CN1240617C - Normal pressure low temperature leaching production method for alumina - Google Patents
Normal pressure low temperature leaching production method for alumina Download PDFInfo
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- CN1240617C CN1240617C CN 03148717 CN03148717A CN1240617C CN 1240617 C CN1240617 C CN 1240617C CN 03148717 CN03148717 CN 03148717 CN 03148717 A CN03148717 A CN 03148717A CN 1240617 C CN1240617 C CN 1240617C
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- aluminum oxide
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Abstract
The present invention relates to an alumina production method through dissolution at a normal pressure and a low temperature. The method comprises the steps that (1) a leaching reaction is carried out by bauxite in an alkali solution, and the alkali solution containing sodium aluminate and slag are obtained through filtration; (2) the alkali solution containing sodium aluminate, which is obtained in the step (1), is concentrated, cooled, crystallized and filtered so as to obtain coarse crystals of hydrating sodium aluminate and filtering mother liquor thereof; (3) the coarse crystals of hydrating sodium aluminate, which are obtained in the step (2), are dissolved in water or thin alkali liquor, and aluminium hydroxide is obtained through the operation of desiliconization and seed precipitation; the obtained aluminium hydroxide is calcinated to prepare alumina. The method also comprises that multi-stage counter current washing is carried out by water on the slag obtained in the step (1), and washing liquor is used for dissolving the thin alkali liquor of the coarse crystals of hydrating sodium aluminate in the step (3); the filtering mother liquor obtained in the step (2) is used for the leaching reaction of the bauxite in the step (1). The alkali liquor is a water solution of NaOH or KOH. The method has low dissolution temperature and low dissolution pressure, and the actual dissolution rate of alumina is more than 90%.
Description
Technical field
The present invention relates to the field of production of aluminum oxide, particularly a kind of atmospheric low-temperature stripping production method of aluminum oxide of the diaspore type bauxite of handling indissoluble.
Background technology
The production of existing aluminum oxide all is to adopt alkali process, mainly contains Bayer process, sintering process and integrated process thereof.Sintering process mainly is to handle the low bauxite of alumina silica ratio, and when handling the high bauxite of alumina silica ratio, its benefit will be much smaller than Bayer process.Bayer process mainly is to adopt the NaOH aqueous solution stripping bauxite of 200-300g/L directly to dilute the technology that desiliconization kind branch obtains aluminium hydroxide then.But be used to handle when accounting for the diaspore type bauxite of China's bauxite resource more than 98%, need high temperature (235-280 ℃) high pressure (3.5-6.0MP) operation, see " the Bayer process stripping of bauxite " of Bi Shiwen work.Because the High Temperature High Pressure operation has increased the energy consumption of facility investment and process, also increased certain degree of difficulty for production operation, manufacturing cost of aluminum oxide is significantly improved.Same because temperature (260-280 ℃) and pressure (more than the 5.0MP) are too high for the high pressure water chemical method that the bauxite of handling low alumina silica ratio is developed, production process is difficult to realize; The dissolution fluid that obtains simultaneously is subjected to the restriction of phase balance condition, and aluminum concentration is too low, so far existing over half a century, industrialized report is not arranged yet, sees " process for making alumina " of the stupid work of Yang Chong.
The research work of existing reinforcement diaspore type bauxite stripping mainly is to carry out under with the condition of sig water, and the ie in solution system remains in the concentration of lye scope of traditional Bayer process and reaches the purpose that improves the aluminum oxide result of extraction by reinforcing mass transfer and raising stripping temperature.But be subjected to the restriction of strength of solution, improve temperature and must cause working pressure to raise, facility investment and operation easier sharply increase.
Summary of the invention
The objective of the invention is to overcome when handling diaspore type bauxite the facility investment height of must the High Temperature High Pressure operation and causing with Bayer process, the defective of the big and operational difficulty of energy consumption, propose a kind of alumina producing novel method, and improve the solubility rate of aluminum oxide with low-temperature atmosphere-pressure stripping diaspore type bauxite of industrial operation.
