CN103131854B - Method for comprehensively recovering scandium and titanium by leaching red mud with titanium white waste acid - Google Patents
Method for comprehensively recovering scandium and titanium by leaching red mud with titanium white waste acid Download PDFInfo
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Abstract
The invention relates to a method for comprehensively recovering scandium and titanium by leaching red mud with titanium white waste acid, which comprises the following steps: at ordinary pressure, dipping red mud with titanium white waste acid having a liquid-to-solid ratio of 4.0-6.0, performing secondary acid dipping on the leached slag, dealkalizing the secondary acid dipping slag, further performing strong magnetic separation to obtain iron-containing ores and tailings, and performing secondary strong magnetic separation on the iron-containing ores to obtain iron concentrated ores and middlings; extracting the leaching solution, performing back extraction, dissolving in acid to perform hydrolysis, performing secondary extraction, removing impurities, performing secondary back extraction, dissolving in hydrochloric acid, adding oxalic acid to precipitate, and calcining to obtain a scandium oxide product; dissolving the back extraction slag in sulfuric acid, and performing hydrolysis under the conditions of heating and boiling for 2-3 hours, thus obtaining metatitanic acid; and drying the metatitanic acid, calcining, and pulverizing to obtain titanium yellow powder. The invention realizes the combined treatment of titanium white waste acid and red mud, treats wastes with wastes, changes wastes into valuable substances, comprehensively recycles the two major pollution sources (i.e. titanium white waste acid and red mud), and mainly recovers the iron ores, titanium and rare noble metal scandium in the pollution sources.
Description
Technical field
The present invention relates to a kind of titanium white waste acid that utilizes and leach the method that red mud comprehensively reclaims scandium and titanium, belong to technical field of wet metallurgy.
Background technology
At present, these traditional processing technologies of sulfuric acid process for the China's titanium white powder manufacturer overwhelming majority, it is 8～10 tons, 15～20% spent acid that 1 ton of titanium white of every production will produce concentration, and its containing scandium amount all at 10～30mg/L, have to recycle and be worth.Existing processing titanium white waste acid mainly by neutralization discharge, concentrated recycling, produce the modes such as Sulfates, these ways are not that cost costliness is exactly that secondary pollution is serious, fail fundamentally to solve the problem of outlet of spent acid.
In red mud, except the metallic elements such as iron content, aluminium, sodium, calcium, also containing multiple valuable component as rare metals such as scandium, rare earths, is a kind of abundant secondary resource.China is alumina producing big country, produces every year ten million ton of above Bayer process red mud, piles up over the years store content huge.At present, domestic and international most alumina producing enterprise all carries out open storage to red mud and stores up, store up for a long time the land resources that not only takies rare preciousness, and very easily cause the pollution of earth's surface, air, underground water and destruction, and the potential safety hazard that leaks of the red mud that lies dormant.Therefore, accelerating the resource utilization recycling of red mud, is the important channel of realizing sustainable development of alumina industry, significant to building a resource-conserving society.For a long time, Chinese scholars has been carried out a large amount of Test And Research Works aspect the comprehensive utilization of red mud.Red mud from sintering process has obtained utilization in various degree, and to Bayer process red mud, although a lot of effectively schemes have been proposed, due to reason technical and economically. the overwhelming majority fails to be put to industrial practice.
In the 9th command < < industry restructuring guidance list (basis in 2011) the > > of National Development and Reform Committee, clearly call the research work of carrying out " red mud and the comprehensive utilization of other melting waste slag " and " metallurgical waste liquid (containing waste water, spent acid, waste oil etc.) utilization process technology ".Therefore, the improvement of red mud and titanium white waste acid and recycling will be the emphasis research direction that Future in China is smelted the waste comprehensive regulation for several years.In addition, owing to containing a large amount of scandium resources in red mud and titanium white waste acid liquid, be the rare metal of tool recovery value in comprehensive regulation process.Simultaneously, the research that China extracts Scium trioxide in these two kinds are smelted wastes early, state of the art is in a leading position in the whole world, once carry out the comprehensive regulation of red mud and titanium white waste acid comprehensively, the output that can predict China's Scium trioxide will promote rapidly, and this will certainly drive the process deeply industry of Scium trioxide fast-developing.
