CN101214983A - Method for preparing aluminum oxide from oil shale clinker - Google Patents
Method for preparing aluminum oxide from oil shale clinker Download PDFInfo
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- CN101214983A CN101214983A CNA2008100502017A CN200810050201A CN101214983A CN 101214983 A CN101214983 A CN 101214983A CN A2008100502017 A CNA2008100502017 A CN A2008100502017A CN 200810050201 A CN200810050201 A CN 200810050201A CN 101214983 A CN101214983 A CN 101214983A
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Abstract
The invention relates to a process for preparing aluminum oxide, in particular to a method for extracting aluminum oxide from discarded oil shale ash as raw material. The oil shale ash is disintegrated into fine powder less than 150 eye to be calcined at a certain temperature, then sulfuric acid solution is added for performing acid dipping, after solid-liquid separation and solid residue removal, aluminum sulfate solution is obtained and is then filtered after sodium hydroxide solution is added in, further metallic ions as Ca2+, Mg2+, Fe3+, Fe2+ and the like are filtered from the solution, thereby sodium aluminate solution is obtained, gas of carbon dioxide is communicated into the sodium aluminate solution to obtain aluminum hydroxide sediment, and after drying and calcining aluminum hydroxide powder is obtained. Compared with the prior art, the raw material is easy to obtain and not only industrial pollution of the ash is eliminated, but also nonferrous metal in the ash can be recycled, limited resources are enabled to be comprehensively utilized, performance index of the prepared aluminum oxide is good, the pureness reaches 98.5%, extraction rate reaches 75%, and the process is simple in technique, low in production cost and suitable in industrial production.
Description
Technical field:
The present invention relates to a kind of preparation method of aluminum oxide, especially extract method of alumina as raw material with depleted resinous shale lime-ash.
Background technology:
Industrial now develops rapidly, and resource problem is one of significant problem of current society.At present, the production of aluminum oxide mainly depends on bauxite.The occurring in nature aluminum-containing mineral has multiple, mainly is bauxite as the raw material of producing aluminum oxide.Producing aluminum oxide with bauxite or other aluminum-containing raw material, is exactly in fact aluminum oxide and other impurity separating process that makes in the ore.The production method of alumina has alkaline process, acid system, electric heating process.Along with the increase of aluminium consumption, the ore extraction amount increases, and bauxite resource reduces year by year, and ore aluminium grade constantly descends, and cost of winning improves constantly, and the utilization of studying high silicon low-grade bauxite or other high silicon aluminum-containing mineral raw materials becomes trend gradually.
China is the abundant countries of oil shale resources, occupies the 4th in the world.Mainly be distributed in 15 provinces district, concentrate on northeast and ALFISOL IN CENTRAL, find out resource reserve 329.89 hundred million t.The development and use of resinous shale have obtained attention both domestic and external, have now 69% resinous shale to be used to burn in the world and generate heat, generate electricity, and 25% resinous shale refines shale oil through various destructive distillation producers, have only 6% resinous shale to be used for aspects such as building, agricultural.
Reach domestic oil shale lime-ash abroad, generally be used for preparing concrete or other material of construction, do not appear in the newspapers and utilize oil shale residues to extract aluminium.A kind of attached waste material that kerosene shale ash slag system resinous shale is produced in the oily process of industry system, its essential mineral composition is a sheet kaolinite, secondly is organic matters such as carbon.The stacking of resinous shale lime-ash, contaminate environment again when taking up an area of.With Fushun shale is example, and after the oil shale distillation, residue accounts for about 80%～90%, and its main chemical constitution is: SiO
2, Al
2O
3, Fe
2O
3, MgO, CaO.Content is respectively 57.8%, 17.84%, and 8.62%, 1.09%, 0.7%.Obviously, from the resinous shale lime-ash, extract aluminium, both eliminated cindery industrial pollution by chemical process, reclaimed the non-ferrous metal in the lime-ash again, limited resources effectively being utilized, met reduction of discharging synergic circular economy concept, is the good method of killing two birds with one stone.
Summary of the invention:
Purpose of the present invention is exactly at above-mentioned the deficiencies in the prior art, and a kind of method with preparing aluminum oxide from oil shale clinker is provided.
