CN104445310A - Novel process for treating middle-low bauxite in complete wet method alkali system - Google Patents
Novel process for treating middle-low bauxite in complete wet method alkali system Download PDFInfo
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Abstract
The invention discloses a novel process for treating middle-low bauxite in a complete wet method alkali system. The novel process is characterized by comprising the following steps: (1) performing Bayer process for treatment, namely, adding calcium oxide (the addition amount accounts for 5-12% of the weight of bauxite) into grinded middle-low bauxite for dissolving out, diluting the dissolved ore pulp, and performing solid-liquid separation, thereby obtaining a coarse liquid and thick red mud, performing leaf filtration, seed precipitation and roasting on the coarse liquid, thereby obtaining metallurgy aluminum oxide, and evaporating a mother liquid obtained after seed precipitation, wherein the evaporated mother liquid is used in a procedure that alkali is recycled from the red mud, and the sodium carbonate crystal separated in the evaporation process is used in a procedure that aluminum is recycled from the red mud; (2) recycling alkali from the red mud, namely, blending the thick red mud slurry obtained in step (1) with calcium oxide, treating by using the evaporated mother liquid, performing solid-liquid separation so as to obtain filtrate and low-alkali filtering residues, blending the filtrate, and feeding back the filtrate to a Bayer process dissolving procedure; and (3) recycling aluminum from the red mud, namely, treating the low-alkali residues obtained in step (2) by using a sodium carbonate solution, performing solid-liquid separation so as to obtain final red mud residues and a sodium aluminate solution, and feeding back the sodium aluminate solution to the Bayer process procedure.
Description
Technical field
The present invention relates to the extraction of field of hydrometallurgy light metal aluminium, specifically under a kind of Whote-wet method alkaline system, process the novel process that middle-low bauxite produces aluminum oxide.
Background technology
At present in alumina producing, what realize suitability for industrialized production mainly contains Bayer process, sintering process and mixed combining method.Wherein to have energy consumption low for Bayer process, flow process is simple, the advantage that production cost is low, but adopts the requirement of alumina producing Bayer process to raw material strict, its alumina silica ratio of general requirement is greater than 8, is specially adapted to the alumina producing that the high gibbsite-type bauxite raw material of alumina silica ratio carries out.And the bauxite more than 60% of China is the middle-low grade diaspore type of alumina silica ratio 4-6, because the dioxide-containing silica of this bauxite is high, therefore can not directly apply in the low pure bayer process of production cost, and have to adopt flow process longer, energy consumption is higher, the sintering process that construction investment is larger or mixed combining method technique.How according to this situation, develop flow process simple, energy consumption is lower, the alumina producing novel process that can effectively reduce costs, and is the strategic problem that China's Alumina Enterprise must solve.
Along with alumina silica ratio is greater than the needs day by day reducing and reduce energy consumption and production cost of the monohydrated bauxite of 8, utilize low-grade diasporite type bauxite for alumina producing raw material, employing alumina producing Bayer process is an important topic of aluminum oxide industry.People have carried out large quantifier elimination for this reason, and one of them approach improves the pure Bayer process of tradition exactly.
Traditional Bayer process essence reacts hocketing at different conditions below being exactly:
Namely bauxite carries out autoclave digestion process through alkaline solution, makes aluminum oxide wherein enter liquid phase.Some impurity components in this course in mineral are harmful to reaction, wherein maximum with the influence degree of silicon composition to reaction.Silicon composition in conventional Bayer Process digestion process ore pulp and alkaline reaction generate containing sodium aluminosilicate of water, and its molecular formula is roughly equivalent to Na
2oAl
2o
31.7SiO
2nH
2o, wherein Al
2o
3with SiO
2be equal in weight, namely A/S is 1, if the whole SiO in ore
2be converted into this containing sodium aluminosilicate of water, every 1kg SiO
21 kg Al will be caused
2o
3with 0.608 kgNa
2o loses.Make under pressure boils condition, the SiO in ore
2generate containing sodium aluminosilicate of water with alkali reaction, discharge flow process with residue red mud, cause the chemical loss of alkali and have to reclaim again by the method for sintering, increasing production energy consumption, make production cost increase.It has been generally acknowledged that the bauxite that alumina silica ratio is low can cause quite high alkaline consumption in Bayer process is produced, and make production cost too high.Generally believe that A/S is just not suitable for producing by conventional Bayer process at below 7-8 at present.