Summary of the invention
The object of the present invention is to provide a kind of titanium white waste acid that utilizes to leach the method that red mud comprehensively reclaims scandium and titanium, titanium white waste acid is combined to improvement with red mud, the treatment of wastes with processes of wastes against one another, turn waste into wealth, realize the comprehensive reutilization of titanium white waste acid and red mud two large source of pollution, iron ore, titanium and rare precious metal scandium wherein carried out to emphasis recovery.
A kind of titanium white waste acid that utilizes of the present invention leaches the method that red mud comprehensively reclaims scandium and titanium, comprises the steps:
1. the spent acid of Bayer process red mud, sulfuric acid method titanium pigment factory by-product of take is raw material, and under normal pressure, the liquid-solid ratio titanium white waste acid that by volume weight ratio is 4.0～6.0 embathes red mud;
2. leached mud is done secondary pickling with sulfuric acid;
3. the dealkalize of secondary pickling slag must contain iron ore and mine tailing by a step high intensity magnetic separation, containing iron ore, obtains iron ore concentrate and chats again through two step high intensity magnetic separations;
4. leach liquor obtains Scium trioxide product through extraction, back extraction, sour molten hydrolysis, reextraction, removal of impurities, secondary back extraction, dissolving with hydrochloric acid, oxalic acid precipitation, calcination process;
5. back extraction slag is through sulfuric acid dissolution, heated and boiled Water Under solution 2～3 hours, obtains metatitanic acid, and metatitanic acid drying is placed in 700～850 ℃ of retort furnaces and calcines 2～3 hours, obtains titanium yellow powder after pulverizing.
It is under normal pressure that described titanium white waste acid embathes red mud, utilizes the titanium white waste acid of 1.0～1.8mol/L concentration to embathe red mud, and liquid-solid ratio by volume weight ratio is 3.0～6.0,50～100 ℃ of temperature of reaction, 30～60 minutes reaction times.
It is under normal pressure that described leached mud is done secondary pickling, with the sulfuric acid of 3.5～5.0mol/L concentration, leached mud is carried out to secondary pickling, and liquid-solid ratio by volume weight ratio is 3.0～6.0,50～100 ℃ of temperature of reaction, 30～60 minutes reaction times.
The dealkalize of described secondary pickling slag is to be to carry out under 10000～12000 Ο e in magneticstrength by a step high intensity magnetic separation, must contain iron ore and mine tailing, containing iron ore, in magneticstrength, is under 9000～12000 Ο e, to carry out two step high intensity magnetic separations to obtain iron ore concentrate and chats.
The extraction of described leach liquor is to make extraction agent with organic phase di (isooctyl) phosphate P204, secondary octanol, sulfonated kerosene=16:4:80, in the ratio of O/A=1:8～10, leach liquor is extracted, and extraction time 20～30 minutes, obtains the organic phase of rich scandium, titanium.
Described back extraction is to make reverse-extraction agent with the NaOH that concentration is 2～2.5mol/L, 20～30 minutes back extraction time, by the scandium in rich scandium, titanium organic phase, titanium back extraction out.
The heavy molten back extraction slag of sulfuric acid that described back extraction slag through sulfuric acid dissolution is is under agitation 1.8～2.2mol/L by concentration, adds crystal seed, keeps solution boiling state 2.0～3.0 hours, solution is carried out to the thermal hydrolysis of titanium.
Described removal of impurities is that compound concentration is the hydrochloric acid soln of 5～8mol/L, in the ratio of O/A=1～1.5:1, washs rich scandium organic phase, and washing time 10～20 minutes, washes away the impurity in organic phase.
Rich scandium organic phase after described removal of impurities is made reverse-extraction agent with the NaOH that concentration is 2～2.5mol/L, carries out secondary counter extraction, 20～30 minutes back extraction time, obtains secondary back extraction slag.
The dissolving with hydrochloric acid secondary back extraction slag that described secondary back extraction slag is 6mol/L by concentration, after dissolving, adjust pH to 1.5～2.0, be heated to 80～90 ℃, add solid oxalic acid to react, 30～60 minutes reaction times, obtain scandium throw out after filtration, washing, dry to be placed in 800 ℃ of retort furnaces and calcine 2～3 hours, obtain 98%～99% Scium trioxide product.
