CN101759210B - Method for extracting high purity alumina and silica gel from coal ash - Google Patents
Method for extracting high purity alumina and silica gel from coal ash Download PDFInfo
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Abstract
The invention discloses a method for extracting high purity alumina and silica gel from coal ash; the method includes the steps of cycle activation, leaching, carbonation, sodium carbonate and water recycling, Si-Al separation, pyrolysis, hydrochloric acid recovery, and realizes the extraction of high purity alumina and silica gel from coal ash. CO2 generated during the whole process, and alkaline, acid and water used in the extraction process can be recovered and used repeatedly. The method has the advantages of high extraction rate of useful compositions, less slag, low cost and simple process. The problem of high slag generation in the alumina extraction process of coal ash in prior art is overcome, more than 95% of Al2O3 in coal ash can be extracted, and more than 90% of silicon dioxide can be extracted through high purity silica gel manner at the same time. The method not only improves the comprehensive utilization rate of coal ash, but also greatly reduces the production cost.
Description
Technical field
The invention belongs to the comprehensive utilization technique field of the solid waste of being discharged in generating, metallurgy, the chemical industry synthetic production process, particularly a kind of method of from flyash, extracting aluminum oxide and silica gel.
Background technology
The ash of the flyash of China storage at present field is unprocessed mostly, air storage.In the flyash 20% is to be easy to blow to airborne cenosphere, is rich in heavy metal, as long as wind-force reaches level Four, flyash will be kicked up, and subsidence range can reach 100,000～150,000 square kilometres, thus the soil around polluting.In addition; Eluviation through weathering and Atmospheric precipitation; Trace toxic heavy metal element (like lead, cadmium, mercury, arsenic, chromium etc.) in the long-term flyash of stacking can permeate the ground, and causes the pollution of soil, surface water body and shallow ground water, influences edatope and water surrounding.
Radioactive substance in the flyash originates from raw coal, and its radionuclide amount there are differences because of former coal district, kind difference.Because radionuclide amounts such as (particularly low grade coal) 226 radium, 232 thoriums, 40 potassium are higher in some coal seam, the also enrichment relatively of radioelement in the flyash of burning back.Therefore, for realizing minimizing, the innoxious and resource utilization of solid waste, the comprehensive utilization of research flyash is significant.
At present flyash be mainly used in backfill, build the road, aspect such as building, although measure greatlyyer with ash, economic benefit is not obvious.Be worth in order to improve utilization of coal ash, people attempt from flyash, extracting valuable material composition.The content of aluminum oxide is only second to silicon-dioxide in the flyash, row second.Especially the content that contains aluminum oxide in the flyash of high alumina is higher, therefore we can say that also flyash is a kind of bauxite resource mineral reserve.Exploit today that reserves reduce day by day because of long-term in the face of the Mineral resources of the earth, strengthen the recycling of flyash equal industrial residue, to solving the Mineral resources shortage, it is significant to improve environment for human survival.
At present, developed countries is paid much attention to the extraction and the development and use that have the high added value component in the flyash, especially utilizes research work that the aspect carries out early from fine chemistry industry, and has obtained satisfied achievement.In recent years, the comprehensive utilization to flyash receives showing great attention to of country, local government and relevant department with disposal.
Summary of the invention
The object of the invention just provides a kind of method of from flyash, extracting high-purity alpha-alumina and silica gel, and this method requires lowly to equipment, and aluminum oxide that is extracted and silica gel are high value added product, the huge market demand.
