CN103708514A - Method for extracting aluminum oxide from activated kaolin - Google Patents
Method for extracting aluminum oxide from activated kaolin Download PDFInfo
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- CN103708514A CN103708514A CN201310689960.9A CN201310689960A CN103708514A CN 103708514 A CN103708514 A CN 103708514A CN 201310689960 A CN201310689960 A CN 201310689960A CN 103708514 A CN103708514 A CN 103708514A
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- ammonium sulfate
- kaolin
- aluminum oxide
- solid
- ammonium
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention relates to a method for extracting aluminum oxide from activated kaolin, which comprises the following: activating kaolin at high temperature, mixing with ammonium sulfate, sintering the mixture, dissolving out the solid sintered charge to obtain a solution containing aluminum ammonium sulfate, carrying out cooling crystallization or evaporation crystallization on the solution containing aluminum ammonium sulfate to obtain solid aluminum ammonium sulfate, preparing the solid aluminum ammonium sulfate into a solution, reacting the aluminum ammonium sulfate solution with ammonia water to obtain an aluminum hydroxide-ammonium sulfate mixed solution, filtering, washing to obtain solid aluminum hydroxide, and roasting the aluminum hydroxide to obtain the aluminum oxide product, wherein the ammonium sulfate entering the liquid phase is evaporated for cyclic use. The mixture of the ammonium sulfate and high-temperature activated kaolin is sintered, so the extraction rate of aluminum oxide is high, and the corrosivity for equipment is low in the sintering process; the ammonium sulfate can be recycled, and the residues can be used for making building materials and the like, thereby saving the cost and protecting the environment; and the integrated process can easily implement industrialization.
Description
Technical field
The present invention relates to relate to a kind of method that residue after aluminum oxide is extracted in aluminum oxide and comprehensive utilization thereof of extracting in kaolin from activating.
Background technology
At present, the production of aluminum oxide mainly be take bauxite as raw material, and the production method of aluminum oxide is mainly alkaline process, comprises Bayer process, sintering process and integrated process.China is alumina producing big country, it is again the relatively poor country of bauxite, at present the whole nation is found out and the bauxite resource reserves of inferring guarantee that to China's aluminum oxide industry degree is low, so resource problem has become one of subject matter of restriction China aluminium industrial sustainable development.
China's kaolin, flyash, coal gangue reserves are huge, and exploitation kaolin, flyash, coal gangue are to China's aluminium industrial expansion important in inhibiting.
Existing lime sinter process is from the patent of Coaseries kaolin aluminium oxide extraction process, but sintering process produces a large amount of solid slags, is unfavorable for large-scale industrial production.
Summary of the invention
The present invention is directed to the deficiency that prior art exists, propose a kind of processing method simple, low to the erosion resistance requirement of equipment, be easy to the method for aluminum oxide of extracting in kaolin that heavy industrialization is applied from activating.
The technical scheme that the present invention solves the problems of the technologies described above is as follows:
Step 1: kaolin is carried out to high-temperature activation;
Step 2: ammonium sulfate is mixed and carries out sintering with kaolin after high-temperature activation;
Step 3: gained solid sintered material obtains solution and the residue of sulfur acid aluminium ammonium after stripping;
Step 4: after the solution of sulfur acid aluminium ammonium is filtered, evaporative crystallization or decrease temperature crystalline obtain the exsiccated ammonium alum of solid;
Step 5: solid sulphuric acid aluminium ammonium wiring solution-forming and ammoniacal liquor are reacted, obtain the mixing solutions of aluminium hydroxide and ammonium sulfate;
Step 6: the ammonium sulfate that enters liquid phase is obtained to solid ammonium sulfate through evaporation, continue to recycle;
Step 7: the aluminium hydroxide that step 5 is obtained and the mixing solutions of ammonium sulfate, through filtration washing, obtain the aluminium hydroxide of solid;
Step 8: aluminium hydroxide obtains alumina product after roasting.
On the basis of technique scheme, the present invention can also do following improvement.
Further, in described step 1, kaolin is carried out to high-temperature activation, activation temperature is 280-1400 ℃.
Further, in described step 2 ammonium sulfate allocate into ratio of components while carrying out sintering in kaolin after activation with ammonium sulfate/activation afterwards the molecular ratio of Alumina from Kaolin count 2:1-13:1; Sintering temperature is 250-920 ℃, and sintering time is 0.1-6 hours.
Further, in described step 3, be the material after water normal pressure digestion sintering, stripping temperature is 45-98 ℃, adopts filtering separation or settlement separate method that solid phase residue is separated after stripping, after stripping, solid phase residue washes with water, and washing water are for stripping sintered material.
Further, in described step 5, the solid sulphuric acid aluminium ammonium after crystallization is added to water and be made into the solution of counting 4.5g/L-50g/L with alumina concentration, ammonia soln concentration is 2%-30%, and reaction end pH value is controlled between 3-11.