Liquid-solid ratio of the present invention by volume weight ratio be by hydrometallurgy sanctified by usage the volume of leach liquor is directly compared with the weight of reaction solid materials, it is ml/g, L/kg or m that unit closes
3/ t.
Beneficial effect of the present invention is:
1, the treatment of wastes with processes of wastes against one another.With titanium white waste acid, administer red mud, realize the comprehensive reutilization of titanium white waste acid and the comprehensive reutilization of red mud.
2, technique is simple, with low cost.Using the most cheap spent acid and red mud is raw material, adopts the simplest technical process, makes the comprehensive reutilization of titanium white waste acid and the red mud simple possible that becomes in suitability for industrialized production.
3, can realize the suitability for industrialized production of Scium trioxide.The scandium element that all contains tool recovery value in titanium white waste acid and red mud, two kinds of raw materials, in conjunction with making scandium obtain enrichment, can make again cost obtain the reduction of maximum amplitude, make the suitability for industrialized production of scandium become feasible.
Accompanying drawing explanation
Fig. 1 is that the titanium white waste acid that utilizes of the present invention leaches the process flow sheet that red mud comprehensively reclaims the method for scandium and titanium.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is further described.
Embodiment 1
The titanium white waste acid that utilizes of the present invention leaches the method that red mud comprehensively reclaims scandium and titanium, comprises the steps:
Red mud is taken from Guangxi pingguo Aluminum company limited, titanium white waste acid is taken from Guangxi Gold Mao Tai industry company limited.
In 100L retort, adding concentration is the titanium white waste acid solution 60L of 1.0mol/L, under agitation adds gradually 13kg red mud, 75 ℃ of temperature of reaction, 30 minutes reaction times.Slurries after leaching obtain leached mud and leach liquor after pressure filter press filtration washing.Sc in leach liquor
2o
3content 29mg/L, TiO
2content is 6.8g/L.
The spent acid that leached mud is 3.5mol/L by concentration carries out secondary leaching, under agitation adds gradually leached mud one time, controls 75 ℃ of temperature of reaction, 30 minutes reaction times.Slurries after leaching obtain secondary leached mud and leach liquor after pressure filter press filtration washing.
Secondary leached mud first carries out high intensity magnetic separation one time with intensity magnetic separator, and magneticstrength 12000 Ο e, obtain mine tailing, productive rate 71%, iron grade 23% and containing iron ore, containing iron ore, through secondary high intensity magnetic separation, magneticstrength 9000 Ο e obtain iron ore concentrate, productive rate 17%, iron grade 58% and chats, productive rate 9%, iron grade 40%.
Preparation organic phase: di (isooctyl) phosphate P204, secondary octanol, sulfonated kerosene=16:4:80.Leach liquor and secondary leach liquor mix, and adopt the leach liquor that compares of O/A=1:8 to extract.Extraction progression is 2, and extraction time is 20 minutes.Obtain rich scandium, titanium organic phase.The percentage extraction 97% of this step scandium, the percentage extraction 92% of titanium.
The NaOH solution that preparation concentration is 2.0mol/L.In the ratio of O/A=1.5:1, scandium, titanium in rich scandium organic phase are stripped.20 minutes back extraction time, the back extraction ratio 99% of scandium, the back extraction ratio 99% of titanium.
In retort, adding concentration is the sulphuric acid soln of 1.8mol/L, adds back extraction slag, adds crystal seed, under agitation keeps solution boiling state 2.5 hours.Reacted feed liquid after filtration, washing obtains metatitanic acid and hydrolyzed solution.Metatitanic acid drying is placed in 700 ℃ of retort furnaces and calcines 2 hours, then can obtain titanium yellow powder product after pulverizing with ball mill.
Except the hydrolyzed solution after titanium carries out reextraction by above-mentioned steps again, obtain the organic camera of rich scandium, raffinate.Compound concentration is the hydrochloric acid soln of 5mol/L, in the ratio of O/A=1.5:1, washs rich scandium organic phase, washing time 15 minutes.
