CN108911599A - A method of iron oxide and aerosil pad are prepared simultaneously from iron tailings - Google Patents
A method of iron oxide and aerosil pad are prepared simultaneously from iron tailings Download PDFInfo
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- CN108911599A CN108911599A CN201810790735.7A CN201810790735A CN108911599A CN 108911599 A CN108911599 A CN 108911599A CN 201810790735 A CN201810790735 A CN 201810790735A CN 108911599 A CN108911599 A CN 108911599A
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- iron tailings
- gel
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- iron
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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
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- 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
Abstract
The invention discloses a kind of methods for preparing iron oxide and aerosil pad simultaneously from iron tailings.It using iron tailings as raw material, it is successively ground crush, high-temperature roasting activation, iron tailings powder after activation and mixed in hydrochloric acid be simultaneously stirred to react, and obtains filter residue and filtrate；Heating is carried out after filter residue is baking mixed with sodium hydrate particle in involvement water to react, cross cation exchange resin; it is adjusted to neutrality again with ammonia spirit; immerse glass mat; repeatedly extrude glass mat; it is evenly distributed to silica solution in glass mat; stand gel after gel mat, then through aging, exchange of solvent, surface it is modified hydrophobic silica aerogel pad；Filtrate adjusts pH alkalescent with ammonium hydroxide, stands filtering, dry ferric oxide nano powder.The entire raw materials technology of the present invention is cheap and easy to get, not high to equipment requirement, and reaction condition is mild, and can largely handle this solid waste of iron tailings, application value with higher.
Description
Technical field
The invention belongs to field of inorganic materials, and in particular to a kind of to prepare iron oxide and silica gas simultaneously from iron tailings
The method of gel mat.
Background technique
Mineral Resources in China exploitation total scale occupy world forefront, and the outstanding feature of China's iron ore deposit is that grade is low, total
Raw associated minerals are more, lead to that a large amount of iron tailings can be generated in ore dressing process, 2.5-3.0t tail will be discharged in every production 1t iron ore concentrate
Mine.Stockpiling iron tailings not only occupies a large amount of soils, also pollutes to soil, water body, air etc., destroys ecological environment, shadow
Sound is very big.
The comprehensive utilization ratio of iron tailings is very low at present, less than 20%, and is mostly used as building filler material, high-end
Product is seldom, and mainly due to factors such as preparation process complexity, severe reaction conditions, being allowed to can not mass production.
Iron oxide micro mist is important the raw material of industry, it not only have many advantages, such as it is fast light, resistant to chemical etching, nontoxic, and
And with good dispersibility, tinting strength, tinting power and the ability for absorbing ultraviolet light, it can be used as the multiple fields such as building, coating, smelting iron.
Aerosil is a kind of inorganic material of high porosity, the spy for both having had common inorganic material nonflammable
Property, and have the stronger thermal insulation property of organic foam material, it is a kind of good heat-insulating heat-preserving material.But due to its material sheet
The characteristic of the easy fragmentation of body, again limits its application space, is badly in need of the thermal insulation material of a kind of heat-insulation and heat-preservation and good mechanical property.
Background in view of the above technology using iron tailings as raw material, while preparing ferric oxide powder and aerosil pad
Both ferro element can be collected to greatest extent, and being also prepared for one kind has stronger heat preservation and insulation, and not easily broken dioxy
SiClx airsetting rubber mat can have the material of preferable heat preservation and insulation while largely processing iron tailings with output, have very big
Meaning.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides one kind using iron tailings as raw material, while preparing ferric oxide powder
And the method for aerosil pad, this method can largely handle this solid waste of iron tailings, and reaction condition
Mildly, it is easy to industrialize, aerosil pad and ferric oxide powder obtained have a wide range of applications again.