In order to realize above-mentioned task, the present invention takes following technical solution: comprise the following steps:
Step 1: calcination activation
Get flyash and Na
2CO
3, by flyash: yellow soda ash is that 1: 0.3～1: 4 mass ratio mixes, roasting under 500 ℃～1000 ℃ conditions of temperature then, and roasting time obtained product of roasting in 20 minutes～90 minutes; Calciner connects gas output tube during roasting, and is connected with carbon branch pond;
Step 2: leaching
Add mass concentration in the product of roasting that step 1 is obtained and be 0～20% sodium hydroxide solution, and to make the solid-liquid mass ratio be 1: 3～1: 50,10 ℃～100 ℃ of leaching temperatures, leaching time 5 minutes～90 minutes; The leaching after-filtration obtains filtrating and filter residue respectively.The composite mixture of filter residue and flyash continues the condition circulation calcination activation with step 1, and adopts the leaching of this step method condition to utilize;
Step 3: carbon branch
With step 2 gained filtrating evaporation concentration under condition of negative pressure, concentrating unit connects condensing works simultaneously and reclaims zero(ppm) water; Filtrating be concentrated into original volume 10%～50% after, insert in the carbon branch pond, normal pressure or pressurized conditions feed down CO
2Carry out the carbon branch; Carbon branch temperature remains on 20 ℃～100 ℃, and filtrating pH value 4～10 is divided terminal point as carbon; Carbon divides after-filtration, and filter residue is H
2SiO
3And Al (OH)
3Mixture, filtrating is Na
2CO
3Solution;
Step 4: yellow soda ash and water reclaim
Na with step 3 gained
2CO
3Crystallization of solution negative pressure evaporation and oven dry, promptly recyclable yellow soda ash; The yellow soda ash that reclaims can directly be used for the circulation calcination activation process of filter residue described in step 1 or the step 2 and the composite mixture of flyash; Na
2CO
3In the solution heating negative pressure evaporation process, connect condensing works and storage tank and reclaim zero(ppm) water;
Step 5: the sial separation is also obtained silica gel
H to step 3 gained
2SiO
3And Al (OH)
3Mixture adds the refining hydrochloric acid of 3mol～10mol, and to make the solid-liquid mass ratio be 1: 1～1: 10, keeps 3 minutes～120 minutes after-filtration of reaction under 10 ℃～100 ℃ conditions of temperature, obtains AlCl respectively
3Seminal fluid and filter residue; Filter residue ageing, washing obtain pure silica gel;
Step 6: obtain aluminum oxide
With step 5 gained AlCl
3Seminal fluid concentrates, and obtains AlCl
3Crystal; With AlCl
3Crystal places the smoke evacuation pyrolysis installation, and pyrolysis is 0.5 hour～12 hours under 260 ℃～1200 ℃ conditions, obtains high-purity alpha-alumina, reclaims hydrochloric acid simultaneously.
Further comprise hydrochloric acid recovering step 7, described hydrochloric acid recovering step is two stages below 7 minutes:
Fs is with the AlCl after the aluminium silicon separation in the step 5
3Seminal fluid heating negative pressure evaporation connects condensing works, absorption tower simultaneously, reclaims hydrochloric acid;
Subordinate phase is with AlCl in the step 6
3The hydrogen chloride gas that the crystal pyrolytic process decomposites connects condensing works and is dissolved in the hydrochloric acid that water or fs reclaim, and is the hydrochloric acid of 3mol～8mol thereby form concentration.
Described concentration is hydrochloric acid recycle in step 5 of 3mol～8mol.
The recycle in step 2 of the zero(ppm) water of described recovery, and be used for step 5 the filter residue ageing, the washing to obtain pure silica gel.
The method of described circulation calcination activation is with step 2 gained filter residue and the composite mixture of flyash, with the condition circulation calcination activation of step 1, and to adopt the leaching of step 2 method condition to utilize; In the described mixture of step 2, the shared mass ratio of filter residue can be 0～100%.
Calciner connects gas output tube during described step 1 roasting, and is connected the CO that arranges with carbon branch pond
2Gas directly is used for the carbon branch process of step 3; The product of roasting that step 1 is obtained adds the sodium hydroxide solution of concentration of volume percent 0～20%, and to make the solid-liquid mass ratio be 1: 3～1: 50, and 10 ℃～100 ℃ of leaching temperatures, leaching time are 5 minutes～90 minutes.
With step 2 gained filtrating be concentrated into original volume 10%～50% after, insert in the carbon branch pond, normal pressure or pressurized conditions feed CO down
2Carry out the carbon branch; Carbon branch temperature remains on 20 ℃～100 ℃, and filtrating pH value 4～10 is divided terminal point as carbon.