For reducing alkaline consumption, energy consumption and more effectively utilize China's bauxite resource, has carried out many improvement to traditional Bayer process, as Liquor of Ore Dressing Bayer process, and lime bayer method, series process, Bayer aquation method, the new production processes such as hydrothermal method.In above-mentioned production technique, still there are some problems, as Liquor of Ore Dressing Bayer process employs chemical agent, and cause a large amount of mine tailing to utilize, be unfavorable for effective utilization of China's bauxite.Although lime bayer method reduces alkaline consumption, there is alumina recovery rate low, the problems such as silicon fouling is serious.Although series process can improve the utilization ratio of resource, also there is sintering process in it, and energy consumption is still larger.Bayer aquation method, hydrothermal method can improve the rate of recovery of aluminum oxide, can reduce alkaline consumption again, energy consumption, process middle-low bauxite has greater advantage, but there is high causticity ratio's solution to be difficult to obtain, high causticity ratio's solution decomposes is more difficult, or adopts the method process of heavy aluminium, there is again heavy filter residue more, can not the problem such as efficient recovery, be therefore difficult to realize industrialization.
In addition, apply for a patent 20041004691 for effectively to process middle-low bauxite, propose " symmetrical Bayer ".It uses lower concentration causticity sodium hydroxide solution unlike traditional Bayer process, but use highly concentrated solution stripping bauxite, after stripping completes, the concentration of the causticity sodium oxide when concentration of causticity sodium oxide is greater than the thermodynamic(al)equilibrium common with sodium aluminate (or sodium aluminate hydrate) of hydrated alumina (bauxite) under leaching temperature in solution.Like this, the balance of stripping system is that dissolution-crystallization between sodium aluminate solution and sodium aluminate crystal balances by the equilibrium conversion between the bauxite of traditional Bayer process and sodium aluminate solution.Therefore, no matter gibbsite, boehmite or diaspore all can not stable existences.But the method needs to adopt higher alkali concn, not easily realizes filtering separation, relatively stricter to equipment requirements, and a large amount of moisture is evaporated in requirements of process, reclaims alkali also more difficult from stripping slag.Chinese patent CN 1807251A discloses one and " from high-silica diaspore ore, extracts the method for aluminum oxide ", and the method is combined at symmetrical Bayer and high pressure water chemical method, utilizes symmetrical Bayer directly to process high-silica diaspore ore, extracts aluminum oxide.Adopt high pressure water chemical Treatment red mud again, reclaim wherein by SiO
2in conjunction with Al
2o
3, the solution obtained need not reprocessing, directly send symmetrical Bayer system stripping next batch ore deposit, and the hydrated sodium silicate calcium generated is by hydrolysis, reclaims alkali wherein.But the alkali concn that the high pressure water chemical part of the method adopts is higher, and solid-liquor separation is comparatively difficult, and flow process relative complex, not easy to operate.
Summary of the invention
The object of the invention is the deficiency existed for above-mentioned prior art, propose processing mode under a kind of Whote-wet method alkaline system, energy consumption is low, alkaline consumption is low, alumina recovery rate is high, resource utilization is high, method that middle-low bauxite that the red mud of outer row is easy to fully utilize produces aluminum oxide.
The object of the invention is to be achieved through the following technical solutions:
Process a novel process for middle-low bauxite under Whote-wet method alkaline system, comprise the following steps:
(1) Bayer process process: the middle-low bauxite after grinding is added calcium oxide (addition is the 5-12% of bauxite weight) and carries out stripping, dissolved mineral slurry obtains thick liquid and thick dense red mud slurry after dilution, solid-liquid separation; Thick liquid obtains metallurgical-grade aluminum oxide after leaf filter, decomposition of crystal seed, roasting, and the mother liquor obtained after decomposition of crystal seed reclaims the workshop section of alkali after evaporation for red mud, and the crystals of sodium carbonate that evaporative process is separated out is used for the workshop section that red mud reclaims aluminium;
(2) red mud reclaims alkali: the thick dense red mud slurry obtain step (1) and calcium oxide are prepared burden, and process with mother liquid evaporation, obtain filtrate and low alkali filter residue after solid-liquid separation, turns back to Bayer Process digestion workshop section after filtrate allotment;
(3) red mud reclaims aluminium: low alkali filter residue sodium carbonate solution step (2) obtained processes, and obtain red mud finishing slag and sodium aluminate solution after solid-liquid separation, sodium aluminate solution turns back in Bayer process flow process.