A kind of method preparing iron oxide and aerosil pad simultaneously from iron tailings, feature mainly 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, it is made the iron tailings powder after activation after being cooled to room temperature, iron tailings powder after activation and mixed in hydrochloric acid are simultaneously stirred to react, instead
It is filtered after answering, filter residue is dried, filtrate container collection；
3）By step 2）Filter residue and sodium hydrate particle after middle drying are mixed and stirred for uniformly, 500-600 DEG C in Muffle furnace
It is kept for 1.5-2.5 hours, will obtain carrying out heating reaction in the iron tailings involvement water after alkali fusion reacts, and filter after reaction
Thick silicon solution；
4）By step 3）In thick silicon solution obtained cross cation exchange resin, then being adjusted to pH value with ammonia spirit is 6.5-
7.5, glass mat is immersed in its non-gel, glass mat is repeatedly extruded, silica solution is made to be evenly distributed to glass fibers
It ties up in felt, obtains gel mat after standing gel；
5）Gel aging：In step 4）In gel Ageing solution is added in gel mat obtained, stand aging at room temperature, obtain aging
Gel mat afterwards；
6）Exchange of solvent：By step 5）Gel mat after middle aging, which immerses 22-26 hours in n-hexane, replaces the water in gel
Out, colloid is obtained；
7）Surface is modified：By step 6）In colloid obtained immerse modification liquid, stand 12-24 hours at room temperature, will finally be made
90-120 DEG C of gel constant pressure and dry 6-8 hours, be able to iron tailings be raw material preparation hydrophobic silica aerogel pad；
8）By step 2）In filtrate to adjust pH with ammonium hydroxide under ultrasound environments be 7-8, there are a large amount of precipitatings, filtered after standing,
It is put into Muffle furnace after filter residue and drying, roasting temperature 1.5-2.5 hours of 600 DEG C -700 DEG C, iron oxide is finally made and receives
Rice flour body.
The method that the slave iron tailings prepares iron oxide and aerosil pad simultaneously, it is characterised in that step 1）
In the ingredient of iron tailings include SiO2、CaO、MgO、Al2O3、Fe2O3。
The method that the slave iron tailings prepares iron oxide and aerosil pad simultaneously, it is characterised in that step 2）
In concentration of hydrochloric acid be 1-3mol/L, preferably 2mol/L, activation mine tailing and hydrochloric acid volume ratio be 1：1.5-2.1, preferably
1.6-1.8。
The method that the slave iron tailings prepares iron oxide and aerosil pad simultaneously, it is characterised in that step 3）
In filter residue and sodium hydroxide mass ratio be 1:1.5-2, and the iron tailings after alkali soluble reaction presses 1:The solid-to-liquid ratio of 3-7 is 60
It is stirred to react at a temperature of DEG C -90 DEG C, thick silicon solution is obtained by filtration.
The method that the slave iron tailings prepares iron oxide and aerosil pad simultaneously, it is characterised in that step 4）
The middle 2-4mol/L ammonia spirit that is added into thick silicon solution adjusts pH, and after uniformly immersing glass mat, felt pan hardening is solidifying
Glue.
The method that the slave iron tailings prepares iron oxide and aerosil pad simultaneously, it is characterised in that step 5）
In Ageing solution be dehydrated alcohol and ethyl orthosilicate mixed liquor, the volume ratio of dehydrated alcohol and ethyl orthosilicate is 8-12：1.
The method that the slave iron tailings prepares iron oxide and aerosil pad simultaneously, it is characterised in that step 7）
Middle modification liquid is n-hexane and trim,ethylchlorosilane mixed liquor, and the volume ratio of n-hexane and trim,ethylchlorosilane is 8-12：1, it is excellent
It is selected as 10:1.
The method that the slave iron tailings prepares iron oxide and aerosil pad simultaneously, it is characterised in that obtain
The density of aerosil pad is 0.162-0.173g/cm3；The tap density of ferric oxide nano powder is 1.063-
1.141 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 uses the solid waste such as iron tailings for raw material, has carried out reasonable utilization to wherein iron, element silicon, has passed through benefit
With the cheap silicon source in iron tailings, hydrophobic silica aerogel pad is prepared；The iron in iron tailings is recycled simultaneously, system
At iron oxide, hydrophobic silica aerogel and iron oxide are used for the comprehensive utilization of next step, to realize a large amount of processing iron tails
The purpose of mine, on the one hand alleviates environmental pressure, reduces environmental pollution, while improving recovery utilization rate, meets green ring
Guaranteed request；
2）The present invention overcomes the spy of its easy fragmentation while maintenance aerosil high heat insulating effect
Its mechanical strength is substantially improved in point；
3）The present invention provides a kind of reactions mildly, the shorter constant pressure and dry method of preparation time, compared with common supercritical drying
Drying method is more conducive to industrialized production；
4）The present invention available ferric oxide powder while aerosil pad is made can be used as painting rubber etc.