Further, in described step 7, the method for separated aluminium hydroxide is filtering separation or settlement separate.
Further, in described step 3, the main component of residue is SiO
2, can be used for producing white carbon black or material of construction.
Further, described raw material is kaolin, can be also flyash, coal gangue.
The invention has the beneficial effects as follows: the residue that the present invention extracts in kaolin, flyash, coal gangue after aluminum oxide from activating can be reused, and as for the production of white carbon black and material of construction etc., has reduced the discharge of waste residue.After the ammonium sulfate simultaneously using and activation, kaolin mixes, little to equipment corrosion, and ammonium sulfate can recycle, cost-saving environmental protection again, and integrated artistic is easy to realize industrialization.
Accompanying drawing explanation
Fig. 1 is that the present invention extracts the process flow sheet of aluminum oxide from activating in kaolin.
Embodiment
Below in conjunction with accompanying drawing, principle of the present invention and feature are described.
As shown in Figure 1, said method comprising the steps of:
Step 1: kaolin is carried out to high-temperature activation, and activation temperature is 280-1400 ℃.
Step 2: ammonium sulfate is mixed and carries out sintering with kaolin after high-temperature activation.Ratio of components when ammonium sulfate is allocated into and carried out sintering in kaolin after activation with ammonium sulfate/activation afterwards the molecular ratio of Alumina from Kaolin count 2:1-13:1; Sintering temperature is 250-920 ℃, and sintering time is 0.1-6 hours.After sintering, obtain solid sintered material and ammonia, ammonia condensation obtains ammoniacal liquor after absorbing, and divides the raw material of reaction for step 5 ammonia.
Step 3: gained solid sintered material obtains solution and the residue of sulfur acid aluminium ammonium after stripping.Water normal pressure digestion sintered material, stripping temperature is 45-98 ℃, can have higher digesting efficiency of alumina.After stripping, the separation of solid phase residue can adopt filtering separation or settlement separate method to realize.For the water of stripping sintered material, can be new water, can be also the washing water of stripping solid phase residue.The main component of residue is SiO2.
Step 4: after the solution of sulfur acid aluminium ammonium is filtered, evaporative crystallization or decrease temperature crystalline obtain the exsiccated ammonium alum of solid.The solution of the sulfur acid aluminium ammonium obtaining after sintered material stripping, obtains solid sulphuric acid aluminium ammonium by decrease temperature crystalline or evaporative crystallization, simultaneously the impurity such as iron in effective separated dissolution fluid.
Step 5: solid sulphuric acid aluminium ammonium wiring solution-forming and ammoniacal liquor are reacted, obtain the mixing solutions of aluminium hydroxide and ammonium sulfate.Solid sulphuric acid aluminium ammonium is added to water and be made into the solution of counting 4.5g/L-50g/L with alumina concentration, the ammoniacal liquor that is 2%-30% by concentration reacts with aluminum ammonium sulfate solution, and this mixing liquid control of reaction end point is between pH value 3-11.Ammoniacal liquor carrys out the ammonia of kaolin after self-activation (or flyash, coal gangue) and the sintering circuit gained of ammonium sulfate, and ammonia water is absorbed and generates ammoniacal liquor.
Step 6: the ammonium sulfate that enters liquid phase is obtained to solid ammonium sulfate through evaporation, continue to recycle.
Step 7: the aluminium hydroxide that step 5 is obtained and the mixing solutions of ammonium sulfate, through filtration washing, obtain the aluminium hydroxide of solid; The method of separated aluminium hydroxide is filtering separation or settlement separate.
Step 8: aluminium hydroxide obtains alumina product after roasting.
The solid sample residue extracting in kaolin from activating after aluminum oxide can be reused, as for the production of white carbon black and material of construction etc.Present method raw material used can be also flyash and coal gangue.
The method applied in the present invention is mainly based on the following principles of chemistry:
Sintering reaction:
4(NH
4)2SO
4+Al
2O
3·2SiO
2·2H
2O=2NH
4Al(SO
4)
2+6NH
3+5H
2O+2SiO
2
Ammonia divides reaction:
NH
4Al(SO
4)
2+3NH
3·H
2O=Al(OH)
3+2(NH
4)
2SO
4
Divide four embodiment to be described in further detail the method that reclaims aluminum oxide from red mud of the present invention below.