The alumina-silica amount of middle-low bauxite used in described step (1) is than being 3-6.
Mother liquid evaporation concentration is 200-300g/L in described step (2), and the mass ratio 2-4 of the calcium oxide of interpolation and silicon-dioxide in red mud, liquid-solid ratio (liquid volume and solid masses compare) 3-8, temperature of reaction 200-300 DEG C, the reaction times is 0.5-3 hour.
Concentration of sodium carbonate 20-100g/L, liquid-solid ratio 5-12, temperature of reaction 80-200 DEG C in described step (3), the reaction times is 1-5 hour.
In described step (3), the red mud finishing slag of gained directly can be stored up or be used as building materials raw material.
First this novel process reclaims most of aluminum oxide with Bayer process process middle-low bauxite, and gained red mud carries out dealkalize and dealuminzation more respectively, thus realizes the alkali of red mud, alum recovery and harmless treatment.The dominant of red mud is sodium aluminium silicate mutually, at 200-300 DEG C, adds calcium oxide, and process red mud with the alkali lye (being mother liquid evaporation in the present invention) of intermediate concentration and generate hydrotalcite garnet, can realize the recovery of alkali in red mud, the chemical equation of generation is:
(1)
Formula (1) is although can realize the recovery of alkali in red mud, but the aluminium in solution can enter in solid phase the loss causing aluminium, therefore the low alkali filter residue (hydrotalcite garnet) after dealkalize is due to containing more aluminium, need to reclaim, consideration sodium carbonate solution leaches, and the chemical reaction of generation may be:
(2)
(3)
Reclaim the mixture of the finishing slag after aluminium mainly calcium silicate hydrate and calcium carbonate, can directly to store up or as material of construction.
Compared with the method processing middle-low bauxite with other, advantage of the present invention has:
(1) middle-low bauxite of suitable treatment China of the present invention, alumina recovery rate is high, and alkaline consumption is low.First reclaim the most of aluminum oxide in bauxite by Bayer process, then process red mud, to reclaim aluminium in red mud and alkali, in red mud finishing slag, alumina silica ratio can reach less than 0.8, sodium-silicon-rate (Na in red mud
2o and SiO
2mass ratio) can less than 0.2 be reached, there is good popularizing application prospect.
(2) whole reaction system is alkali systems, there is not high density, high causticity ratio's alkali lye, and be convenient to be connected with Bayer process, and there is not high temperature sintering, energy consumption is low.
(3) crystals of sodium carbonate that Bayer process partial mother liquid evaporization process of the present invention obtains does not need causticization, and is directly used in the workshop section reclaiming aluminium in red mud.
(4) Na in the red mud arranged outward
2o content is low, is conducive to the comprehensive utilization of red mud.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention.
Embodiment
Embodiment 1
(1) Bayer process process: by ground somewhere low-grade bauxite (place of production Jin Jiang River, primary chemical composition is in table 1) and calcium oxide (addition is 8% of bauxite weight) and circulating mother liquor (Na
2o
kfor 240g/L) prepare burden, and at 260 DEG C stripping 60min.Dissolved mineral slurry obtains thick liquid and thick dense red mud slurry after dilution, solid-liquid separation.Thick liquid obtains seminal fluid after leaf filter, add aluminium hydroxide and do crystal seed (aluminium hydroxide of interpolation and the ratio of hydroxide aluminum amount in sodium aluminate solution, namely seed ratio is 4), filter after decomposing 45h at 60 DEG C and obtain aluminium hydroxide, after 1050 DEG C of roastings, obtain metallurgical-grade aluminum oxide.The mother liquid evaporation obtained after decomposition of crystal seed is to Na
2o
kfor reclaiming the workshop section of alkali after 240g/L for red mud, the crystals of sodium carbonate that evaporative process is separated out is used for the workshop section that red mud reclaims aluminium.