The method of the present invention alkali lye stripping bauxite of high density, then the dissolution fluid crystallization is obtained aluminate hydrates sodium coarse-grain, again with its dissolving dissolving, desiliconization, kind is divided and calcining makes method of alumina, if therefore avoided dissolution fluid is diluted directly that water evaporation quantity that desiliconization kind branch will cause increases greatly and the energy consumption that improved alumina producing.The main reaction of diaspore type bauxite stripping is:
Technical scheme of the present invention is as follows:
The atmospheric low-temperature stripping production method of aluminum oxide provided by the invention comprises the steps:
1) be to leach reaction in the 50%-70% alkaline solution with bauxite in weight percent concentration, the weight part proportioning of described bauxite and alkaline solution is 1: 1-2: 1, it leaches temperature of reaction is 150-200 ℃, leaching the reaction times is 0.5-10 hour, adding water or sig water, alkaline solution is diluted to weight percent concentration is 40%-50%, under 40-150 ℃ condition, filter the alkaline solution and the slag that obtain containing sodium aluminate;
2) after the alkaline solution that contains sodium aluminate that step 1) is obtained is concentrated into the weight percent concentration that makes alkaline solution and is 40-60%, be cooled to 50-110 ℃ and carry out crystallization, filter and obtain aluminate hydrates sodium coarse-grain and filtrated stock thereof;
3) the aluminate hydrates sodium coarse-grain water that obtains of step (2) or sig water dissolving, then through desiliconization, plant and divide operation to obtain aluminium hydroxide, again with the aluminium hydroxide that obtains through calcining, just make aluminum oxide;
This stripping production method comprises that also the slag water with step 1) carries out the multi-stage countercurrent washing, countercurrent washing progression is the 3-5 level, wash temperature is 50-90 ℃, its washings be used in the dilution of step 1) alkali lye or the step 3) to the macrocrystalline sig water dissolving of aluminate hydrates sodium;
This stripping production method also comprises step 2) filtrated stock be directly used in the leaching reaction of the bauxite of step 1);
Described alkaline solution is the NaOH aqueous solution;
The leaching pressure of described leaching reaction is that 0-0.55Mpa is good;
The extraction time of described leaching reaction be 0.5-3 hour for good.
The atmospheric low-temperature stripping production method of aluminum oxide provided by the invention is compared with having industrialization technology-Bayer process, sintering process or integrated process both at home and abroad now, has following obvious superiority:
(1) extraction temperature of the present invention is 150-200 ℃, about 60-100 ℃ of more traditional Bayer process decline, make leaching process in, low pressure heating, capable of reducing energy consumption more than 5%, and the rate of recovery that improves aluminium is more than 3%;
(2) leaching pressure of the present invention is 0-0.55MP, has overcome that the facility investment that high pressure leaches under the 3.5-6.0MP of traditional Bayer process is big, life cycle short, the shortcoming of operational difficulty, has reduced facility investment significantly, and has made operating process be easy to carry out;
(2) the present invention does not add any auxiliary material, and bed drain purge reduces:
(3) the present invention adopts high high alkali liquid to leach, and in the stripping aluminum oxide, is easy to silicon is separated with iron, realizes the comprehensive utilization of bauxite Al-Si-Fe;
(4) circulation of high high alkali liquid of the present invention and isolation technique greatly reduce production energy consumption, have simplified production process, have reduced the equipment input, have improved industrial operability, have reduced production cost;
(5) reaction conditions gentleness of the present invention, industrial implementation is workable;
(6) the alumina product quality of alumina product of the present invention and Bayer process is suitable, is better than the aluminum oxide quality of sintering process.