The objective of the invention is to realize in the following manner:
With the method for preparing aluminum oxide from oil shale clinker, comprise following order and step:
A, the kerosene shale ash ground-slag is broken to＜150 purpose fine powders, at a certain temperature calcining;
B, the resinous shale lime-ash after will calcining mix with the ratio heating of sulphuric acid soln according to solid-liquid 1: 2～5, aluminum sulfate aqueous solution, mixing afterwards, the vitriolic massfraction is 20～30%;
C, with said mixture through solid-liquid separation, remove solid residue, must contain Ca
2+, Mg
2+, Fe
3+, Fe
2+Tai-Ace S 150 filtrate Deng metal ion;
D, with step c gained Tai-Ace S 150 filtrate, in filtrate, add massfraction and be 10%～30% sodium hydroxide solution after-filtration, the Ca in the filtering solution
2+, Mg
2+, Fe
3+, Fe
2+Deng metal ion, get sodium aluminate solution;
E, in sodium aluminate solution, feed carbon dioxide, obtain aluminum hydroxide precipitation;
F, step e gained aluminum hydroxide precipitation oven dry, calcining are obtained aluminium-hydroxide powder.
Purpose of the present invention can also realize in the following manner:
Calcining among the step a, its calcining temperature are at 600～750 ℃, and calcination time is 3～4hr; Heating temperature described in the step b is 80～105 ℃, and the reaction times is 2～5hr; The shared total liquid quality fraction of the described sodium hydroxide of step c is 20～40%, and the pH value of neutralization back solution is greater than 13; The described feeding carbon dioxide of steps d, feeding speed is 5～60mL/min, the pH value of neutralization back solution is 8～9; The described calcining of step f, its temperature are 600～1000 ℃.
Beneficial effect: compared with the prior art, raw material is cheap and easy to get, both eliminated cindery industrial pollution, reclaimed the non-ferrous metal in the lime-ash again, and made limited resources obtain comprehensive utilization, the good performance indexes of the aluminum oxide of preparation, purity reaches 98.5%, extraction rate reached 75%, and technology is simple, production cost is low, is fit to suitability for industrialized production.
Description of drawings
Accompanying drawing is: with the method process flow sheet of preparing aluminum oxide from oil shale clinker
Embodiment
The present invention is described in further detail below in conjunction with embodiment:
With the method for preparing aluminum oxide from oil shale clinker, comprise following order and step:
A, the kerosene shale ash ground-slag is broken to＜150 purpose fine powders, at a certain temperature calcining;
B, the resinous shale lime-ash after will calcining mix with the ratio heating of sulphuric acid soln according to solid-liquid 1: 2～5, aluminum sulfate aqueous solution, mixing afterwards, the vitriolic massfraction is 20～30%;
C, with said mixture through solid-liquid separation, remove solid residue, must contain Ca
2+, Mg
2+, Fe
3+, Fe
2+Tai-Ace S 150 filtrate Deng metal ion;
D, with step c gained Tai-Ace S 150 filtrate, in filtrate, add massfraction and be 10%～30% sodium hydroxide solution after-filtration, the Ca in the filtering alum liquor
2+, Mg
2+, Fe
3+, Fe
2+Deng metal ion, get sodium aluminate solution;
E, in sodium aluminate solution, feed carbon dioxide, obtain aluminum hydroxide precipitation;
F, step e gained aluminum hydroxide precipitation oven dry, calcining are obtained aluminium-hydroxide powder.
Purpose of the present invention can also realize in the following manner:
Calcining among the step a, its calcining temperature are at 600～750 ℃, and calcination time is 3～4hr; Heating temperature described in the step b is 80～105 ℃, and the reaction times is 2～5hr; PH 〉=13 of in the described sodium hydroxide of step c and back solution; The described feeding carbon dioxide of steps d, feeding speed is 5～60mL/min, the pH value of neutralization back solution is 8～9; The described calcining of step f, its temperature are 600～1000 ℃.
Embodiment one:
Take by weighing 100g resinous shale lime-ash,, add 500g30%H at 600 ℃ of calcining 2h
2SO
4Solution (98% vitriol oil 83ml, water 347ml), heating while stirring is heated to 95 ℃ of reaction 5h, stops to stir, and treats that solution is cooled to 70 ℃ of after-filtration, removes residue through solid-liquid separation, adds 20%NaOH solution 74g (NaOH14.8g, H in filtrate
2O59.2ml), neutralization back pH value of solution 〉=13, after filtration, the Ca in the filtering solution
2+, Mg
2+, Fe
3+, Fe
2+Deng metal ion, get sodium aluminate solution (NaAlO
2), from the bottom to sodium metaaluminate (NaAlO
2) filtrate feeding CO
2Gas, the speed that feeds gas is 10ml/min, the pH value of solution is 9, gets Al (OH)
3Precipitation is with Al (OH)
3The precipitation oven dry obtains Al 700 ℃ of calcinings
2O
3Extraction yield is 74.90%, and purity is 98.20%.
