass fiber felt, and standing for gelation to obtain a gel pad;
5) aging the gel: adding the gel aging liquid into the gel pad prepared in the step 4), standing and aging at room temperature to obtain an aged gel pad;
6) solvent exchange: immersing the gel pad aged in the step 5) into n-hexane for 22-26 hours to displace water in the gel to obtain a colloid;
7) surface modification: immersing the colloid prepared in the step 6) into the modified solution, standing for 12-24 hours at room temperature, and finally drying the prepared gel at 90-120 ℃ under normal pressure for 6-8 hours to obtain a hydrophobic silica aerogel pad prepared by taking iron tailings as a raw material;
8) adjusting the pH of the filtrate obtained in the step 2) to 7-8 by using ammonia water under an ultrasonic environment, allowing a large amount of precipitate to appear, standing, filtering, drying filter residue, putting the filter residue into a muffle furnace, and roasting at the temperature of 600-700 ℃ for 1.5-2.5 hours to finally obtain the iron oxide nano powder.
2. The method for simultaneously preparing iron oxide and silica aerogel mats from iron tailings according to claim 1, wherein the components of the iron tailings in step 1) comprise SiO2、CaO、MgO、Al2O3、Fe2O3。
3. The method for simultaneously preparing iron oxide and silica aerogel mats from iron tailings according to claim 1, wherein the hydrochloric acid concentration in step 2) is 1-3mol/L, and the volume ratio of the activated tailings powder to the hydrochloric acid is 1: 1.5-2.1.
4. The method for simultaneously preparing the iron oxide and silica aerogel pad from the iron tailings according to claim 1, wherein the mass ratio of the filter residue to the sodium hydroxide in the step 3) is 1:1.5-2, the iron tailings after the alkali fusion reaction are stirred and reacted at the temperature of 60-90 ℃ according to the solid-to-liquid ratio of 1:3-7, and the crude silicon solution is obtained by filtering.
5. The method for simultaneously preparing the iron oxide and silica aerogel pads from the iron tailings according to claim 1, wherein 2-4mol/L ammonia water solution is added into the crude silicon solution in the step 4) to adjust the pH value, and the gel pads are obtained after the crude silicon solution is uniformly immersed into the glass fiber felt and hardened.
6. The method for simultaneously preparing the iron oxide and silica aerogel pad from the iron tailings according to claim 1, wherein the aging solution in the step 5) is a mixed solution of anhydrous ethanol and ethyl orthosilicate, and the volume ratio of the anhydrous ethanol to the ethyl orthosilicate is 8-12: 1.
7. the method for simultaneously preparing the iron oxide and the silica aerogel pad from the iron tailings according to claim 1, wherein the modification liquid in the step 7) is a mixed liquid of n-hexane and trimethylchlorosilane, and the volume ratio of the n-hexane to the trimethylchlorosilane is 8-12: 1.
8. the process for simultaneously preparing iron oxide and silica aerogel pads from iron tailings according to claim 1, wherein the obtained silica aerogel pad has a density of 0.162 to 0.173g/cm3(ii) a The tap density of the ferric oxide nano powder is 1.063-1.141 g/cm3The particle size is less than 50 nm.
9. The method for simultaneously preparing iron oxide and silica aerogel mats from iron tailings according to claim 1, wherein the hydrochloric acid concentration in step 2) is 2mol/L, and the volume ratio of the activated tailings powder to the hydrochloric acid is 1.6-1.8.
10. The method for simultaneously preparing the iron oxide and the silica aerogel pad from the iron tailings according to claim 1, wherein the modification liquid in the step 7) is a mixed liquid of n-hexane and trimethylchlorosilane, and the volume ratio of the n-hexane to the trimethylchlorosilane is 10: 1.
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CN111534683A (en) * | 2020-04-13 | 2020-08-14 | 广东工业大学 | Method for enriching iron oxide in iron tailings by using alkali fusion method |
CN112661193B (en) * | 2020-12-18 | 2022-07-19 | 河北工业大学 | Method for simultaneously preparing binary and ternary high-performance composite aerogel by using iron tailings |
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