Colorant and other industrial uses.
Detailed description of the invention
Fig. 1 is implementation flow chart of the present invention；
Fig. 2 is the SEM figure of aerosil pad made from present example 1；
Fig. 3 is that the Fourier of aerosil pad made from present example 1 is infrared（FTIR）Analysis chart；
Fig. 4 is the SEM figure of ferric oxide powder made from present example 1；
Fig. 5 is the pictorial diagram that aerosil pad is made in 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 ferric oxide powder and aerosil pad
As shown in Figure 1, the embodiment of the present invention 1 prepares the system of ferric oxide powder and aerosil pad using iron tailings as raw material
Preparation Method includes 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）, sodium hydroxide, hydrochloric acid, concentrated ammonia liquor, glass mat, n-hexane, trimethyl
Chlorosilane, dehydrated alcohol；
（2）Iron tailings after will be levigate sieves with 100 mesh sieve, and is put into Muffle furnace later and is heated to 850 DEG C, is kept for temperature 4.5 hours,
After being cooled to room temperature and 2mol/L hydrochloric acid by volume 1:1.5 are mixed and stirred for 2 hours, filter to take filter residue is dried, filter
Liquid container collection；
（3）By filter residue and sodium hydroxide in mass ratio 1:1.5 are mixed and stirred for uniformly, being heated to 500 DEG C and being kept for 1.5 hours, taken
It incorporates in water out, by 1:3 solid-to-liquid ratio is stirred to react 24 hours at 60 DEG C, and thick silicon solution is obtained by filtration；
（4）Thick silicon solution is crossed into cation exchange resin, is adjusted to pH=6.5 with 2mol/L ammonia spirit later, in its non-gel
When immerse glass mat, repeatedly extrude glass mat, be evenly distributed to silica solution in glass mat, stand solidifying to it
Glue；
（5）Gel aging：Gel mat obtained is immersed into gel Ageing solution（It is 10 that dehydrated alcohol and ethyl orthosilicate, which press volume,:1
Mixing）, aging in 20 hours is stood at room temperature；
（6）Exchange of solvent：Gel mat after aging is immersed into 22 hours progress exchange of solvent in n-hexane, by the water in colloid pad
It cements out；
（7）Surface is modified：Colloid obtained is immersed into modification liquid（N-hexane and trim,ethylchlorosilane by volume 10:1 ratio
Mixing）, 12 hours are stood at room temperature, finally by 90 DEG C of gel constant pressure and dry 6 hours obtained, obtains one kind finally with iron tailings
For the hydrophobic silica aerogel pad of raw material preparation, pictorial diagram is as shown in Figure 5；
（8）By step（2）Middle iron content filtrate is adjusted to pH=7 with ammonium hydroxide under ultrasound environments, a large amount of precipitatings occurs, stands 2 hours
After filter, be put into Muffle furnace after filter residue and drying, roasting temperature 1.5 hours of 600 DEG C, finally be made ferric oxide nano powder
Body.And measured performance parameter has been carried out to resulting iron oxide and aerosil pad, it is specific as follows：
1）Airsetting rubber mat scanning electron microscope prepared by embodiment 1（SEM）Analysis
Fig. 2 is morphology of the aerosil pad under electronic scanner microscope.From figure 2 it can be seen that more
The aerosil attachment in hole on the glass fibers, glass fiber is fixed together, silica airsetting is overcome
The soft frangible disadvantage of colloid, belongs to typical composite aerogel structure；
2）Aeroge Fourier prepared by embodiment 1 is infrared（FTIR）Analysis
Fig. 3 is the Fourier transform infrared spectroscopy figure of aerosil.As can be seen from Figure 3：In 1090 cm-1Place is strong
And wide peak is Si-O-Si vibration peak；Prove the tridimensional network that the aerosil is made of Si-O-Si；
3）The scanning electron microscope of ferric oxide powder prepared by embodiment 1（SEM）Analysis
Fig. 4 is morphology of the ferric oxide powder under electronic scanner microscope.It can be seen from the figure that the oxidation of preparation
Iron powder body is corynebacterium particle, and particle diameter distribution is uniform, is less than 50nm, belongs to nano material scope.