Embodiment 1
Adopt Chinese somewhere kaolin, chemical composition is aluminum oxide 37%, silicon-dioxide 44%, it is carried out to high-temperature activation, 280 ℃ of activation temperatures, by the molecular ratio of Alumina from Kaolin after ammonium sulfate/activation, count 2:1 batching, 250 ℃ of sintering temperatures, reaction times is 0.1 hour, sintered material stripping under 45 ℃ of conditions, dissolution fluid obtains exsiccated ammonium alum solid after crystallization, solid sulphuric acid aluminium ammonium is made into the solution of counting 4.5g/L with alumina concentration, the ammoniacal liquor of 2% concentration is reacted with aluminum ammonium sulfate solution, generate the solution of aluminium hydroxide and ammonium sulfate, this mixing liquid control of reaction end point is at pH value 3.Through filtering separation or settlement separate method, aluminium hydroxide is separated, aluminium hydroxide is washed, the aluminium hydroxide after washing carries out roasting, obtains alumina product after roasting.Gained alumina product impurity chemical composition: Fe
2o
3: 0.02%, SiO
2: 0.01%.
Embodiment 2
Adopt somewhere, inner mongolia kaolin, chemical composition is aluminum oxide 39%, silicon-dioxide 47%, it is carried out to high-temperature activation, 1400 ℃ of activation temperatures, by the molecular ratio of Alumina from Kaolin after ammonium sulfate/activation, count 13:1 batching, 920 ℃ of sintering temperatures, reaction times is 6 hours, sintered material stripping under 98 ℃ of conditions, dissolution fluid obtains exsiccated ammonium alum solid after crystallization, solid sulphuric acid aluminium ammonium is made into the solution of counting 50g/L with alumina concentration, the ammoniacal liquor of 30% concentration is reacted with aluminum ammonium sulfate solution, generate the solution of aluminium hydroxide and ammonium sulfate, this mixing liquid control of reaction end point is at pH value 11.Through filtering separation or settlement separate method, aluminium hydroxide is separated, aluminium hydroxide is washed, the aluminium hydroxide after washing carries out roasting, obtains alumina product after roasting.Gained alumina product impurity chemical composition: Fe
2o
3: 0.01%, SiO
2: 0.01%.
Embodiment 3
Adopt Chinese somewhere coal gangue, through levigate fragmentation, chemical composition is aluminum oxide 25%, silicon-dioxide 60%, it is carried out to high-temperature activation, 1120 ℃ of activation temperatures, by the molecular ratio of aluminum oxide in coal gangue after ammonium sulfate/activation, count 11:1 batching, 670 ℃ of sintering temperatures, reaction times is 5.9 hours, sintered material stripping under 53 ℃ of conditions, dissolution fluid obtains exsiccated ammonium alum solid after crystallization, solid sulphuric acid aluminium ammonium is made into the solution of counting 45.5g/L with alumina concentration, the ammoniacal liquor of 28% concentration is reacted with aluminum ammonium sulfate solution, generate the solution of aluminium hydroxide and ammonium sulfate, this mixing liquid control of reaction end point is at pH value 8.Through filtering separation or settlement separate method, aluminium hydroxide is separated, aluminium hydroxide is washed, the aluminium hydroxide after washing carries out roasting, obtains alumina product after roasting.Gained alumina product impurity chemical composition: Fe
2o
3: 0.02%, SiO
2: 0.02%.
Embodiment 4
Adopt the flyash in Chinese somewhere, chemical composition is aluminum oxide 41%, silicon-dioxide 42%, it is carried out to high-temperature activation, 700 ℃ of activation temperatures, by the molecular ratio of aluminum oxide in flyash after ammonium sulfate/activation, count 7.5:1 batching, 585 ℃ of sintering temperatures, reaction times is 3.05 hours, sintered material stripping under 71.5 ℃ of conditions, dissolution fluid obtains exsiccated ammonium alum solid after crystallization, solid sulphuric acid aluminium ammonium is made into the solution of counting 27.25g/L with alumina concentration, the ammoniacal liquor of 16% concentration is reacted with aluminum ammonium sulfate solution, generate the solution of aluminium hydroxide and ammonium sulfate, this mixing liquid control of reaction end point is at pH value 7.Through filtering separation or settlement separate method, aluminium hydroxide is separated, aluminium hydroxide is washed, the aluminium hydroxide after washing carries out roasting, obtains alumina product after roasting.Gained alumina product impurity chemical composition: Fe
2o
3: 0.01%, SiO
2: 0.02%.
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (8)
1. from activating, in kaolin, extract a method for aluminum oxide, it is characterized in that, said method comprising the steps of:
Step 1: kaolin is carried out to high-temperature activation;
Step 2: ammonium sulfate is mixed and carries out sintering with kaolin after high-temperature activation;
Step 3: gained solid sintered material obtains solution and the residue of sulfur acid aluminium ammonium after stripping;
Step 4: after the solution of sulfur acid aluminium ammonium is filtered, evaporative crystallization or decrease temperature crystalline obtain the exsiccated ammonium alum of solid;
Step 5: solid sulphuric acid aluminium ammonium wiring solution-forming and ammoniacal liquor are reacted, obtain the mixing solutions of aluminium hydroxide and ammonium sulfate;
Step 6: the ammonium sulfate that enters liquid phase is obtained to solid ammonium sulfate through evaporation, continue to recycle;
Step 7: the aluminium hydroxide that step 5 is obtained and the mixing solutions of ammonium sulfate, through filtration washing, obtain the aluminium hydroxide of solid;
Step 8: aluminium hydroxide obtains alumina product after roasting.