Embodiment two:
Take by weighing 100g resinous shale lime-ash, at 650 ℃ of calcining 2h, add 400g30%H2SO4 solution (98% vitriol oil 67ml, water 278ml), heating while stirring, be heated to 90 ℃ of reaction 5h, stop to stir, treat that solution is cooled to 70 ℃ of after-filtration, remove residue through solid-liquid separation, in filtrate, add 20%NaOH solution 75g (NaOH15g, H
2O60ml), neutralization back pH value of solution 〉=13, after filtration, the Ca in the filtering solution
2+, Mg
2+, Fe
3+, Fe
2+Deng metal ion, get sodium aluminate solution (NaAlO
2), from the bottom to sodium aluminate solution (NaAlO
2) feeding CO
2Gas, the feeding gas velocity is 20ml/min, the pH value of solution is 9, gets Al (OH)
3Precipitation is with Al (OH)
3The precipitation oven dry, 800 ℃ of calcinings obtain Al
2O
3Extraction yield is 72.54%, and purity is 98.17%.
Embodiment three:
Take by weighing 100g resinous shale lime-ash,, add 400g20%H at 650 ℃ of calcining 3h
2SO
4Solution (98% vitriol oil 44ml, water 318ml), heating while stirring is heated to 95 ℃ of reaction 5h, stops to stir, and treats that solution is cooled to 70 ℃ of after-filtration, removes residue through solid-liquid separation, adds 20%NaOH solution 74g (NaOH14.8g, H in filtrate
2O59.2ml).Neutralization back pH value of solution 〉=13, after filtration, the Ca in the filtering solution
2+, Mg
2+, Fe
3+, Fe
2+Deng metal ion, get sodium aluminate solution (NaAlO
2), from the bottom to sodium aluminate solution (NaAlO
2) feeding CO
2Gas, the feeding gas velocity is 30ml/min, the pH value of solution is 8.Get Al (OH)
3Precipitation is with Al (OH)
3The precipitation oven dry, 700 ℃ of calcinings obtain Al
2O
3Extraction yield is 63.58%, and purity is 98.22%.
Embodiment four:
Take by weighing 100g resinous shale lime-ash,, add 300g40%H at 700 ℃ of calcining 3h
2SO
4Solution (98% vitriol oil 67ml, water 178ml), heating while stirring is heated to 90 ℃ of reaction 3h, stops to stir, and treats that solution is cooled to 70 ℃ of after-filtration, removes residue through solid-liquid separation, adds 20%NaOH solution 75g (NaOH15g, H in filtrate
2O60ml).Neutralization back pH value of solution 〉=13, after filtration, the Ca in the filtering solution
2+, Mg
2+, Fe
3+, Fe
2+Deng metal ion, get sodium aluminate solution (NaAlO
2), from the bottom to sodium aluminate solution (NaAlO
2) feeding CO
2Gas, the feeding gas velocity is 20ml/min, the pH value of solution is 8.Get Al (OH)
3Precipitation is with Al (OH)
3The precipitation oven dry, 700 ℃ of calcinings obtain Al
2O
3Extraction yield is 69.65%, and purity is 98.30%.
Claims (6)
1. method with preparing aluminum oxide from oil shale clinker is characterized in that comprising following order and step:
A, the kerosene shale ash ground-slag is broken to＜150 purpose fine powders, at a certain temperature calcining;
B, the resinous shale lime-ash after will calcining mix with the ratio heating of sulphuric acid soln according to solid-liquid 1: 2～5, aluminum sulfate aqueous solution, mixing afterwards, the vitriolic massfraction is 20～30%;
C, with said mixture through solid-liquid separation, remove solid residue, must contain Ca
2+, Mg
2+, Fe
3+, Fe
2+Tai-Ace S 150 filtrate Deng metal ion;
D, with step c gained Tai-Ace S 150 filtrate, in filtrate, add massfraction and be 10%～30% sodium hydroxide solution after-filtration, the Ca in the filtering solution
2+, Mg
2+, Fe
3+, Fe
2+Deng metal ion, get sodium aluminate solution;
E, in sodium aluminate solution, feed carbon dioxide, obtain aluminum hydroxide precipitation;
F, step e gained aluminum hydroxide precipitation oven dry, calcining are obtained aluminium-hydroxide powder.
2. according to the described method of claim 1, it is characterized in that with preparing aluminum oxide from oil shale clinker, the calcining among the step a, its calcining temperature is at 600～750 ℃, and calcination time is 3～4hr.
