CN110395755A - A method of aluminium oxide is produced using flyash - Google Patents
A method of aluminium oxide is produced using flyash Download PDFInfo
- Publication number
- CN110395755A CN110395755A CN201910835970.6A CN201910835970A CN110395755A CN 110395755 A CN110395755 A CN 110395755A CN 201910835970 A CN201910835970 A CN 201910835970A CN 110395755 A CN110395755 A CN 110395755A
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- CN
- China
- Prior art keywords
- aluminium oxide
- sodium aluminate
- intermediate product
- aluminate solution
- flyash
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/40—Destroying solid waste or transforming solid waste into something useful or harmless involving thermal treatment, e.g. evaporation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/20—Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts
- C01F7/22—Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts with halides or halogen acids
Abstract
The present invention provides a kind of method using flyash production aluminium oxide, includes the following steps: in high temperature to dissolve out aluminous fly-ash with hydrochloric acid, obtained aluminium chloride dissolution fluid is separated with white clay, obtain impure AlCl through pervaporation3.6H2O crystal；By impure AlCl3.6H2O crystal hydrolyzes under water vapour atmosphere, controls hydrolysis temperature at 200 DEG C~850 DEG C, obtains a kind of amorphous substance based on aluminium oxide；Lye is used to dissolve out in atmospheric conditions the amorphous substance of acquisition, leaching temperature is 70 DEG C~100 DEG C, or is dissolved out under an increased pressure using lye, and leaching temperature is 100 DEG C~300 DEG C, is filtered out slag phase, is finally obtained sodium aluminate solution；Sodium aluminate solution is filtered, is diluted, kind of a point decomposition is carried out after cooling, obtains aluminium hydroxide；The method of the invention is effectively reduced by the cost of flyash production aluminium oxide, improves the quality of aluminium oxide, while solid waste being utilized in large quantities, alleviates China's bauxite resource problem in short supply；It is suitble to carry out application in the industrial production.
Description
Technical field
The present invention relates to commercial alumina extractive technique field, specially a kind of new side using flyash production aluminium oxide
Method.
Background technique
With the rapid development of China's aluminum i ndustry, bauxite resource is largely consumed, currently, high-grade bauxite is deficient
Weary, a large amount of middle-low bauxites have been produced use, but the development of China's aluminum i ndustry faces still shortage of resources problem, existing rank
Section import bauxite resource has been over 50%, and the percentage of import is also constantly expanding, and China's aluminum i ndustry has at any time can
" seizing by the throat " problem can be faced.We generate a large amount of flyash solid waste, the processing of these flyash solid wastes every year simultaneously
It is the problem of a urgent need to resolve, therefore using flyash as silicon source, extracts aluminium element therein and produced, can effectively be solved
The certainly above problem has the commercial run of some treated coal ash production aluminium oxide at present, but these methods all have a series of ask
Topic needs to solve, such as: for alkaline process, technology is needed to be improved to realize solid waste decrement treatment；It is acid for acid system
The cost of solution removal of impurities is excessively high, and quality of alumina is difficult to ensure, needs one kind is new to produce using flyash regarding to the issue above
The method of aluminium oxide.
Summary of the invention
Technical assignment of the invention is to be directed to the above the deficiencies in the prior art, and provide a kind of produce using flyash and aoxidize
The method of aluminium, this method use acid and alkali combination method, it can the solid waste for playing acid treatment flyash is reduced advantage, and can send out
The advantage of alkaline process removal of impurities is waved, therefore is all of great significance for the development of China's aluminum i ndustry and the processing of flyash solid waste.
The technical solution adopted by the present invention to solve the technical problems is: a kind of side using flyash production aluminium oxide
Method includes the following steps:
(1) aluminous fly-ash is dissolved out in high temperature with hydrochloric acid, obtained aluminium chloride dissolution fluid is separated with white clay, by steaming
Hair obtains impure AlCl3.6H2O crystal；
(2) by impure AlCl3.6H2O crystal hydrolyzes under water vapour atmosphere, controls hydrolysis temperature 200 DEG C~850
DEG C, intermediate product is obtained, the intermediate product is a kind of amorphous substance based on aluminium oxide；
(3) lye is used to dissolve out in atmospheric conditions the intermediate product obtained in step (2), leaching temperature is 70 DEG C~
100 DEG C, or dissolved out under an increased pressure using lye, leaching temperature is 100 DEG C~300 DEG C, filters out slag phase, obtains sodium aluminate
Solution；
(4) sodium aluminate solution is subjected to kind of a point decomposition and obtains aluminium hydroxide, obtain aluminium oxide after aluminium hydroxide is calcined.