Embodiment 2 prepares ferric oxide powder and aerosil pad
The embodiment of the present invention 2 prepares ferric oxide powder and aerosil pad 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, glass fibre, n-hexane, trimethyl
Chlorosilane, dehydrated alcohol；
（2）Iron tailings after will be levigate sieves with 100 mesh sieve, and is put into Muffle furnace later and is heated to 950 DEG C, is kept for temperature 5.5 hours,
After being cooled to room temperature and 2mol/L hydrochloric acid by volume 1:2.1 are mixed and stirred for 4 hours, filter to take filter residue is dried, filter
Liquid container collection；
（3）By filter residue and sodium hydroxide in mass ratio 1:2 are mixed and stirred for uniformly, being heated to 600 DEG C and being kept for 2.5 hours, taken out
It incorporates in water, by 1:7 solid-to-liquid ratio is stirred to react 27 hours at 90 DEG C, and thick silicon solution is obtained by filtration；
（4）Thick silicon solution is crossed into cation exchange resin, is adjusted to pH=7.5 with 2mol/L ammonia spirit later, in its non-gel
When immerse glass mat, repeatedly extrude glass mat, be evenly distributed to silica solution in glass mat, stand solidifying to it
Glue；
（5）Gel aging：Gel mat obtained is immersed into gel Ageing solution（It is 10 that dehydrated alcohol and ethyl orthosilicate, which press volume,:1
Mixing）, aging in 26 hours is stood at room temperature；
（6）Exchange of solvent：Gel mat after aging is immersed into 26 hours progress exchange of solvent in n-hexane, by the water in colloid pad
It cements out；
（7）Surface is modified：Colloid obtained is immersed into modification liquid（N-hexane and trim,ethylchlorosilane by volume 10:1 ratio
Mixing）, 24 hours are stood at room temperature, finally by 120 DEG C of gel constant pressure and dry 8 hours obtained, obtains one kind finally with iron tail
Mine is the hydrophobic silica aerogel pad of raw material preparation；
（8）By step（2）Middle iron content filtrate is adjusted to pH=8 with ammonium hydroxide under ultrasound environments, a large amount of precipitatings occurs, stands 2 hours
After filter, be put into Muffle furnace after filter residue and drying, roasting temperature 2.5 hours of 700 DEG C, finally be made ferric oxide nano powder
Body.And measured performance parameter, iron oxide and silica nanometer are carried out to resulting iron oxide and aerosil pad
Material property parameter is measured with embodiment 1.
Embodiment 3 prepares ferric oxide powder and aerosil pad
The embodiment of the present invention 3 prepares ferric oxide powder and aerosil pad 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, glass fibre, n-hexane, trimethyl
Chlorosilane, dehydrated alcohol；
（2）Iron tailings after will be levigate sieves with 100 mesh sieve, and is put into Muffle furnace later and is heated to 900 DEG C, is kept for temperature 5 hours, cold
But to after room temperature with 2mol/L hydrochloric acid by volume 1:1.8 are mixed and stirred for 4.5 hours, filter to take filter residue is dried, filter
Liquid container collection；
（3）By filter residue and sodium hydroxide in mass ratio 1:1.7 are mixed and stirred for uniformly, being heated to 550 DEG C and being kept for 2 hours, taken out
It incorporates in water, by 1:5 solid-to-liquid ratio is stirred to react 25 hours at 85 DEG C, and thick silicon solution is obtained by filtration；
（4）Thick silicon solution is crossed into cation exchange resin, pH=7 are adjusted to 2mol/L ammonia spirit later, in its non-gel
Glass mat is immersed, glass mat is repeatedly extruded, is evenly distributed to silica solution in glass mat, is stood solidifying to it
Glue；
（5）Gel aging：Gel mat obtained is immersed into gel Ageing solution（It is 10 that dehydrated alcohol and ethyl orthosilicate, which press volume,:1
Mixing）, aging in 25 hours is stood at room temperature；
（6）Exchange of solvent：Gel mat after aging is immersed into 24 hours progress exchange of solvent in n-hexane, by the water in colloid pad
It cements out；
（7）Surface is modified：Colloid obtained is immersed into modification liquid（N-hexane and trim,ethylchlorosilane by volume 10:1 ratio
Mixing）, 14 hours are stood at room temperature, finally by 80 DEG C of gel constant pressure and dry 6 hours obtained, obtains one kind finally with iron tailings
For the hydrophobic silica aerogel pad of raw material preparation；
（8）By step（2）Middle iron content filtrate is adjusted to pH=7.5 with ammonium hydroxide under ultrasound environments, a large amount of precipitatings occurs, it is small to stand 2
When after filter, be put into Muffle furnace after filter residue and drying, roasting temperature 2 hours of 650 DEG C, finally be made ferric oxide nano powder
Body.And measured performance parameter, iron oxide and silica nanometer are carried out to resulting iron oxide and aerosil pad
Material property parameter is measured with embodiment 1.