Na with step 3 gained
2CO
3Yellow soda ash is reclaimed in crystallization of solution negative pressure evaporation and oven dry; The yellow soda ash that reclaims directly is used for the circulation calcination activation process of step 1 or step 2 gained filter residue and the composite combination ash of flyash.
H to step 3 gained
2SiO
3And Al (OH)
3In the mixture, add the refining hydrochloric acid of 3mol～10mol, and to make the solid-liquid mass ratio be 1: 1～1: 10, kept under 10 ℃～100 ℃ conditions of temperature reaction 3 minutes～120 minutes.
The filter residue ageing of step 5 gained, washing obtain pure silica gel; Step 5 gained AlCl
3Crystal places the pyrolysis installation of can discharging fume, and pyrolysis is 0.5 hour～12 hours under 260 ℃～1200 ℃ conditions.
The present invention can obtain the high purity aluminium oxide and the silica gel of high added value from flyash, can extenuate China's flyash and stack land occupation, problem of environment pollution caused.The CO that is produced in the whole technological process
2And all recyclable and realization recycle of employed alkali, acid and water in the leaching process.The present invention has alumina extraction ratio is high, residue is few, cost is low, technological process is simple, simultaneously the characteristic of separable extraction silica gel.Simplified traditional technological processs such as aluminum oxide purifying deironing, reduced cost, having broken through flyash, to extract aluminum oxide deironing cost high and produce the difficult problem of a large amount of residues.
Description of drawings
Fig. 1 is the process flow sheet that from flyash, extracts high purity aluminium oxide and silica gel, also is one embodiment of the present of invention.
Fig. 2 is the recovery process flow sheet of yellow soda ash and water.
Fig. 3 is the process flow sheet of fs salt acid recovery.
Fig. 4 is the process flow sheet of subordinate phase salt acid recovery.
The present invention is described in further detail below in conjunction with embodiment that accompanying drawing and inventor provide.
Embodiment
Fig. 1 is one embodiment of the present of invention, promptly from flyash, extracts the process flow sheet of high purity aluminium oxide and silica gel.Specifically comprise the following steps.
Step 1: calcination activation
Make flyash and Na
2CO
3By flyash: yellow soda ash is that 1: 0.3～1: 4 mass ratio mixes, roasting under 500 ℃～1000 ℃ conditions of temperature then, roasting time 20 minutes～90 minutes.Calciner connects gas output tube during roasting, and is connected with carbon branch pond, is convenient to make the CO that produces during the calcining
2Gas directly is used for carbon branch process.The main thing of sinter after the roasting is nepheline, sodium metaaluminate and water glass mutually.
The chemical reaction that takes place in the roasting process is following:
Al
6Si
2O
13(mullite)+4SiO
2+ 3Na
2CO
3→ 6NaAlSiO
4(nepheline)+3CO
2↑
Al
2O
3+Na
2CO
3＝2NaAlO
2+CO
2↑
SiO
2+Na
2CO
3＝Na
2SiO
3+CO
2↑
Step 2: leaching
In the product of roasting that step 1 is obtained, add mass concentration and be 0～20% sodium hydroxide solution, and to make solid-to-liquid ratio be 1: 3～1: 50, make it under 10 ℃～100 ℃ temperature condition, leach leaching time 5 minutes～90 minutes then.
After the leaching, Na
2SiO
3And NaAlO
2Be dissolved in the water, cross and filter filtrating and filter residue.The composite mixture of filter residue and flyash continues the condition circulation calcination activation with step 1, and adopts the leaching of this step method condition to utilize.