Further, the alumina content in the step (1) in aluminous fly-ash is no less than 40%, and leaching temperature is
150℃。
Further, AlCl in the step (1)3.6H2The impurity element contained in O crystal include: Fe, Ca, Na, K,
Ti, Mg, Cl, miscellaneous by hydrolysis removing chlorine element in step (2), Impurity Fe in step (3), Ca, Mg, Ti are de- with filter residue
It removes.
Further, in the intermediate product obtained in the step (2), Al2O3> 90%, the chlorinity of intermediate product
0.1%~10%.
Further, lye described in the step (3) is sodium hydroxide solution or sodium aluminate solution.
Further, when dissolving out using sodium aluminate solution, the liquid stereoplasm of sodium aluminate solution and intermediate product used is dissolved out
Ratio is measured as 3:1~13:1, in process in leaching, the molecular proportion variation of sodium aluminate solution is 1.65~3.4, and alumina concentration, which changes, is
130g/L~310g/L.
Further, the concentration of sodium hydroxide solution is 200g/L, with Na2O densimeter, sodium hydroxide solution and centre
It is 3:1~13:1 that the liquid of product, which consolidates mass ratio,.
Further, it is all made of universal autoclave in the step (1) and (3) process in leaching, dissolution rate is 85%~
99%.
The present invention provides a kind of aluminium chloride for obtaining hydrochloric acid method dissolution flyash, protect and hydrolyze by Low Temperature Steam,
Aluminium oxide indefinite form product is obtained, by intermediate product under normal pressure or condition of high voltage, using sodium hydroxide (or sodium aluminate) solution
Dissolution obtains sodium aluminate solution, then sodium aluminate solution progress decomposition of crystal seed is obtained aluminium hydroxide, after aluminium hydroxide is calcined
To up-to-standard commercial alumina product, while the method for the invention has energy consumption low, and alumina product quality is high
The characteristics of.
Compared with prior art, the invention has the benefit that
1. obtained liquor alumini chloridi needs to remove except iron, deliming etc. in the technique of existing hydrochloric acid method production aluminium oxide
The process flow of decontamination, removal of impurities process is complicated, at high cost, unstable product quality；Present invention eliminates acid system impurity removal process,
Considerably reduce cost；The present invention is stripped of part Cl element impurity in hydrolytic process, Fe, Ca, Mg in alkali soluble step,
Ti can be removed with filter residue；
Existing acid and alkali combination method technique aluminium sulphate production aluminium oxide, then the technique gone out with alkali soluble, or use chlorination
Aluminium pyrohydrolysis (hydrolysis temperature is higher than 900 DEG C) obtains aluminium oxide, then the technique gone out with alkali soluble, the two techniques are gone out using alkali soluble
Material be all alumina primary product that high-temperature roasting obtains, be all the aluminium oxide crystallized, so the needs when alkali soluble goes out
Very high temperature, consumption energy are high；
The method of the invention uses low temperature hydrolysis to obtain intermediate amorphous state intermediate product first, just saves a large amount of energy
Then amount uses normal pressure alkali soluble technique, and energy is greatly saved, therefore the method for the invention process is simple, energy disappears
Consume low, good product quality.
2. the method for the invention effectively reduces by the cost of flyash production aluminium oxide, improves the matter of aluminium oxide
Amount, while solid waste being utilized in large quantities, China's bauxite resource problem in short supply is alleviated, is suitble to be answered in the industrial production
With popularization；Simultaneously the present invention is based on the purpose of flyash production aluminium oxide, low temperature hydrolysis aluminium chloride is successfully developed, in normal pressure
Alkali soluble goes out to prepare the technology of sodium aluminate, to solve flyash fixed-end forces, expands China's aluminum i ndustry resource scarcity problem and makes
Contribution.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that described herein, specific examples are only used to explain the present invention, is not used to limit
The fixed present invention.