(2) red mud reclaims alkali: the thick dense red mud slurry obtain step (1) and mother liquid evaporation, calcium oxide carries out preparing burden (mass ratio 2.5 of silicon-dioxide in calcium oxide addition and red mud, Na in feed liquid
2o
kbe about 200g/L, liquid-solid ratio (liquid volume and solid masses ratio) is 5) and react 2h at 280 DEG C, to reclaim the alkali in red mud, obtain filtrate and low alkali filter residue after solid-liquid separation, filtrate is formulated to Na
2o
kfor turning back to Bayer Process digestion workshop section after 240g/L.Know that in red mud, the rate of recovery of alkali is about 92% as calculated.
(3) red mud reclaims aluminium: low alkali filter residue step (2) obtained and sodium carbonate solution carry out preparing burden (concentration of sodium carbonate 60g/L in feed liquid, liquid-solid ratio is 10) and 3h is reacted at 150 DEG C, to reclaim the aluminium in red mud, obtain red mud finishing slag and sodium aluminate solution after solid-liquid separation, sodium aluminate solution turns back in Bayer process flow process.Know alumina silica ratio about 0.75 in red mud finishing slag as calculated, sodium-silicon-rate about 0.17.
Table 1: unit wt%
Al 2O 3 | SiO 2 | Fe 2O 3 | TiO 2 | H 2O | A/S |
60.5 | 11.9 | 6.3 | 2.8 | - | 5.1 |
Embodiment 2
(1) Bayer process process: by ground somewhere low-grade bauxite (derive from Cayman, Sanmenxia Gorge Aluminum, primary chemical composition is in table 2) and calcium oxide (addition is 6% of bauxite weight) and circulating mother liquor (Na
2o
kfor 260g/L) prepare burden, and at 265 DEG C stripping 45min.Dissolved mineral slurry obtains thick liquid and thick dense red mud slurry after dilution, solid-liquid separation.Thick liquid obtains seminal fluid after leaf filter, and interpolation aluminium hydroxide does crystal seed (seed ratio is 4) filtration after 65 DEG C of decomposition 40h and obtains aluminium hydroxide, after 1100 DEG C of roastings, obtain metallurgical-grade aluminum oxide.The mother liquid evaporation obtained after decomposition of crystal seed is to Na
2o
kfor reclaiming the workshop section of alkali after 260g/L for red mud, the crystals of sodium carbonate that evaporative process is separated out is used for the workshop section that red mud reclaims aluminium.
(2) red mud reclaims alkali: the thick dense red mud slurry obtain step (1) and mother liquid evaporation, calcium oxide carries out preparing burden (mass ratio 3 of silicon-dioxide in calcium oxide addition and red mud, Na in feed liquid
2o
kbe about 210g/L, liquid-solid ratio is 5) and at 280 DEG C of reaction 3h, to reclaim the alkali in red mud, obtain filtrate and low alkali filter residue after solid-liquid separation, filtrate is formulated to Na
2o
kfor turning back to Bayer Process digestion workshop section after 260g/L.Know that in red mud, the rate of recovery of alkali is about 93% as calculated.
(3) red mud reclaims aluminium: low alkali filter residue step (2) obtained and sodium carbonate solution carry out preparing burden (concentration of sodium carbonate 80g/L in feed liquid, liquid-solid ratio is 8) and 3h is reacted at 180 DEG C, to reclaim the aluminium in red mud, obtain red mud finishing slag and sodium aluminate solution after solid-liquid separation, sodium aluminate solution turns back in Bayer process flow process.Know alumina silica ratio about 0.72 in red mud finishing slag as calculated, sodium-silicon-rate about 0.16.
Table 2: unit wt%
Al 2O 3 | SiO 2 | Fe 2O 3 | TiO 2 | H 2O | A/S |
62.3 | 11.47 | 6.29 | 2.8 | - | 5.43 |
Embodiment 3
(1) Bayer process process: by ground somewhere, Guizhou low-grade bauxite (primary chemical composition is in table 3) and calcium oxide (addition is 10% of bauxite weight) and circulating mother liquor (Na
2o
kfor 245g/L) prepare burden, and at 280 DEG C stripping 45min.Dissolved mineral slurry obtains thick liquid and thick dense red mud slurry after dilution, solid-liquid separation.Thick liquid obtains seminal fluid after leaf filter, and interpolation aluminium hydroxide does crystal seed (seed ratio is 4.5) filtration after 65 DEG C of decomposition 50h and obtains aluminium hydroxide, after 1100 DEG C of roastings, obtain metallurgical-grade aluminum oxide.The mother liquid evaporation obtained after decomposition of crystal seed is to Na
2o
kfor reclaiming the workshop section of alkali after 245g/L for red mud, the crystals of sodium carbonate that evaporative process is separated out is used for the workshop section that red mud reclaims aluminium.