The method of circulation calcination activation is, with step 2 gained filter residue and the composite mixture of flyash (in the mixture, the shared mass ratio of filter residue can be 0～100%), with Na
2CO
3Mixed according to 1: 0.3～1: 4 is even, and roasting is 20 minutes～90 minutes under 500 ℃～1000 ℃ conditions of temperature.Wherein, the chemical reaction that is taken place in the filter residue calcination activation process is following:
NaAlSiO
4(nepheline)+Na
2CO
3=NaAlO
2+ Na
2SiO
3+ CO
2↑
Step 3: carbon branch
With step 2 gained filtrating evaporation concentration under condition of negative pressure, be connected to condensing works simultaneously and reclaim zero(ppm) water.Filtrating is concentrated into original volume 10%～50%, inserts in the carbon branch pond, and normal pressure or pressurized conditions feed CO down
2Carry out the carbon branch.Carbon branch temperature remains on 20 ℃～100 ℃, and filtrating pH value 4～10 is divided terminal point as carbon.The chemical reaction that carbon divides process to take place is following:
Na
2SiO
3+CO
2+H
2O→H
2SiO
3↓+Na
2CO
3
2NaAlO
2+CO
2+3H
2O→2Al(OH)
3↓+Na
2CO
3
2NaOH+CO
2→H
2O+Na
2CO
3
Carbon divides after-filtration, and filter residue is H
2SiO
3And Al (OH)
3Mixture, filtrating is Na
2CO
3Solution.
Step 4: yellow soda ash and water reclaim
Na with step 3 gained
2CO
3Crystallization of solution negative pressure evaporation and oven dry, promptly recyclable yellow soda ash (see figure 2).The yellow soda ash that reclaims directly is used for the circulation calcination activation of combination ash described in calcination activation or the step 2 of step 1 pair flyash.
Na
2CO
3In the solution heating negative pressure evaporation process, connecing condensing works and storage tank is recyclable zero(ppm) water (see figure 2).
Step 5: sial separates and silica gel obtains
H to step 3 gained
2SiO
3And Al (OH)
3Mixture, the refining hydrochloric acid of adding 3mol～10mol is 1: 1～1: 10 in solid-to-liquid ratio, keeps 3 minutes～120 minutes after-filtration of reaction under 10 ℃～100 ℃ conditions of temperature, obtains AlCl respectively
3Seminal fluid and filter residue.Filter residue ageing, washing can get pure silica gel.
It is following that mixture adds the sour chemical reaction that takes place:
Al(OH)
3+3HCl→AlCl
3+3H
2O
Step 6: obtain aluminum oxide
With step 5 gained AlCl
3Seminal fluid concentrates, and obtains AlCl
3Xln.With AlCl
3Crystal places the pyrolysis installation of can discharging fume, and pyrolysis is 0.5 hour～12 hours under 260 ℃～1200 ℃ conditions, obtains high-purity alpha-alumina.
The chemical reaction that pyrolysis takes place is:
2AlCl
3·6H
2O→Al
2O
3+6HCl↑+3H
2O
Through above step, can be with the Al more than 95% in the flyash
2O
3Extract, and simultaneously the mode of the silicon-dioxide more than 90% with high-purity silica gel extracted.
Aforesaid method also comprises the hydrochloric acid recovering step, and described salt acid recovery is divided into following two stages:
Fs is with the AlCl after the aluminium silicon separation in the step 5
3Seminal fluid heating negative pressure evaporation connects condensing works, absorption tower, reclaims hydrochloric acid and sees Fig. 3;
Subordinate phase is with AlCl in the step 6
3The hydrogen chloride gas that the crystal pyrolytic process decomposites connects condensing works and is dissolved in the Hydrogen chloride that water or fs reclaim, and is the hydrochloric acid of 3mol～8mol thereby form concentration, sees Fig. 4.
The hydrochloric acid of described concentration 3mol～8mol is capable of circulation to be used for the sepn process of step 5 sial.
The zero(ppm) water of described recovery is capable of circulation to be used for ageing, the washing to filter residue of step 2 and step 5, thereby obtains pure silica gel.
Below be the embodiment that the contriver provides, need to prove that these embodiment are some more excellent instances, the invention is not restricted to these embodiment.
Embodiment 1
1, gets flyash and Na
2CO
3By 1: 0.8 mixed, stir after, roasting obtained product of roasting in 20 minutes under 700 ℃ of conditions of temperature.Calciner connects gas output tube during roasting, and is connected with carbon branch pond, makes institute's exhaust body directly be used for carbon branch process.
