CN104120268A - Method for extracting scandium from waste titanium dioxide acid and bayer method red mud in normal pressure at low temperature - Google Patents
Method for extracting scandium from waste titanium dioxide acid and bayer method red mud in normal pressure at low temperature Download PDFInfo
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- CN104120268A CN104120268A CN201410376603.1A CN201410376603A CN104120268A CN 104120268 A CN104120268 A CN 104120268A CN 201410376603 A CN201410376603 A CN 201410376603A CN 104120268 A CN104120268 A CN 104120268A
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Abstract
The invention discloses a method for extracting scandium from waste titanium dioxide acid and bayer method red mud in normal pressure at low temperature. The method comprises the following steps: transforming bayer method red mud in a solution in normal pressure at low temperature, reacting transformed pulp with the waste titanium dioxide acid, filtering, conveying the residue to a residue pile for storage, adding an active agent liquid into the acid filtrate to activate, filtering, and performing procedures such as organic phase extraction, alkali liquid reverse extraction, acid solution hydrolysis, secondary extraction, decontamination, secondary reverse extraction, dissolving in hydrochloric acid, deposition in oxalic acid and calcining in oxalic acid on the filtrate, thereby obtaining a scandium oxide product. By adopting the method, waste titanium dioxide acid and bayer method red mud can be treated together, the waste is treated by waste, the waste is turned into wealth, the comprehensive recycling of the two main pollutants, namely, waste titanium dioxide acid and bayer method red mud is achieved, and the scandium element and the titanium dioxide in the components are mainly recycled.
Description
Technical field
The present invention relates to chemical industry metallurgical technical field, specifically under a kind of atmospheric low-temperature, from titanium white waste acid and Bayer process red mud, extract the method for scandium.
Background technology
Scandium is described as new millennium strategy element.Be widely used in the fields such as national defence, space flight, nuclear technique, laser, electronics, metallurgy, chemical industry, glass, computer power supply, superconduction and medical science, and tellurian scandium resource-constrained.
China has approximately 1,000 ten thousand tons of titanium dioxide production capacities of annual output at present, and the titanium white production producer overwhelming majority adopts this traditional processing technology of sulfuric acid process, it is 6～8 tons of 15～20% titanium white waste acids that 1 ton of titanium dioxide of every production will produce concentration, titanium white waste acid scandium content, about 5～25mg/L, has the value of recycling.Up to the present, the existing processing titanium white waste acid of most of producers is all to adopt in the alkaline matters such as lime, carbide slag and the mode such as discharge, and treatment cost is higher, and secondary pollution is serious, fails fundamentally to solve the problem of outlet of titanium white waste acid.
China is alumina producing big country, and the Guangxi large province of alumina producing (district) especially, built have produce per year 9,000,000 tons of alumina producing devices, millions of tons of Bayer process red muds of annual generation, store up in stockyard in the open over the years, pile up at present store content huge, very easily periphery water resources and soil are polluted and destroyed, and the potential safety hazard that leaks of the red mud that lies dormant.In Bayer process red mud, except the metallic element such as iron content, aluminium, also containing multiple valuable component as rare metals such as titanium, scandium, rare earths, is a kind of abundant secondary resource.Therefore, accelerating the resource utilization recycling of Bayer process red mud, is the important channel of realizing sustainable development of alumina industry, significant to building a resource-conserving society.
For the research of reclaiming the comprehensive utilizations such as scandium, titanium, sulfuric acid from titanium white waste acid, and for the research of reclaiming the comprehensive utilizations such as scandium, aluminium from Bayer process red mud, forefathers have designed multiple different technique circuit and have done a large amount of research work, have also obtained certain useful achievement.But, no matter reclaiming scandium from Bayer process red mud, or reclaim scandium from titanium white waste acid, its technique all requires cost rationally and needs to solve the final environmental issue of spent acid or red mud, not so in industrial application, all cannot carry out or cannot long-time running.
Summary of the invention
The object of the present invention is to provide a kind of extract scandium under atmospheric low-temperature from titanium white waste acid and Bayer process red mud method.By red mud being carried out to spent acid leaching under atmospheric low-temperature, at titanium white waste acid and Bayer process red mud carries out acid-base neutralisation and by effective scandium leaching process, can control preferably the solubility rate of detrimental impurity in red mud, realize the recycling of the comprehensive regulation of titanium white waste acid and Bayer process red mud two large industrial pollution sources and scandium, titanium.