(2) red mud reclaims alkali: the thick dense red mud slurry obtain step (1) and mother liquid evaporation, calcium oxide carries out preparing burden (mass ratio 4 of silicon-dioxide in calcium oxide addition and red mud, Na in feed liquid
2o
kbe about 190g/L, liquid-solid ratio is 3) and at 300 DEG C of reaction 1.5h, to reclaim the alkali in red mud, obtain filtrate and low alkali filter residue after solid-liquid separation, filtrate is formulated to Na
2o
kfor turning back to Bayer Process digestion workshop section after 245g/L.Know that in red mud, the rate of recovery of alkali is about 86% as calculated.
(3) red mud reclaims aluminium: low alkali filter residue step (2) obtained and sodium carbonate solution carry out preparing burden (concentration of sodium carbonate 100g/L in feed liquid, liquid-solid ratio is 5) and 1h is reacted at 200 DEG C, to reclaim the aluminium in red mud, obtain red mud finishing slag and sodium aluminate solution after solid-liquid separation, sodium aluminate solution turns back in Bayer process flow process.Know alumina silica ratio about 0.88 in red mud finishing slag as calculated, sodium-silicon-rate about 0.2.
Table 3: unit wt%
Al 2O 3 | SiO 2 | Fe 2O 3 | TiO 2 | H 2O | A/S |
62.65 | 13 | 2.58 | 2.95 | - | 4.82 |
Embodiment 4
(1) Bayer process process: by ground Yangquan Shanxi low-grade bauxite (primary chemical composition is in table 4) and calcium oxide (addition is 11% of bauxite weight) and circulating mother liquor (Na
2o
kfor 270g/L) prepare burden, and at 280 DEG C stripping 60min.Dissolved mineral slurry obtains thick liquid and thick dense red mud slurry after dilution, solid-liquid separation.Thick liquid obtains seminal fluid after leaf filter, and interpolation aluminium hydroxide does crystal seed (seed ratio is 4) filtration after 65 DEG C of decomposition 50h and obtains aluminium hydroxide, after 1050 DEG C of roastings, obtain metallurgical-grade aluminum oxide.The mother liquid evaporation obtained after decomposition of crystal seed is to Na
2o
kfor reclaiming the workshop section of alkali after 270g/L for red mud, the crystals of sodium carbonate that evaporative process is separated out is used for the workshop section that red mud reclaims aluminium.
(2) red mud reclaims alkali: the thick dense red mud slurry obtain step (1) and mother liquid evaporation, calcium oxide carries out preparing burden (mass ratio 3 of silicon-dioxide in calcium oxide addition and red mud, Na in feed liquid
2o
kbe about 205g/L, liquid-solid ratio is 8) and at 200 DEG C of reaction 3h, to reclaim the alkali in red mud, obtain filtrate and low alkali filter residue after solid-liquid separation, filtrate is formulated to Na
2o
kfor turning back to Bayer Process digestion workshop section after 270g/L.Know that in red mud, the rate of recovery of alkali is about 90% as calculated.
(3) red mud reclaims aluminium: low alkali filter residue step (2) obtained and sodium carbonate solution carry out preparing burden (concentration of sodium carbonate 20g/L in feed liquid, liquid-solid ratio is 12) and 5h is reacted at 80 DEG C, to reclaim the aluminium in red mud, obtain red mud finishing slag and sodium aluminate solution after solid-liquid separation, sodium aluminate solution turns back in Bayer process flow process.Know alumina silica ratio about 0.96 in red mud finishing slag as calculated, sodium-silicon-rate about 0.18.