The present invention provides a kind of method using flyash production aluminium oxide, includes the following steps:
(1) aluminous fly-ash is dissolved out at 150 DEG C with hydrochloric acid in general autoclave, by obtained aluminium chloride dissolution fluid with
White clay separation, obtains impure AlCl through pervaporation3.6H2O crystal；
(2) by impure AlCl3.6H2O crystal hydrolyzes under water vapour atmosphere, is hydrolyzed using universal autoclave
Reaction, for control hydrolysis temperature at 200 DEG C~850 DEG C, 0.1~2.5Mpa of pressure, it is 10~200L/min that vapor, which is passed through rate,
(in terms of 25 DEG C of mark pressures of room temperature), and the chlorine-containing gas of generation is exported into autoclave, amorphous state intermediate product is obtained, intermediate product is
Al2O3> 90%, chlorinity 0.1%~10%；
(3) lye is used to dissolve out in atmospheric conditions the intermediate product obtained in step (2), leaching temperature is 70 DEG C~
100 DEG C, or dissolved out under an increased pressure using lye, leaching temperature is 100 DEG C~300 DEG C, filters out slag phase, obtains sodium aluminate
Solution；Lye is sodium hydroxide solution or sodium aluminate solution, when dissolving out using sodium aluminate solution, dissolves out sodium aluminate solution used
It is 3:1~13:1 that the liquid of liquid and intermediate product, which consolidates mass ratio, in process in leaching, the molecular proportion variation of sodium aluminate solution for 1.65~
3.4, alumina concentration variation is 130g/L~310g/L；When being dissolved out using sodium hydroxide solution, concentration of sodium hydroxide solution is
200g/L, with Na2It is 3:1~13:1 that the liquid of O densimeter, sodium hydroxide solution and intermediate product, which consolidates mass ratio,；
(4) current Bayer process production technology is combined, kind point point is carried out by obtained sodium aluminate solution through diluting, after cooling
Solution, obtains aluminium hydroxide, after then calcining aluminium hydroxide, obtains commercial alumina.
The flyash sample extracted in the embodiment of the present invention comes from certain electricity power enterprise's aluminous fly-ash, fine coal ash component are as follows:
SiO2- 40.10%, TiO2- 1.57%, Al2O3- 50.71%, Fe2O3- 1.76%, MnO-0.02%, MgO-0.47%, CaO-
2.85%, Na2O-0.12%, K2O-0.50%, P2O5- 0.17%, SO3- 0.22%, igloss 1.14%, the above ingredient is with oxygen
Compound form mark, % representation quality percentage, similarly hereinafter.
Flyash is dissolved out in autoclave with hydrochloric acid in step (1), liquor alumini chloridi is obtained after filtering, is obtained after evaporation
AlCl3.6H2O crystal, the aluminium chloride crystalline component are as follows: SiO2- 2.10%, TiO2- 0.026%, Fe2O3- 0.243%, MgO-
0.210%, CaO-0.01%, Na2O-0.350%, K2O-0.150%, P2O5- 0.250%, SO3- 0.260%, remaining is
AlCl3·6H2O。
Embodiment 1
Take above-mentioned AlCl3.6H2It 1 kilogram of O crystal, hydrolyzes 2 hours for 300 DEG C, obtains salic under steam atmosphere
205.0 grams of intermediate product, chlorinity 9.7%；Intermediate product 615g sodium aluminate solution is dissolved out, sodium aluminate solution used
In: Al2O3130g/L, (the causticity Na in sodium aluminate solution of molecular proportion 3.402O and Al2O3Molar ratio be known as sodium aluminate solution
Molecular proportion, similarly hereinafter), 90 DEG C of leaching temperature, sodium aluminate solution is obtained, in sodium aluminate solution obtained: Al2O3267g/L, molecule
Than 1.65, filter residue 10g is obtained after filtering, is decomposed using kind point and is obtained 306 grams of aluminium hydroxide, calcining obtains Al2O3200 grams.