Compound concentration is the sodium hydroxide solution of 2.0mol/L, in the ratio of O/A=1.5:1, rich scandium organic phase is carried out to back extraction, obtains scandium hydroxide enrichment slag after back extraction.
The hydrochloric acid soln that first compound concentration is 6mol/L, under agitation adds scandium hydroxide enrichment slag, after fully dissolving, filters, and adjusts PH to 1.8, adds solid oxalic acid to react, 40 minutes reaction times under 80 ℃ of conditions.Gained scandium throw out after filtration, washing, dry to be placed in 800 ℃ of retort furnaces and calcine 3 hours, obtain 99% Scium trioxide product.
Embodiment 2
The titanium white waste acid that utilizes of the present invention leaches the method that red mud comprehensively reclaims scandium and titanium, comprises the steps:
Red mud is taken from Guangxi pingguo Aluminum company limited, titanium white waste acid is taken from Guangxi Gold Mao Tai industry company limited.
In 100L retort, adding concentration is the titanium white waste acid solution 60L of 1.5mol/L, under agitation adds gradually 13kg red mud, 50 ℃ of temperature of reaction, 60 minutes reaction times.Slurries after leaching obtain leached mud and leach liquor after pressure filter press filtration washing.Sc in leach liquor
2o
3content 35mg/L, TiO
2content is 9g/L.
The spent acid that leached mud is 4.0mol/L by concentration carries out secondary leaching, under agitation adds gradually leached mud one time, controls 100 ℃ of temperature of reaction, 60 minutes reaction times.Slurries after leaching obtain secondary leached mud and leach liquor after pressure filter press filtration washing.
Secondary leached mud first carries out high intensity magnetic separation one time with intensity magnetic separator, magneticstrength 12500 Ο e, obtain mine tailing, productive rate 75%, iron grade 25% and containing iron ore, contain iron ore through secondary high intensity magnetic separation, magneticstrength 9600 Ο e, obtain iron ore concentrate, productive rate 15.5%, iron grade 57%, and chats, productive rate 8.8%, iron grade 42%.
Preparation organic phase: di (isooctyl) phosphate (P204), secondary octanol, sulfonated kerosene=16:4:80.Leach liquor and secondary leach liquor mix, and adopt the leach liquor that compares of O/A=1:10 to extract.Extraction progression is 2, and extraction time is 25 minutes, obtains rich scandium, the organic camera of titanium.The percentage extraction 96% of this step scandium, the percentage extraction 90% of titanium.
The NaOH solution that preparation concentration is 2.5mol/L.In the ratio of O/A=1.5:1, scandium, titanium in rich scandium organic phase are stripped.30 minutes back extraction time, the back extraction ratio 99% of scandium, the back extraction ratio 99% of titanium.
In retort, adding concentration is the sulphuric acid soln of 2.2mol/L, adds back extraction slag, adds crystal seed, under agitation keeps solution boiling state 2.0 hours.Reacted feed liquid after filtration, washing obtains metatitanic acid and hydrolyzed solution.Metatitanic acid drying is placed in 800 ℃ of retort furnaces and calcines 2 hours, then can obtain titanium yellow powder product after pulverizing with ball mill.
Except the hydrolyzed solution after titanium carries out reextraction by above-mentioned steps again, obtain the organic camera of rich scandium, raffinate.Compound concentration is the hydrochloric acid soln of 6mol/L, in the ratio of O/A=1.5:1, washs rich scandium organic phase, washing time 20 minutes.
Compound concentration is the sodium hydroxide solution of 2.5mol/L, in the ratio of O/A=1.5:1, rich scandium organic phase is carried out to back extraction, obtains scandium hydroxide enrichment slag after back extraction.
The hydrochloric acid soln that first compound concentration is 6mol/L, under agitation adds scandium hydroxide enrichment slag, after fully dissolving, filters, and adjusts PH to 1.5, adds solid oxalic acid to react, 60 minutes reaction times under 85 ℃ of conditions.Gained scandium throw out after filtration, washing, dry to be placed in 800 ℃ of retort furnaces and calcine 2 hours, obtain 98% Scium trioxide product.
Embodiment 3
The titanium white waste acid that utilizes of the present invention leaches the method that red mud comprehensively reclaims scandium and titanium, comprises the steps:
Red mud is taken from Guangxi pingguo Aluminum company limited, titanium white waste acid is taken from Guangxi Gold Mao Tai industry company limited.