Embodiment 3 prepares ferric oxide powder and aerosil pad
The embodiment of the present invention 3 prepares ferric oxide powder and aerosil pad 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, glass fibre, n-hexane, trimethyl
Chlorosilane, dehydrated alcohol；
（2）Iron tailings after will be levigate sieves with 100 mesh sieve, and is put into Muffle furnace later and is heated to 920 DEG C, is kept for temperature 5 hours, cold
But to after room temperature with 2mol/L hydrochloric acid by volume 1:1.7 are mixed and stirred for 4.5 hours, filter to take filter residue is dried, filter
Liquid container collection；
（3）By filter residue and sodium hydroxide in mass ratio 1:1.5 are mixed and stirred for uniformly, being heated to 520 DEG C and being kept for 2.5 hours, taken
It incorporates in water out, by 1:6 solid-to-liquid ratio is stirred to react 23 hours at 80 DEG C, and thick silicon solution is obtained by filtration；
（4）Thick silicon solution is crossed into cation exchange resin, is adjusted to pH=7.5 with 2mol/L ammonia spirit later, in its non-gel
When immerse glass mat, repeatedly extrude glass mat, be evenly distributed to silica solution in glass mat, stand solidifying to it
Glue；
（5）Gel aging：Gel mat obtained is immersed into gel Ageing solution（It is 10 that dehydrated alcohol and ethyl orthosilicate, which press volume,:1
Mixing）, aging in 26 hours is stood at room temperature；
（6）Exchange of solvent：Gel mat after aging is immersed into 22 hours progress exchange of solvent in n-hexane, by the water in colloid pad
It cements out；
（7）Surface is modified：Colloid obtained is immersed into modification liquid（N-hexane and trim,ethylchlorosilane by volume 10:1 ratio
Mixing）, 16 hours are stood at room temperature, finally by 90 DEG C of gel constant pressure and dry 7 hours obtained, obtains one kind finally with iron tailings
For the hydrophobic silica aerogel pad of raw material preparation；
（8）By step（2）Middle iron content filtrate is adjusted to pH=7.5 with ammonium hydroxide under ultrasound environments, a large amount of precipitatings occurs, it is small to stand 2
When after filter, be put into Muffle furnace after filter residue and drying, roasting temperature 2 hours of 680 DEG C, finally be made ferric oxide nano powder
Body.And measured performance parameter, iron oxide and silica nanometer are carried out to resulting iron oxide and aerosil pad
Material property parameter is measured with embodiment 1.