Embodiment 2
Take above-mentioned AlCl3.6H2It 2 kilograms of O crystal, hydrolyzes 3 hours for 400 DEG C, obtains salic under steam atmosphere
408 grams of intermediate product, chlorinity 6.2%；Intermediate product 3260g sodium aluminate solution is dissolved out, in sodium aluminate solution used:
Al2O3135g/L, molecular proportion 3.40, obtain sodium aluminate solution by 80 DEG C of leaching temperature, in sodium aluminate solution obtained:
Al2O3278g/L, molecular proportion 1.65 obtain filter residue 18g after filtering, decomposed using kind point and obtain 613 grams of aluminium hydroxide, calcined
To Al2O3401 grams.
Embodiment 3
Take above-mentioned AlCl3.6H2It 5 kilograms of O crystal, hydrolyzes 3 hours for 600 DEG C, obtains salic under steam atmosphere
1020 grams of intermediate product, chlorinity 1.5%；Intermediate product 13250g sodium aluminate solution is dissolved out, sodium aluminate solution used
In: Al2O3140g/L, molecular proportion 3.40, obtain sodium aluminate solution by 150 DEG C of leaching temperature, in sodium aluminate solution obtained:
Al2O3288g/L, molecular proportion 1.65 obtain filter residue 45g after filtering, decomposed using kind point and obtain 1545 grams of aluminium hydroxide, calcined
To Al2O31010 grams.
Embodiment 4
Take above-mentioned AlCl3.6H2It 5 kilograms of O crystal, hydrolyzes 2 hours for 800 DEG C, obtains salic under steam atmosphere
1020 grams of intermediate product, chlorinity 0.3%.Intermediate product 3060g sodium aluminate solution is dissolved out, sodium aluminate solution used
In: Al2O3145g/L, molecular proportion 3.40, obtain sodium aluminate solution by 220 DEG C of leaching temperature, in sodium aluminate solution obtained:
Al2O3299g/L, molecular proportion 1.65 obtain filter residue 46g after filtering, decomposed using kind point and obtain 1548 grams of aluminium hydroxide, calcined
To Al2O31012 grams.
Embodiment 5
Take above-mentioned AlCl3.6H2It 2 kilograms of O crystal, hydrolyzes 2 hours for 850 DEG C, obtains salic under steam atmosphere
408 grams of intermediate product, chlorinity 0.2% dissolves out intermediate product 3270g sodium aluminate solution, in sodium aluminate solution used:
Al2O3150g/L, molecular proportion 3.40, obtain sodium aluminate solution by 300 DEG C of leaching temperature, in sodium aluminate solution obtained:
Al2O3309g/L, molecular proportion 1.65 obtain filter residue 22g after filtering, decomposed using kind point and obtain 614 grams of aluminium hydroxide, calcined
To Al2O3402 grams.
Embodiment 6
Take above-mentioned AlCl3.6H2It 1 kilogram of O crystal, hydrolyzes 2 hours for 300 DEG C, obtains salic under steam atmosphere
205.0 grams of intermediate product, chlorinity 9.7%.Intermediate product 2660g sodium hydroxide solution is dissolved out, sodium hydroxide used
Solution: Na2O 200g/L, (concentration conversion of sodium hydroxide solution is with Na2O densimeter), 90 DEG C of leaching temperature, obtain aluminic acid
Sodium solution, in sodium aluminate solution obtained: Al2O3268g/L, molecular proportion 1.23 obtain filter residue 9g after filtering, using kind point point
Solution obtains 308 grams of aluminium hydroxide, and calcining obtains Al2O3201 grams.
Above technical scheme elaborates technical thought of the invention, and this does not limit the scope of protection of the present invention, all
Without departing from the content of technical solution of the present invention, according to the technical essence of the invention to made by above technical scheme it is any change and
Modification, belongs to the protection scope of technical solution of the present invention.