2. the method for extracting aluminum oxide from activating in kaolin according to claim 1, is characterized in that, in described step 1, kaolin is carried out to high-temperature activation, and activation temperature is 280-1400 ℃.
3. the method for extracting aluminum oxide from activating in kaolin according to claim 1, it is characterized in that, ratio of components when ammonium sulfate is allocated into and carried out sintering in kaolin after activation in described step 2 with ammonium sulfate/activation afterwards the molecular ratio of Alumina from Kaolin count 2:1-13:1; Sintering temperature is 250-920 ℃, and sintering time is 0.1-6 hours.
4. the method for extracting aluminum oxide from activating in kaolin according to claim 1, it is characterized in that, it in described step 3, is the material after water normal pressure digestion sintering, stripping temperature is 45-98 ℃, after stripping, adopt filtering separation or settlement separate method that solid phase residue is separated, after stripping, solid phase residue washes with water, and washing water are for stripping sintered material.
5. the method for extracting aluminum oxide from activating in kaolin according to claim 1, it is characterized in that, in described step 5, the solid sulphuric acid aluminium ammonium after crystallization is added to water and be made into the solution of counting 4.5g/L-50g/L with alumina concentration, ammonia soln concentration is 2%-30%, and reaction end pH value is controlled between 3-11.
6. the method for extracting aluminum oxide from activating in kaolin according to claim 1, is characterized in that, in described step 7, the method for separated aluminium hydroxide is filtering separation or settlement separate.
7. the method for extracting aluminum oxide from activating in kaolin according to claim 1, is characterized in that, in described step 3, the main component of residue is SiO
2, can be used for producing white carbon black or material of construction.
8. the method that reclaims aluminum oxide from red mud according to claim 1, is characterized in that, described raw material is kaolin, can be also flyash, coal gangue.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105439153A (en) * | 2015-12-22 | 2016-03-30 | 福建龙岩精博化工科技有限公司 | Preparation method of high-dispersibility white carbon black |
| CN109455747A (en) * | 2018-11-28 | 2019-03-12 | 陕西好化工科技有限公司 | A method of aluminium oxide is prepared using methanol-to-olefins dead catalyst and containing phosphatic manure |
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| JP2000256011A (en) * | 1999-03-10 | 2000-09-19 | Taimei Chemicals Co Ltd | Boehmite and its production |
| CN101117229A (en) * | 2007-07-12 | 2008-02-06 | 中国铝业股份有限公司 | Method for extracting aluminium oxide from andalusite ore |
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| CN101117227A (en) * | 2007-07-12 | 2008-02-06 | 中国铝业股份有限公司 | Method for extracting aluminium oxide from clay ore |
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| CN102531013A (en) * | 2010-12-16 | 2012-07-04 | 贵阳铝镁设计研究院有限公司 | Method used for extracting aluminium oxide from low-grade bauxite |
-
2013
- 2013-12-11 CN CN201310689960.9A patent/CN103708514A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1072656A (en) * | 1991-11-26 | 1993-06-02 | 兰州大学 | The production method of aluminium hydroxide |
| JP2000256011A (en) * | 1999-03-10 | 2000-09-19 | Taimei Chemicals Co Ltd | Boehmite and its production |
| CN101117229A (en) * | 2007-07-12 | 2008-02-06 | 中国铝业股份有限公司 | Method for extracting aluminium oxide from andalusite ore |
| CN101117228A (en) * | 2007-07-12 | 2008-02-06 | 中国铝业股份有限公司 | Method for extracting aluminium oxide from coal ash |
| CN101117227A (en) * | 2007-07-12 | 2008-02-06 | 中国铝业股份有限公司 | Method for extracting aluminium oxide from clay ore |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105439153A (en) * | 2015-12-22 | 2016-03-30 | 福建龙岩精博化工科技有限公司 | Preparation method of high-dispersibility white carbon black |
| CN109455747A (en) * | 2018-11-28 | 2019-03-12 | 陕西好化工科技有限公司 | A method of aluminium oxide is prepared using methanol-to-olefins dead catalyst and containing phosphatic manure |
| CN109455747B (en) * | 2018-11-28 | 2021-01-05 | 陕西好一化工科技有限公司 | Method for preparing alumina and phosphorus-containing fertilizer by using methanol-to-olefin waste catalyst |
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Application publication date: 20140409 |