2, it is behind 1% the sodium hydroxide solution that the product of roasting that step 1 is obtained adds concentration, and making solid-to-liquid ratio is 50 minutes after-filtration of leaching under 1: 5,80 ℃ of conditions of temperature, obtains filtrating and filter residue.
3, with step 2 gained filtrating evaporation concentration under condition of negative pressure, be connected to condensing works simultaneously and reclaim zero(ppm) water.After filtrating is concentrated into original volume 20%, feed the CO that step 2 is discharged
2Carry out the carbon branch.Make solution temperature remain on 60 ℃ in the carbon branch process, carbon divides 8 hours after-filtration, and filter residue is H
2SiO
3And Al (OH)
3Mixture, filtrating is Na
2CO
3Solution.
4, the Na that step 3 is obtained
2CO
3The solution negative pressure evaporation reclaims Na
2CO
3The yellow soda ash that reclaims directly is used for the circulation calcination activation process to flyash and filter residue.Na
2CO
3The steam that produces in the solution negative pressure evaporation process connects the recovery of condensing works and storage tank and obtains zero(ppm) water.
5, the filter residue that step 3 is obtained adds the refining hydrochloric acid of 3mol, solid-to-liquid ratio 1: 3, and reaction 80 minutes under 100 ℃ of conditions of temperature.Filtration obtains AlCl
3Seminal fluid and filter residue.Obtain pure silica gel after filter residue ageing, the washing;
6, with step 5 gained AlCl
3Seminal fluid is concentrated into AlCl
3Xln is separated out, and is placed in the pyrolysis installation that the acid recovery system is housed, and pyrolysis is 6 hours under 500 ℃ of conditions, obtains high purity aluminium oxide, reclaims hydrochloric acid simultaneously.
The salt acid recovery is divided into following two stages:
Fs is with the AlCl after the aluminium silicon separation in the step 5
3The seminal fluid negative pressure evaporation connects condensing works, absorption tower, reclaims hydrochloric acid;
Subordinate phase is with AlCl in the step 6
3The hydrogen chloride gas that the crystallization pyrolytic process decomposites connects the condensing and recycling device and is dissolved in the Hydrogen chloride that the fs reclaims, and forms the hydrochloric acid of concentration 3.5mol.
Embodiment 2
1, get step 2 gained filter residue among the embodiment 1, and with itself and Na
2CO
3By 1: 1.2 mixed, stir after, roasting is 20 minutes under 1000 ℃ of conditions of temperature, obtains product of roasting.Calciner connects gas output tube during roasting, and is connected with carbon branch pond, and institute's exhaust body directly is used for carbon branch process.
2, it is 5% sodium hydroxide solution that the product of roasting that step 1 is obtained adds concentration, and to make solid-to-liquid ratio be under 1: 10,50 ℃ of conditions of temperature, leach 60 minutes after-filtration, obtains filtrating and filter residue.
3, with step 2 gained filtrating evaporation concentration under condition of negative pressure, be connected to condensing works simultaneously and reclaim zero(ppm) water.After filtrating is concentrated into original volume 10%, in concentrated filtrate, feed CO
2, treat its pH value to 9 after-filtration, filter residue is H
2SiO
3And Al (OH)
3Mixture, filtrating is Na
2CO
3Solution.
4, the Na that step 3 is obtained
2CO
3The solution negative pressure evaporation reclaims Na
2CO
3Na
2CO
3The steam that produces in the solution negative pressure evaporation process connects the recovery of condensing works and storage tank and obtains zero(ppm) water.
5, the filter residue that step 3 is obtained adds the refining hydrochloric acid of concentration 5mol, and made solid-to-liquid ratio 1: 4, under 90 ℃ of conditions of temperature, reacts 50 minutes then, filters and obtains AlCl
3Seminal fluid obtains pure silica gel after filter residue ageing, the washing;
6, with the AlCl of step 5 gained
3Seminal fluid is concentrated into AlCl
3Xln is separated out, and is placed in the pyrolysis installation that the acid recovery system is housed, and pyrolysis is 4 hours under 800 ℃ of conditions, obtains high purity aluminium oxide, reclaims hydrochloric acid simultaneously.