Embodiment
Embodiment 1:
With the atmospheric low-temperature stripping production method of aluminum oxide of the present invention, do the stripping production that raw material carries out aluminum oxide with Yangquan, Shanxi bauxite, the composition (wt%) of Yangquan, Shanxi bauxitic feed materials is as follows:
SiO
2 Fe
2O
3 Al
2O
3 CaO TiO
2 A/S
8.10 5.61 69.80 1.0 2.15 8.62
Its stripping step is:
1, be that 70% NaOH solution mixes with 120-200 purpose bauxite and weight percent concentration, its weight part proportioning is a bauxite: NaOH solution=1: 2 is placed on during reactor carries out, be warming up to 170 ℃, reaction is 0.5 hour under the pressure of 0.55Mpa, obtain containing alkali lye, sodium aluminate, the reaction product mixture of aluminosilicate and scum; After reactant to be mixed is cooled to 90 ℃, adds water the weight percent concentration of NaOH solution be diluted to 40%, 40 ℃ down insulation filter, separate the alkaline solution and the slag that obtain containing sodium aluminate; The solubility rate of aluminium this moment (being contained in the alkaline solution of sodium aluminate) is 96.4%.
2, after alkaline solution evaporation concentration to the weight percent concentration that makes NaOH solution that will contain sodium aluminate is 50%, obtain aluminate hydrates sodium coarse-grain and filtrated stock (bauxite that this mother liquor can be directly used in step 1 leaches reaction) after 5 hours in crystallization under 100 ℃ the temperature;
3, aluminate hydrates sodium coarse-grain is dissolved in water again, is heated to 160 ℃, desiliconization 2 hours makes the sial index of solution reach 500; With the sodium aluminate solution redilution after the desiliconization, and begin to carry out kind of a branch hydrolysis after being cooled to 70 ℃ and obtain aluminium hydroxide, aluminium hydroxide obtains alumina product after calcining.
The alumina product that present embodiment obtains meets the standard of first grade.
The slag that obtains in the above-mentioned steps 2 is through 3 stage countercurrent pulping and washing, and wash temperature is 50 ℃, its washings be used in the dilution of step 1 alkali lye or the step 3 to the macrocrystalline sig water dissolving of aluminate hydrates sodium;
Embodiment 2:
The NaOH solution that the circulation of embodiment 1 is turned back to reactor removes (this moment, the weight percent concentration of NaOH solution was 60%) after the portion water, be warming up to 200 ℃, the bauxite that adds embodiment 1, reacting 3 hours under the mixing condition fully, wherein, NaOH solution and ore deposit weight ratio are 1.5: 1, obtain containing the reaction product mixture of alkali lye, aluminate and red mud (slag); The solubility rate of aluminium is 96.4%.Laterite washing liquid dilute reaction solution with embodiment 1 in 90 ℃ of filtering separation, obtains sodium aluminate alkali solution and red mud; Sodium aluminate alkali lye is concentrated the back obtain the aluminate hydrates sodium crystal in 105 ℃ of crystallizations; Water dissolves it again, then through desiliconization, plant to divide operation to make the aluminium hydroxide product, again with aluminium hydroxide through sintering, just obtain aluminum oxide (standard that meets first grade).The red mud of present embodiment is through 2 stage countercurrent pulping and washing, 90 ℃ of wash temperatures, its washings can be used in the dilution of alkali lye in the step 1 or the step 3 to the macrocrystalline sig water dissolving of aluminate hydrates sodium.
Embodiment 3:
With the atmospheric low-temperature stripping production method of aluminum oxide of the present invention, do the stripping production that raw material carries out aluminum oxide with Henan bauxite, (wt%) is as follows for the composition of Henan bauxite raw material:
SiO
2 Fe
2O
3 Al
2O
3 CaO TiO
2 A/S
6.33 4.07 71.50 0.80 4.31 11.3
Its stripping step is:
1, be that 67% NaOH solution mixes with 120-200 purpose bauxite and weight percent concentration, its weight part proportioning is a bauxite: NaOH solution=1: 1.5 is placed on during reactor carries out, be warming up to 150 ℃, reaction is 7 hours under the pressure of 0.3Mpa, obtain containing alkali lye, sodium aluminate, the reaction product mixture of aluminosilicate and scum; Add water the weight percent concentration of NaOH solution be diluted to 50%, 40 ℃ down insulation filter, 100 ℃ down insulation filter, separate the alkaline solution and the slag that obtain containing sodium aluminate; The solubility rate of aluminium is 83.60% at this moment.