In 100L retort, adding concentration is the titanium white waste acid solution 60L of 1.8mol/L, under agitation adds gradually 13kg red mud, 100 ℃ of temperature of reaction, 60 minutes reaction times.Slurries after leaching obtain leached mud and leach liquor after pressure filter press filtration washing.Sc in leach liquor
2o
3content 40mg/L, TiO
2content is 9g/L.
The spent acid that leached mud is 5.0mol/L by concentration carries out secondary leaching, under agitation adds gradually leached mud one time, controls 100 ℃ of temperature of reaction, 60 minutes reaction times.Slurries after leaching obtain secondary leached mud and leach liquor after pressure filter press filtration washing.
Secondary leached mud first carries out high intensity magnetic separation one time with intensity magnetic separator, and magneticstrength 13000 Ο e, obtain mine tailing, productive rate 71%, iron grade 23%, and containing iron ore, contain iron ore through secondary high intensity magnetic separation, magneticstrength 10000 Ο e, obtain iron ore concentrate, productive rate 18%, iron grade 60%, and chats, productive rate 8%, iron grade 42.5%.
Preparation organic phase: di (isooctyl) phosphate P204, secondary octanol, sulfonated kerosene=16:4:80.Leach liquor and secondary leach liquor mix, and adopt the leach liquor that compares of O/A=1:9 to extract.Extraction progression is 2, and extraction time is 30 minutes, obtains rich scandium, the organic camera of titanium.The percentage extraction 96% of this step scandium, the percentage extraction 91% of titanium.
The NaOH solution that preparation concentration is 2.5mol/L.In the ratio of O/A=1.5:1, scandium, titanium in rich scandium organic phase are stripped.30 minutes back extraction time, the back extraction ratio 99% of scandium, the back extraction ratio 99% of titanium.
In retort, adding concentration is the sulphuric acid soln of 2.2mol/L, adds back extraction slag, adds crystal seed, under agitation keeps solution boiling state 3 hours.Reacted feed liquid after filtration, washing obtains metatitanic acid and hydrolyzed solution.Metatitanic acid drying is placed in 850 ℃ of retort furnaces and calcines 2 hours, then can obtain titanium yellow powder product after pulverizing with ball mill.
Except the hydrolyzed solution after titanium carries out reextraction by above-mentioned steps again, obtain the organic camera of rich scandium, raffinate.Compound concentration is the hydrochloric acid soln of 8mol/L, in the ratio of O/A=1.5:1, washs rich scandium organic phase, washing time 20 minutes.
Compound concentration is the sodium hydroxide solution of 2.2mol/L, in the ratio of O/A=1.5:1, rich scandium organic phase is carried out to back extraction, obtains scandium hydroxide enrichment slag after back extraction.
The hydrochloric acid soln that first compound concentration is 6mol/L, under agitation adds scandium hydroxide enrichment slag, after fully dissolving, filters, and adjusts PH to 2.0, adds solid oxalic acid to react, 60 minutes reaction times under 90 ℃ of conditions.Gained scandium throw out after filtration, washing, dry to be placed in 800 ℃ of retort furnaces and calcine 3 hours, obtain 99% Scium trioxide product.