Comparative example 1 prepares ferric oxide powder and aerosil pad
Comparative example 1 of the present invention prepares ferric oxide powder and aerosil pad 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, glass fibre, n-hexane, trimethyl
Chlorosilane, dehydrated alcohol；
（2）Iron tailings after will be levigate sieves with 100 mesh sieve, and is put into Muffle furnace later and is heated to 900 DEG C, is kept for temperature 5 hours, often
After temperature is cooling with 2mol/L hydrochloric acid by volume 1:1.5 are mixed and stirred for 2 hours, filter to take filter residue is dried, filtrate use
Container collection；
（3）By filter residue and sodium hydroxide in mass ratio 1:1.5 are mixed and stirred for uniformly, being heated to 500 DEG C and being kept for 1 hour, taken out
It incorporates in water, by 1:3 solid-to-liquid ratio is stirred to react 24 hours at 60 DEG C, and thick silicon solution is obtained by filtration；
（4）Near thick silicon solution is adjusted to neutrality with 2mol/L hydrochloric acid, glass mat is immersed in its non-gel, is squeezed repeatedly
Glass mat is pressed, is evenly distributed to silica solution in glass mat, is stood to its gel；
（5）Gel aging：Gel mat obtained is immersed into gel Ageing solution（It is 10 that dehydrated alcohol and ethyl orthosilicate, which press volume,:1
Mixing）, aging in 20 hours is stood at room temperature；
（6）Exchange of solvent：Gel mat after aging is immersed into 20 hours progress exchange of solvent in n-hexane, by the water in colloid pad
It cements out；
（7）Surface is modified：Colloid obtained is immersed into modification liquid（N-hexane and trim,ethylchlorosilane by volume 10:1 ratio
Mixing）, 20 hours are stood at room temperature, finally by 70 DEG C of gel constant pressure and dry 6 hours obtained, obtains one kind finally with iron tailings
For the hydrophobic silica aerogel pad of raw material preparation.
Comparative example 2 prepares ferric oxide powder and aerosil pad
Comparative example 2 of the present invention prepares ferric oxide powder and aerosil pad 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, glass fibre, n-hexane, trimethyl
Chlorosilane, dehydrated alcohol；
（2）Iron tailings after will be levigate sieves with 100 mesh sieve, and is put into Muffle furnace later and is heated to 900 DEG C, is kept for temperature 5 hours, often
After temperature is cooling with 2mol/L hydrochloric acid by volume 1:2.1 are mixed and stirred for 4 hours, filter to take filter residue is dried, filtrate use
Container collection；
（3）By filter residue and sodium hydroxide in mass ratio 1:2 are mixed and stirred for uniformly, being heated to 500 DEG C and being kept for 3 hours, taking-up is melted
Enter in water, by 1:7 solid-to-liquid ratio is stirred to react 28 hours at 90 DEG C, and thick silicon solution is obtained by filtration；
（4）Thick silicon solution is crossed into cation exchange resin, be adjusted to neutrality later with 2mol/L ammonia spirit near, do not coagulate at it
Glass mat is immersed when glue, repeatedly extrudes glass mat, is evenly distributed to silica solution in glass mat, is stood to it
Gel；
（5）Gel aging：Gel mat obtained is immersed into gel Ageing solution（It is 10 that dehydrated alcohol and ethyl orthosilicate, which press volume,:1
Mixing）, aging in 26 hours is stood at room temperature；
（6）Surface is modified：Colloid obtained is immersed into modification liquid（N-hexane and trim,ethylchlorosilane by volume 10:1 ratio
Mixing）, 24 hours are stood at room temperature, finally by 80 DEG C of gel constant pressure and dry 8 hours obtained, obtains one kind finally with iron tailings
For the hydrophobic silica aerogel pad of raw material preparation.
By two above comparative example, comparative example 1 is in step（4）In to thick silicon solution carry out cation exchange behaviour
Make, pH is directly adjusted to neutrality to gel, compared with original method, the aerosil pad finally prepared feels like jelly, glass fibers
It ties up exposed, there is no to form gel during the preparation process；Comparative example 2 is in step（5）Solvent friendship is not carried out after gel aging
Operation is changed, keeps aerosil pad mechanical strength obtained not high, being primarily due to water has very big surface tension, two
By duct be collapsed when silica wet gel is dry, cause not form aerosil pad.