2, after alkaline solution evaporation concentration to the weight percent concentration that makes NaOH solution that will contain sodium aluminate is 650%, obtain aluminate hydrates sodium coarse-grain and filtrated stock (bauxite that this mother liquor can be directly used in step 1 leaches reaction) after 5 hours in crystallization under 50 ℃ the temperature;
3, aluminate hydrates sodium coarse-grain is dissolved in water again, is heated to 160 ℃, desiliconization 2 hours makes the sial index of solution reach 500; With the sodium aluminate solution redilution after the desiliconization, and begin to carry out kind of a branch hydrolysis after being cooled to 70 ℃ and obtain aluminium hydroxide, aluminium hydroxide obtains alumina product after calcining.
The alumina product that present embodiment obtains meets the standard of first grade.
The slag that obtains in the above-mentioned steps 2 is through 1 stage countercurrent pulping and washing, and wash temperature is 90 ℃, its washings be used in the dilution of step 1 alkali lye or the step 3 to the macrocrystalline sig water dissolving of aluminate hydrates sodium;
Embodiment 4:
With the atmospheric low-temperature stripping production method of aluminum oxide of the present invention, do the stripping production that raw material carries out aluminum oxide with Used in Guangxi Pingguo Bauxite Project, (wt%) is as follows for the composition of Used in Guangxi Pingguo Bauxite Project raw material:
SiO
2 Fe
2O
3 Al
2O
3 CaO TiO
2 A/S
7.93 12.87 59.20 3.10 3.47 7.5
Its stripping step is:
1,120-200 purpose bauxite is mixed with the NaOH solution of weight percent concentration 570%, its weight part proportioning is a bauxite: NaOH solution=1: 1 is placed on during reactor carries out, be warming up to 200 ℃, reaction is 10 hours under the pressure of OMpa, obtain containing alkali lye, sodium aluminate, the reaction product mixture of aluminosilicate and scum; Add water the weight percent concentration of NaOH solution be diluted to 45%, 150 ℃ down insulation filter, separate the alkaline solution and the slag that obtain containing sodium aluminate; The solubility rate of aluminium this moment (being contained in the alkaline solution of sodium aluminate) is 97.10%.
2, after alkaline solution evaporation concentration to the weight percent concentration that makes NaOH solution that will contain sodium aluminate is 40%, obtain aluminate hydrates sodium coarse-grain and filtrated stock (bauxite that this mother liquor can be directly used in step 1 leaches reaction) after 5 hours in crystallization under 80 ℃ the temperature;
3, aluminate hydrates sodium coarse-grain is dissolved in water again, is heated to 160 ℃, desiliconization 2 hours makes the sial index of solution reach 500; With the sodium aluminate solution redilution after the desiliconization, and begin to carry out kind of a branch hydrolysis after being cooled to 70 ℃ and obtain aluminium hydroxide, aluminium hydroxide obtains alumina product after calcining.
The alumina product that present embodiment obtains meets the standard of first grade.
The slag that obtains in the above-mentioned steps 2 is through 3 stage countercurrent pulping and washing, and wash temperature is 90 ℃, its washings be used in the dilution of step 1 alkali lye or the step 3 to the macrocrystalline sig water dissolving of aluminate hydrates sodium.