Claims (8)
1. a kind of method using flyash production aluminium oxide, which comprises the steps of:
(1) aluminous fly-ash is dissolved out in high temperature with hydrochloric acid, obtained aluminium chloride dissolution fluid is separated with white clay, is obtained through pervaporation
To impure AlCl3.6H2O crystal；
(2) by impure AlCl3.6H2O crystal hydrolyzes under water vapour atmosphere, control hydrolysis temperature at 200 DEG C~850 DEG C,
Intermediate product is obtained, the intermediate product is a kind of amorphous substance based on aluminium oxide；
(3) lye is used to dissolve out in atmospheric conditions the intermediate product obtained in step (2), leaching temperature is 70 DEG C~100
DEG C, or dissolved out under an increased pressure using lye, leaching temperature is 100 DEG C~300 DEG C, filters out slag phase, obtains sodium aluminate solution
Liquid；
(4) sodium aluminate solution is subjected to kind of a point decomposition and obtains aluminium hydroxide, obtain aluminium oxide after aluminium hydroxide is calcined.
2. a kind of method using flyash production aluminium oxide according to claim 1, which is characterized in that the step
(1) alumina content in aluminous fly-ash is no less than 40%, and leaching temperature is 150 DEG C.
3. a kind of method using flyash production aluminium oxide according to claim 1, which is characterized in that the step
(2) in the intermediate product obtained in, Al2O3> 90%, the chlorinity 0.1%~10% of intermediate product.
4. a kind of method using flyash production aluminium oxide according to claim 1, which is characterized in that in step (3)
The lye is sodium hydroxide solution or sodium aluminate solution.
5. a kind of method using flyash production aluminium oxide according to claim 4, which is characterized in that use sodium aluminate
When solution dissolves out, the liquid for dissolving out used sodium aluminate solution and intermediate product consolidate mass ratio as 3:1~13:1, in process in leaching,
The molecular proportion variation of sodium aluminate solution is 1.65~3.4, and alumina concentration variation is 130g/L~310g/L.
6. a kind of method using flyash production aluminium oxide according to claim 4, which is characterized in that the hydroxide
Sodium solution concentration is 200g/L (with Na2O densimeter), it is 3:1~13 that the liquid of sodium hydroxide solution and intermediate product, which consolidates mass ratio:
1。
7. a kind of method using flyash production aluminium oxide according to claim 1, which is characterized in that the step
(1) and in (3) process in leaching it is all made of universal autoclave, dissolution rate is 85%~99%.
8. a kind of method using flyash production aluminium oxide according to claim 1, which is characterized in that the step
(1) AlCl in3.6H2The impurity element contained in O crystal includes: Fe, Ca, Na, K, Ti, Mg, Cl, and step passes through hydrolysis in (2)
Removing chlorine element is miscellaneous, Impurity Fe in step (3), Ca, Mg, and Ti is removed with filter residue.
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| CN110963515A (en) * | 2019-12-27 | 2020-04-07 | 眉山顺应动力电池材料有限公司 | Method for recovering alumina from fly ash |
| CN111204784A (en) * | 2020-01-20 | 2020-05-29 | 东北大学 | Method and device for deep hydrolysis and dechlorination of crystalline aluminum chloride |
| CN111792660A (en) * | 2020-07-15 | 2020-10-20 | 东北大学 | Method for producing boehmite micro-nano powder by using aluminum chloride |
| CN112850762A (en) * | 2021-02-09 | 2021-05-28 | 东北大学 | Method for preparing aluminum oxide by aluminum ash pellets through chlorination-oxygen pressure conversion and utilizing all components |
| CN113292088A (en) * | 2021-05-19 | 2021-08-24 | 神华准能资源综合开发有限公司 | Method for producing low-magnesium and low-calcium alumina from crystalline aluminum chloride |
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| CN111792660A (en) * | 2020-07-15 | 2020-10-20 | 东北大学 | Method for producing boehmite micro-nano powder by using aluminum chloride |
| CN112850762A (en) * | 2021-02-09 | 2021-05-28 | 东北大学 | Method for preparing aluminum oxide by aluminum ash pellets through chlorination-oxygen pressure conversion and utilizing all components |
| CN113292088A (en) * | 2021-05-19 | 2021-08-24 | 神华准能资源综合开发有限公司 | Method for producing low-magnesium and low-calcium alumina from crystalline aluminum chloride |
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Application publication date: 20191101 |