By above embodiments and comparative example it is found that the present invention provides one kind to prepare iron oxide by raw material of iron tailings simultaneously
The method of powder and aerosil pad, including：The elements such as the iron, silicon, aluminium being rich in iron tailings are recycled；It obtains
A kind of cheap silicon source preparing aerosil pad；Carrying out a series of aging, exchange of solvent, surface modification
Afterwards, aerosil pad obtained is enable to be dried under normal pressure；Ferric oxide powder obtained is also in coating, building
Equal fields extensive application.The preparation condition of ferric oxide powder and aerosil pad provided by the invention is mild, system
The standby period is short, largely handles solid waste, is 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 aerosil pad 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, it is made the iron tailings powder after activation after being cooled to room temperature, iron tailings powder after activation and mixed in hydrochloric acid are simultaneously stirred to react, instead
It is filtered after answering, filter residue is dried, filtrate container collection；
3）By step 2）Filter residue and sodium hydrate particle after middle drying are mixed and stirred for uniformly, 500-600 DEG C in Muffle furnace
It is kept for 1.5-2.5 hours, will obtain carrying out heating reaction in the iron tailings involvement water after alkali fusion reacts, and filter after reaction
Thick silicon solution；
4）By step 3）In thick silicon solution obtained cross cation exchange resin, then being adjusted to pH value with ammonia spirit is 6.5-
7.5, glass mat is immersed in its non-gel, glass mat is repeatedly extruded, silica solution is made to be evenly distributed to glass fibers
It ties up in felt, obtains gel mat after standing gel；
5）Gel aging：In step 4）In gel Ageing solution is added in gel mat obtained, stand aging at room temperature, obtain aging
Gel mat afterwards；
6）Exchange of solvent：By step 5）Gel mat after middle aging, which immerses 22-26 hours in n-hexane, replaces the water in gel
Out, colloid is obtained；
7）Surface is modified：By step 6）In colloid obtained immerse modification liquid, stand 12-24 hours at room temperature, will finally be made
90-120 DEG C of gel constant pressure and dry 6-8 hours, be able to iron tailings be raw material preparation hydrophobic silica aerogel pad；
8）By step 2）In filtrate to adjust pH with ammonium hydroxide under ultrasound environments be 7-8, there are a large amount of precipitatings, filtered after standing,
It is put into Muffle furnace after filter residue and drying, roasting temperature 1.5-2.5 hours of 600 DEG C -700 DEG C, iron oxide is finally made and receives
Rice flour body.
2. the method according to claim 1 for preparing iron oxide and aerosil pad simultaneously from iron tailings, special
Sign is step 1）In the ingredient of iron tailings include SiO2、CaO、MgO、Al2O3、Fe2O3。
3. the method according to claim 1 for preparing iron oxide and aerosil pad simultaneously from iron tailings, special
Sign is step 2）In concentration of hydrochloric acid be 1-3mol/L, preferably 2mol/L, activation mine tailing and hydrochloric acid volume ratio be 1：
1.5-2.1 preferably 1.6-1.8.
4. the method according to claim 1 for preparing iron oxide and aerosil pad simultaneously from iron tailings, special
Sign is step 3）In filter residue and sodium hydroxide mass ratio be 1:1.5-2, and the iron tailings after alkali soluble reaction presses 1:3-7
Solid-to-liquid ratio be stirred to react at a temperature of 60 DEG C -90 DEG C, thick silicon solution is obtained by filtration.
5. the method according to claim 1 for preparing iron oxide and aerosil pad simultaneously from iron tailings, special
Sign is step 4）The middle 2-4mol/L ammonia spirit that is added into thick silicon solution adjusts pH, after uniformly immersing glass mat, felt
Pad hardening is gel.
6. the method according to claim 1 for preparing iron oxide and aerosil pad simultaneously from iron tailings, special
Sign is step 5）In Ageing solution be dehydrated alcohol and ethyl orthosilicate mixed liquor, the volume of dehydrated alcohol and ethyl orthosilicate
Than for 8-12：1.
7. the method according to claim 1 for preparing iron oxide and aerosil pad simultaneously from iron tailings, special
Sign is step 7）Middle modification liquid is n-hexane and trim,ethylchlorosilane mixed liquor, the volume ratio of n-hexane and trim,ethylchlorosilane
For 8-12：1, preferably 10:1.
8. the method according to claim 1 for preparing iron oxide and aerosil pad simultaneously from iron tailings, special
The density for levying the aerosil pad being is 0.162-0.173g/cm3；The tap density of ferric oxide nano powder
For 1.063-1.141 g/cm3, partial size is less than 50nm.
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