For achieving the above object, technical scheme of the present invention is: under a kind of atmospheric low-temperature, from titanium white waste acid and Bayer process red mud, extract the method for scandium, comprise the steps:
(1) red mud transforms
In device has the acid-proof reaction groove of mechanical stirrer, add size mixing after Bayer process red mud, under stirring, slowly add water and titanium white waste acid, additional proportion is red mud: water: spent acid=1:2～6:0.8～1.2; Temperature of reaction is 20～45 DEG C, after 40～50 minutes reaction times, filters, and transforms a filtrate part and returns to uses of sizing mixing of red mud of lower cycle, and conversion slag enters step (2);
(2) acid-leaching reaction
In device has the acid-proof reaction groove of mechanical stirrer, add and transform slag and add after aquation slurry, under stirring, slowly inject titanium white waste acid by 10ml/min, additional proportion is red mud: water: spent acid=1:1:2.8; Temperature of reaction is 20～45 DEG C, reacts after 60～80 minutes and filters, the leach liquor that must be 10～15mg/L containing scandium; Acidleach residue send slag field to store up;
(3) activation treatment
In leach liquor: activator liquid=10:1 ratio, add toward leaching in filtrate the activator liquid containing polyethers 0.5～5% preparing, under normal temperature, stir after 30 minutes and filter, after filtering, residue send slag field to store up, and after activation, filtrate is sent to extraction;
(4) organic extractant phase
Organic extractant phase is with di-(2-ethylhexyl)phosphoric acid (P204), methyl phenyl ketone, 260
#sulfonated kerosene=16:4:80 makes organic extractant, in the ratio of O/A=1:5～10, activation filtrate is extracted, and extraction time 10～30 minutes, obtains being rich in scandium, titanium organic phase;
(5) alkali lye back extraction
NaOH solution using concentration as 2～3.5mol/L is as strip liquor, with mixing containing adding in back extraction case together with scandium, titanium organic phase of above-mentioned steps (4) gained, 20～30 minutes back extraction time is separated scandium, titanium from organic phase, and obtaining back extraction slag is scandium, titanium enriched substance;
(6) acid-soluble hydrolysis
The dissolve with hydrochloric acid solution back extraction slag that the acid-soluble hydrolysis of back extraction slag is is under agitation 1.5～3mol/L by concentration, keep 100～105 DEG C of boilings of solution 2.0～3.0 hours, titanium in solution is carried out after thermal hydrolysis is realized the separation of scandium titanium obtaining rich titanium slag, rich titanium slag is as the raw material that reclaims titanium dioxide, and the scandium solution that contains after heavy titanium is used as extraction fluid;
(7) reextraction
Reextraction is with di-(2-ethylhexyl)phosphoric acid (P204), 260
#sulfonated kerosene=20:80 makes organic extractant, and in the ratio of O/A=1:8～10, to sinking extracting containing scandium solution after titanium, extraction time 10～30 minutes, obtains being rich in scandium organic phase;
(8) removal of impurities
Removal of impurities is that compound concentration is the hydrochloric acid soln of 5～10mol/L, is rich in scandium organic phase in the ratio washing of O/A=1～1.5:1, washing time 10～20 minutes, and the impurity in organic phase is removed in eccysis, obtains impure few rich scandium organic phase;
(9) secondary back extraction
The NaOH solution that rich scandium organic phase after removal of impurities is 2～3.5mol/L by concentration is made reverse-extraction agent, carries out secondary counter extraction, 20～30 minutes back extraction time, obtains secondary back extraction slag.
(10) dissolving with hydrochloric acid-oxalic acid precipitation-calcining
Compound concentration is the dissolve with hydrochloric acid solution secondary back extraction slag of 6mol/L, after dissolving, adjust pH to 1.5～2.5, be heated to 60～90 DEG C, add solid oxalic acid to carry out precipitin reaction, 30～60 minutes reaction times, obtain oxalic acid scandium throw out after filtration, washing, dry and be placed in 800～900 DEG C of retort furnaces and calcine 2～3 hours, obtain the Scium trioxide of purity > 93%.
The outstanding beneficial effect of the present invention is:
Under atmospheric low-temperature, the sulfuric acid making full use of in titanium white waste acid is removed the alkali in Bayer process red mud, and in acid-base reaction simultaneously, realizes the extraction of combining of scandium in scandium and the Bayer process red mud in titanium pigment waste acid.Do like this and on the one hand solved Bayer process red mud and put forward separately the too high problem of scandium production cost; Utilize on the other hand the alkalescence of Bayer process red mud and the acidity of titanium white waste acid liquid to neutralize the environment protection emission problem that solves both, the treatment of wastes with processes of wastes against one another, energy-conserving and environment-protective; Make the comprehensive reutilization of titanium white waste acid and Bayer process red mud in suitability for industrialized production, become simple possible.