Claims (6)
1, a kind of atmospheric low-temperature stripping production method of aluminum oxide, this stripping production method comprises the steps:
1) be to leach reaction in the 50%-70% alkaline solution with bauxite in weight percent concentration, the weight part proportioning of described bauxite and alkaline solution is 1: 1-2: 1, it leaches temperature of reaction is 150-200 ℃, leaching the reaction times is 0.5-10 hour, adding water or sig water, alkaline solution is diluted to weight percent concentration is 40%-50%, under 40-150 ℃ condition, filter the alkaline solution and the slag that obtain containing sodium aluminate;
2) after the alkaline solution that contains sodium aluminate that step 1) is obtained is concentrated into the weight percent concentration that makes alkaline solution and is 40-60%, be cooled to 50-110 ℃ and carry out crystallization, filter and obtain aluminate hydrates sodium coarse-grain and filtrated stock thereof;
3) with step 2) the aluminate hydrates sodium coarse-grain water that obtains or sig water dissolving, then through desiliconization, plant and divide operation to obtain aluminium hydroxide, again with the aluminium hydroxide that obtains through calcining, just make aluminum oxide.
2, press the atmospheric low-temperature stripping production method of the described aluminum oxide of claim 1, it is characterized in that, this stripping production method comprises that also the slag water of step 1) carries out the multi-stage countercurrent washing, countercurrent washing progression is the 3-5 level, wash temperature is 50-90 ℃, its washings be used in the dilution of step 1) alkali lye or the step 3) to the macrocrystalline sig water dissolving of aluminate hydrates sodium.
3, by the atmospheric low-temperature stripping production method of the described aluminum oxide of claim 1, it is characterized in that this stripping production method also comprises step 2) filtrated stock be directly used in the leaching reaction of the bauxite of step 1).
4, by the atmospheric low-temperature stripping production method of the described aluminum oxide of claim 1, it is characterized in that described alkaline solution is the NaOH aqueous solution.
By the atmospheric low-temperature stripping production method of the described aluminum oxide of claim 1, it is characterized in that 5, the leaching pressure of described leaching reaction is 0-0.55Mpa
By the atmospheric low-temperature stripping production method of the described aluminum oxide of claim 1, it is characterized in that 6, the extraction time of described leaching reaction is 0.5-3 hour.
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| CN 03148717 CN1240617C (en) | 2003-06-24 | 2003-06-24 | Normal pressure low temperature leaching production method for alumina |
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| CN 03148717 CN1240617C (en) | 2003-06-24 | 2003-06-24 | Normal pressure low temperature leaching production method for alumina |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1332884C (en) * | 2005-04-29 | 2007-08-22 | 华建村 | Method for preparing sodium aluminate solution |
| CN100411989C (en) * | 2006-01-23 | 2008-08-20 | 中国铝业股份有限公司 | Method for dissolving out gibbsite |
| CN100386451C (en) * | 2006-03-30 | 2008-05-07 | 中南大学 | Low temperature bauxite leaching process |
| CN101397604B (en) * | 2007-09-30 | 2011-04-20 | 中国科学院过程工程研究所 | Dense alkali liquid leaching pre-desiliconisation method for bauxite |
| CN101746795B (en) * | 2008-12-02 | 2012-04-25 | 中国科学院过程工程研究所 | Method for producing alumina from bauxite |
| CN102476820B (en) * | 2010-11-25 | 2014-04-02 | 中国科学院过程工程研究所 | Method for extracting alumina from coal ash through wet process |
| CN102502733B (en) * | 2011-10-26 | 2013-06-12 | 中国铝业股份有限公司 | Method for treating gibbsite by using high-concentration alkali liquor under normal pressure |
| CN104140122B (en) * | 2013-05-10 | 2016-02-24 | 中国科学院过程工程研究所 | A kind of pre-sulfur method of high-sulfur bauxite |
| CN105126815B (en) * | 2015-07-16 | 2017-09-05 | 福州大学 | A kind of inferior heavy oil suspension bed hydrogenation catalyst and its preparation and application |
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