Table 4: unit wt%
Al 2O 3 | SiO 2 | Fe 2O 3 | TiO 2 | H 2O | A/S |
60.34 | 17.16 | 5.61 | 2.15 | - | 3.5 |
Claims (5)
1. process a novel process for middle-low bauxite under Whote-wet method alkaline system, it is characterized in that: comprise the following steps:
(1) Bayer process process: the middle-low bauxite after grinding is added the calcium oxide accounting for bauxite weight 5-12% and carries out stripping, dissolved mineral slurry obtains thick liquid and thick dense red mud slurry after dilution, solid-liquid separation; Thick liquid obtains metallurgical-grade aluminum oxide after leaf filter, decomposition of crystal seed, roasting, and the mother liquor obtained after decomposition of crystal seed reclaims the workshop section of alkali after evaporation for red mud, and the crystals of sodium carbonate that evaporative process is separated out is used for the workshop section that red mud reclaims aluminium;
(2) red mud reclaims alkali: the thick dense red mud slurry obtain step (1) and calcium oxide are prepared burden, and process with mother liquid evaporation, obtain filtrate and low alkali filter residue after solid-liquid separation, turns back to Bayer Process digestion workshop section after filtrate allotment;
(3) red mud reclaims aluminium: low alkali filter residue sodium carbonate solution step (2) obtained processes, and obtain red mud finishing slag and sodium aluminate solution after solid-liquid separation, sodium aluminate solution turns back in Bayer process flow process.
2. process the novel process of middle-low bauxite under a kind of Whote-wet method alkaline system according to claim 1, it is characterized in that: the alumina-silica amount of middle-low bauxite used in step (1) is than being 3-6.
3. under a kind of Whote-wet method alkaline system according to claim 1, process the novel process of middle-low bauxite, it is characterized in that: in step (2), mother liquid evaporation concentration is 200-300g/L, the mass ratio 2-4 of silicon-dioxide in the calcium oxide added and red mud, liquid-solid ratio 3-8, temperature of reaction 200-300 DEG C, the reaction times is 0.5-3 hour.
4. process the novel process of middle-low bauxite under a kind of Whote-wet method alkaline system according to claim 1, it is characterized in that: concentration of sodium carbonate 20-100g/L, liquid-solid ratio 5-12, temperature of reaction 80-200 DEG C in step (3), the reaction times is 1-5 hour.
5. process the novel process of middle-low bauxite under a kind of Whote-wet method alkaline system according to claim 1, it is characterized in that: in step (3), the red mud finishing slag of gained directly can be stored up or be used as building materials raw material.
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Cited By (5)
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WO2018233687A1 (en) * | 2017-06-23 | 2018-12-27 | 东北大学 | Method for producing sodium aluminate from medium and low-grade bauxite by one-step alkali thermal treatment through andradite |
WO2018233688A1 (en) * | 2017-06-23 | 2018-12-27 | 东北大学 | Method for preparing aluminum hydroxide by treating medium- and low-grade bauxite by using one-step alkali heat process of andradite |
WO2018233689A1 (en) * | 2017-06-23 | 2018-12-27 | 东北大学 | Method for preparing metallurgical-level aluminum oxide by treating bayer process-based red mud by using one-step alkali heat process of andradite |
WO2018233686A1 (en) * | 2017-06-23 | 2018-12-27 | 东北大学 | Method for preparing metallurgical-level aluminum oxide by treating medium- and low-grade bauxite by using one-step alkali heat process of andradite |
CN111960440A (en) * | 2020-09-02 | 2020-11-20 | 陶予敏 | Process for producing soda ash and building insulating brick from red mud |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2018233687A1 (en) * | 2017-06-23 | 2018-12-27 | 东北大学 | Method for producing sodium aluminate from medium and low-grade bauxite by one-step alkali thermal treatment through andradite |
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WO2018233689A1 (en) * | 2017-06-23 | 2018-12-27 | 东北大学 | Method for preparing metallurgical-level aluminum oxide by treating bayer process-based red mud by using one-step alkali heat process of andradite |
WO2018233686A1 (en) * | 2017-06-23 | 2018-12-27 | 东北大学 | Method for preparing metallurgical-level aluminum oxide by treating medium- and low-grade bauxite by using one-step alkali heat process of andradite |
CN111960440A (en) * | 2020-09-02 | 2020-11-20 | 陶予敏 | Process for producing soda ash and building insulating brick from red mud |
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