The salt acid recovery divides two stages:
Fs is with the AlCl after the aluminium silicon separation in the step 5
3The seminal fluid negative pressure evaporation connects condensing works, absorption tower, reclaims hydrochloric acid;
Subordinate phase is with AlCl in the step 6
3The hydrogen chloride gas that the xln pyrolytic process decomposites connects condensing works and is dissolved in the Hydrogen chloride that the fs reclaims, and forms the hydrochloric acid of concentration 3mol.
Embodiment 3
1, gets step 2 gained filter residue among the embodiment 1: flyash: Na
2CO
3By 1: 2: 2 mixed, stir after, roasting obtained product of roasting in 40 minutes under 900 ℃ of conditions of temperature.Calciner connects gas output tube during roasting, and is connected with carbon branch pond, is that institute's exhaust body directly is used for carbon branch process.
2, it is 15% sodium hydroxide solution that the product of roasting that step 1 is obtained adds concentration, and to make solid-to-liquid ratio be under 1: 15,80 ℃ of conditions of temperature, leach 80 minutes after-filtration, obtains filtrating and filter residue.
3, with step 2 gained filtrating evaporation concentration under condition of negative pressure, be connected to condensing works simultaneously and reclaim zero(ppm) water.After filtrating is concentrated into original volume 15%, in concentrated filtrate, feed CO
2, treat its pH value to 9 after-filtration, filter residue is H
2SiO
3And Al (OH)
3Mixture, filtrating is Na
2CO
3Solution.
4, the Na that step 3 is obtained
2CO
3The solution negative pressure evaporation reclaims Na
2CO
3Na
2CO
3The steam that produces in the solution negative pressure evaporation process connects the recovery of condensing works and storage tank and obtains zero(ppm) water.
5, the filter residue that step 3 is obtained, the refining hydrochloric acid of adding concentration 4.5mol, reaction is 60 minutes under solid-to-liquid ratio 1: 8,850 ℃ of conditions of temperature, filters and obtains AlCl
3Seminal fluid obtains pure silica gel after filter residue ageing, the washing;
6, with the AlCl of step 5 gained
3Seminal fluid is concentrated into AlCl
3Xln is separated out, and is placed in the pyrolysis installation that the acid recovery system is housed, and pyrolysis is 2 hours under 1200 ℃ of conditions, obtains high purity aluminium oxide, reclaims hydrochloric acid simultaneously.
The salt acid recovery divides following two stages:
Fs is with the AlCl after the aluminium silicon separation in the step 5
3The seminal fluid negative pressure evaporation connects condensing works, absorption tower, reclaims hydrochloric acid;
Subordinate phase is with AlCl in the step 6
3The hydrogen chloride gas that the xln pyrolytic process decomposites connects condensing works and is dissolved in the Hydrogen chloride that the fs reclaims, and forms the hydrochloric acid of concentration 4mol.
The foregoing description can also be given an example, and needs only in the parameter area of the technical scheme that the present invention provides according to experiment showed, of applicant, and those skilled in the art all can extract high-purity alpha-alumina and silica gel with reference to embodiments of the invention from flyash.