Claims (1)
1. utilize titanium white waste acid to leach the method that red mud comprehensively reclaims scandium and titanium, it is characterized in that, comprise the steps:
1. the spent acid of Bayer process red mud, sulfuric acid method titanium pigment factory by-product of take is raw material, under normal pressure, utilizes the titanium white waste acid of 1.0～1.8mol/L concentration to embathe red mud, and liquid-solid ratio by volume weight ratio is 4.0～6.0, and the unit of envelope-bulk to weight ratio is ml/g, L/kg or m
3/ t, 50～100 ℃ of temperature of reaction, in 30～60 minutes reaction times, the slurries after leaching obtain leached mud and leach liquor after pressure filter press filtration washing;
2. a leached mud, under normal pressure, carries out secondary pickling with the sulfuric acid of 3.5～5.0mol/L concentration, and liquid-solid ratio by volume weight ratio is 3.0～6.0, and the unit of envelope-bulk to weight ratio is ml/g, L/kg or m
3/ t, 50～100 ℃ of temperature of reaction, in 30～60 minutes reaction times, the slurries after leaching obtain secondary leached mud and leach liquor after pressure filter press filtration washing;
3. the dealkalize of secondary pickling slag is to be to carry out under 10000～12000 Ο e in magneticstrength by a step high intensity magnetic separation, must contain iron ore and mine tailing, containing iron ore, in magneticstrength, is under 9000～12000 Ο e, to carry out two step high intensity magnetic separations to obtain iron ore concentrate and chats;
4. leach liquor obtains Scium trioxide product through extraction, back extraction, sour molten hydrolysis, reextraction, removal of impurities, secondary back extraction, dissolving with hydrochloric acid, oxalic acid precipitation, calcination process;
The extraction of described leach liquor is to make extraction agent with organic phase di (isooctyl) phosphate P204, secondary octanol, sulfonated kerosene=16:4:80, in the ratio of O/A=1:8～10, leach liquor is extracted, and extraction time 20～30 minutes, obtains the organic phase of rich scandium, titanium;
Described back extraction is to make reverse-extraction agent with the NaOH that concentration is 2～2.5mol/L, 20～30 minutes back extraction time, by the scandium in rich scandium, titanium organic phase, titanium back extraction out, obtains back extraction slag;
The sulfuric acid that the molten hydrolysis of described acid is is 1.8～2.2mol/L by back extraction slag by concentration is heavy molten, add crystal seed, keep solution boiling state 2.0～3.0 hours, solution is carried out to the thermal hydrolysis of titanium, obtain metatitanic acid, metatitanic acid drying is placed in 700～850 ℃ of retort furnaces and calcines 2～3 hours, obtains titanium yellow powder after pulverizing;
Described removal of impurities is that compound concentration is the hydrochloric acid soln of 5～8mol/L, in the ratio of O/A=1～1.5:1, washs rich scandium organic phase, and washing time 10～20 minutes, washes away the impurity in organic phase;
Described secondary back extraction is that the rich scandium organic phase after removal of impurities is made reverse-extraction agent with the NaOH that concentration is 2～2.5mol/L, carries out secondary counter extraction, 20～30 minutes back extraction time, obtains secondary back extraction slag;
Described dissolving with hydrochloric acid, oxalic acid precipitation, calcination process are the dissolving with hydrochloric acid that secondary back extraction slag is 6mol/L by concentration, after dissolving, adjust pH to 1.5～2.0, be heated to 80～90 ℃, add solid oxalic acid to react, 30～60 minutes reaction times, obtain scandium throw out after filtration, washing, dry to be placed in 800 ℃ of retort furnaces and calcine 2～3 hours, obtain 98%～99% Scium trioxide product.
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| CN115057470B (en) * | 2022-08-12 | 2022-11-01 | 山西三尽材料科技有限公司 | Process for preparing metatitanic acid by using alumina red mud |
| CN115974128B (en) * | 2022-12-29 | 2024-05-14 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recycling scandium from fused salt chlorination comprehensive utilization byproducts by utilizing titanium white waste acid |
| CN115896463A (en) * | 2022-12-29 | 2023-04-04 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for extracting scandium from titanium white waste acid and titanium extraction tailings in cooperation mode |
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| US4119698A (en) * | 1976-11-26 | 1978-10-10 | Kernforschungsanlage Julich, Gesellschaft Mit Beschrankter Haftung | Reclamation treatment of red mud |
| SU1715874A1 (en) * | 1986-09-19 | 1992-02-28 | Уральский филиал Всесоюзного научно-исследовательского и проектного института алюминиевой, магниевой и электродной промышленности | Method of processing alumina production red slime |
| CN100370040C (en) * | 2006-03-17 | 2008-02-20 | 汪友华 | Method for extracting scandium from red mud |
| CN100549193C (en) * | 2007-12-08 | 2009-10-14 | 中国铝业股份有限公司 | From red mud, extract the method for metal scandium, titanium |
| CN102690962A (en) * | 2012-06-18 | 2012-09-26 | 湖南宝盈新材料有限公司 | Method for recovering scandium in waste acidic water from titanium dioxide production |
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