3. according to the described method with preparing aluminum oxide from oil shale clinker of claim 1, it is characterized in that the Heating temperature described in the step b is 80～105 ℃, the reaction times is 2～5hr.
4. according to the described method of claim 1, it is characterized in that pH value 〉=13 of in the described sodium hydroxide of step c and back solution with preparing aluminum oxide from oil shale clinker.
5. according to the described method of claim 1, it is characterized in that with preparing aluminum oxide from oil shale clinker, the described feeding carbon dioxide of steps d, feeding speed is 5～60mL/min, the pH value of neutralization back solution is 8～9.
6. according to the described method of claim 1, it is characterized in that with preparing aluminum oxide from oil shale clinker, the described calcining of step f, its temperature is 600～1000 ℃.
Priority Applications (1)
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|---|---|---|---|
| CNA2008100502017A CN101214983A (en) | 2008-01-02 | 2008-01-02 | Method for preparing aluminum oxide from oil shale clinker |
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|---|---|---|---|
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102000446A (en) * | 2010-10-22 | 2011-04-06 | 上海福贝宠物用品有限公司 | Preparation technique of pancake rock stock solution |
| CN101723397B (en) * | 2009-11-27 | 2011-04-06 | 抚顺矿业集团有限责任公司 | Method for preparing zeolite molecular sieve by using oil shale residues |
| CN103539183A (en) * | 2013-10-29 | 2014-01-29 | 广东石油化工学院 | Acid method for preparing aluminum polychlorid and high-purity nanoscale white carbon black through ash of oil shale |
| CN106762136A (en) * | 2017-02-09 | 2017-05-31 | 上海博历机械科技有限公司 | A kind of automobile engine hot junction heat shield |
| CN106839458A (en) * | 2017-02-09 | 2017-06-13 | 上海源紊新能源科技有限公司 | A kind of solar thermal collector of high efficient antifreeze insulation |
| CN106938866A (en) * | 2017-05-03 | 2017-07-11 | 福建龙净环保股份有限公司 | A kind of desulfurization wastewater resource utilization system and method |
| CN109455748A (en) * | 2018-12-17 | 2019-03-12 | 北京建工金源环保发展股份有限公司 | A method of recycling aluminum nitrate from waste acid liquor |
| CN112358895A (en) * | 2020-11-07 | 2021-02-12 | 新能能源有限公司 | Ash treatment system and method for high-silicon high-aluminum coal catalytic gasification process |
| CN114163012A (en) * | 2021-09-23 | 2022-03-11 | 中交路桥南方工程有限公司 | Method for treating sulfate in wastewater |
-
2008
- 2008-01-02 CN CNA2008100502017A patent/CN101214983A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101723397B (en) * | 2009-11-27 | 2011-04-06 | 抚顺矿业集团有限责任公司 | Method for preparing zeolite molecular sieve by using oil shale residues |
| CN102000446A (en) * | 2010-10-22 | 2011-04-06 | 上海福贝宠物用品有限公司 | Preparation technique of pancake rock stock solution |
| CN102000446B (en) * | 2010-10-22 | 2012-09-19 | 上海福贝宠物用品有限公司 | Preparation technique of pancake rock stock solution |
| CN103539183A (en) * | 2013-10-29 | 2014-01-29 | 广东石油化工学院 | Acid method for preparing aluminum polychlorid and high-purity nanoscale white carbon black through ash of oil shale |
| CN106762136A (en) * | 2017-02-09 | 2017-05-31 | 上海博历机械科技有限公司 | A kind of automobile engine hot junction heat shield |
| CN106839458A (en) * | 2017-02-09 | 2017-06-13 | 上海源紊新能源科技有限公司 | A kind of solar thermal collector of high efficient antifreeze insulation |
| CN106938866A (en) * | 2017-05-03 | 2017-07-11 | 福建龙净环保股份有限公司 | A kind of desulfurization wastewater resource utilization system and method |
| CN109455748A (en) * | 2018-12-17 | 2019-03-12 | 北京建工金源环保发展股份有限公司 | A method of recycling aluminum nitrate from waste acid liquor |
| CN112358895A (en) * | 2020-11-07 | 2021-02-12 | 新能能源有限公司 | Ash treatment system and method for high-silicon high-aluminum coal catalytic gasification process |
| CN114163012A (en) * | 2021-09-23 | 2022-03-11 | 中交路桥南方工程有限公司 | Method for treating sulfate in wastewater |
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Open date: 20080709 |