Claims (3)
1. a method of from flyash, extracting high-purity alpha-alumina and silica gel is characterized in that, comprises the following steps:
Step 1: calcination activation
Get flyash and Na
2CO
3, by flyash: yellow soda ash is that 1: 0.3～1: 4 mass ratio mixes, roasting under 500 ℃～1000 ℃ conditions of temperature then, and roasting time obtained product of roasting in 20 minutes～90 minutes; Calciner connects gas output tube during roasting, and is connected with carbon branch pond;
Step 2: leaching
Add mass concentration in the product of roasting that step 1 is obtained and be 0～20% sodium hydroxide solution, and to make the solid-liquid mass ratio be 1: 3～1: 50,10 ℃～100 ℃ of leaching temperatures, leaching time 5 minutes～90 minutes; The leaching after-filtration obtains filtrating and filter residue respectively; The composite mixture of filter residue and flyash continues the condition circulation calcination activation with step 1, and adopts the leaching of this step method condition to utilize;
Step 3: carbon branch
With step 2 gained filtrating evaporation concentration under condition of negative pressure, concentrating unit connects condensing works simultaneously and reclaims zero(ppm) water; Filtrating be concentrated into original volume 10%～50% after, insert in the carbon branch pond, normal pressure or pressurized conditions feed down CO
2Carry out the carbon branch; Carbon branch temperature remains on 20 ℃～100 ℃, and filtrating pH value 4～10 is divided terminal point as carbon; Carbon divides after-filtration, and filter residue is H
2SiO
3And Al (OH)
3Mixture, filtrating is Na
2CO
3Solution;
Step 4: yellow soda ash and water reclaim
Na with step 3 gained
2CO
3Crystallization of solution negative pressure evaporation and oven dry, promptly recyclable yellow soda ash; The yellow soda ash that reclaims can directly be used for the circulation calcination activation process of filter residue described in step 1 or the step 2 and the composite mixture of flyash; Na
2CO
3In the solution heating negative pressure evaporation process, connect condensing works and storage tank and reclaim zero(ppm) water;
Step 5: the sial separation is also obtained silica gel
H to step 3 gained
2SiO
3And Al (OH)
3Mixture adds the refining hydrochloric acid of 3mol～10mol, and to make the solid-liquid mass ratio be 1: 1～1: 10, keeps 3 minutes～120 minutes after-filtration of reaction under 10 ℃～100 ℃ conditions of temperature, obtains AlCl respectively
3Seminal fluid and filter residue; Filter residue ageing, washing obtain pure silica gel;
Step 6: obtain aluminum oxide
With step 5 gained AlCl
3Seminal fluid concentrates, and obtains AlCl
3Crystal; With AlCl
3Crystal places the smoke evacuation pyrolysis installation, and pyrolysis is 0.5 hour～12 hours under 260 ℃～1200 ℃ conditions, obtains high-purity alpha-alumina, reclaims hydrochloric acid simultaneously.
2. the method for claim 1 is characterized in that, the recycle in step 2 of the zero(ppm) water of described recovery, and be used for step 5 the filter residue ageing, the washing to obtain pure silica gel.
3. the method for claim 1 is characterized in that, calciner connects gas output tube during described step 1 roasting, and is connected the CO that arranges with carbon branch pond
2Gas directly is used for the carbon branch process of step 3.
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| CN102180492B (en) * | 2011-01-07 | 2012-10-31 | 潘爱芳 | Method for producing alumina from fly ash |
| CN102180494B (en) * | 2011-01-07 | 2013-04-24 | 潘爱芳 | Method for extracting alumina from coal ash |
| CN102923742B (en) * | 2012-11-19 | 2014-07-09 | 河北工程大学 | Method for comprehensively extracting aluminum and lithium from coal ash |
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| CN106365173B (en) * | 2016-08-29 | 2018-10-02 | 昆明理工大学 | A kind of method that sial slag prepares White Carbon black and water treatment agent |
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| US4254088A (en) * | 1979-03-27 | 1981-03-03 | The United States Of America As Represented By The United States Department Of Energy | Salt-soda sinter process for recovering aluminum from fly ash |
| CN1207719A (en) * | 1995-12-15 | 1999-02-10 | 玛莎尔铝工业有限公司 | Process for recovery of alumina and silica |
| CN101254933A (en) * | 2008-04-02 | 2008-09-03 | 潘爱芳 | Method for extracting high-purity alumina and silica gel from coal ash |
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2010
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4254088A (en) * | 1979-03-27 | 1981-03-03 | The United States Of America As Represented By The United States Department Of Energy | Salt-soda sinter process for recovering aluminum from fly ash |
| CN1207719A (en) * | 1995-12-15 | 1999-02-10 | 玛莎尔铝工业有限公司 | Process for recovery of alumina and silica |
| CN101254933A (en) * | 2008-04-02 | 2008-09-03 | 潘爱芳 | Method for extracting high-purity alumina and silica gel from coal ash |
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