Brief description of the drawings
Fig. 1 is the process flow sheet that extracts the method for scandium under atmospheric low-temperature of the present invention from titanium white waste acid and Bayer process red mud.
Embodiment
By the following examples technical scheme of the present invention is further described.
Embodiment 1
At 1m
3in retort, add the 300L water of sizing mixing, start mechanical stirring and gradually 100kg granular red mud added, then add 300 liters, water, add 120 liters, spent acid, under normal pressure, 25 DEG C of conditions, transform 40 minutes, then filter.Filter residue adds 1m
3after retort, add 100 premium on currency, start and stir after pulp, add 280 liters, spent acid by 10 liters/min of speed, react 65 minutes, after filtration, filtrate adds 38 liters of activator liquid, stirring reaction 30 minutes, filter, filtrate extracts, and back extraction is dissolved and removes titanium 2 hours 100 DEG C of hydrolysis, after filtering, filtrate is carried out reextraction, back extraction again after washing impurity-removing, back extraction slag dissolves with 6mol/L hydrochloric acid again, and filtrate adds oxalic acid precipitation at 65 DEG C, throw out adds after water washing 850 DEG C of calcinings, obtains the scandium oxide of purity 93.9%.
Embodiment 2
At 1m
3in retort, add the 300L water of sizing mixing, start mechanical stirring and gradually 100kg granular red mud added, then add 300 liters, water, add 120 liters, spent acid, under normal pressure, 30 DEG C of conditions, transform 40 minutes, then filter.Filter residue adds 1m
3after retort, add 100 premium on currency, start and stir after pulp, add 280 liters, spent acid by 10 liters/min of speed, react 65 minutes, after filtration, filtrate adds 38 liters of activator liquid, stirring reaction 30 minutes, filter, filtrate extracts, and back extraction is dissolved and removes titanium 2 hours 100 DEG C of hydrolysis, after filtering, filtrate is carried out reextraction, back extraction again after washing impurity-removing, back extraction slag dissolves with 6mol/L hydrochloric acid again, and filtrate adds oxalic acid precipitation at 65 DEG C, throw out adds after water washing 860 DEG C of calcinings, obtains the scandium oxide of purity 95.2%.
Embodiment 3
At 1m
3in retort, add the 300L water of sizing mixing, start mechanical stirring and gradually 100kg granular red mud added, then add 300 liters, water, add 120 liters, spent acid, under normal pressure, 38 DEG C of conditions, transform 40 minutes, then filter.Filter residue adds 1m
3after retort, add 100 premium on currency, start and stir after pulp, add 280 liters, spent acid by 10 liters/min of speed, react 65 minutes, after filtration, filtrate adds 38 liters of activator liquid, stirring reaction 30 minutes, filter, filtrate extracts, and back extraction is dissolved and removes titanium 2 hours 102 DEG C of hydrolysis, after filtering, filtrate is carried out reextraction, back extraction again after washing impurity-removing, back extraction slag dissolves with 6mol/L hydrochloric acid again, and filtrate adds oxalic acid precipitation at 70 DEG C, throw out adds after water washing 880 DEG C of calcinings, obtains the scandium oxide of purity 95.6%.
Embodiment 4
At 1m
3in retort, add the 300L water of sizing mixing, start mechanical stirring and gradually 100kg granular red mud added, then add 300 liters, water, add 120 liters, spent acid, under normal pressure, 42 DEG C of conditions, transform 40 minutes, then filter.Filter residue adds 1m
3after retort, add 100 premium on currency, start and stir after pulp, add 280 liters, spent acid by 10 liters/min of speed, react 70 minutes, after filtration, filtrate adds 38 liters of activator liquid, stirring reaction 30 minutes, filter, filtrate extracts, and back extraction is dissolved and removes titanium 2 hours 102 DEG C of hydrolysis, after filtering, filtrate is carried out reextraction, back extraction again after washing impurity-removing, back extraction slag dissolves with 6mol/L hydrochloric acid again, and filtrate adds oxalic acid precipitation at 75 DEG C, throw out adds after water washing 880 DEG C of calcinings, obtains the scandium oxide of purity 95.3%.
Embodiment 5
At 1m
3in retort, add the 300L water of sizing mixing, start mechanical stirring and gradually 100kg granular red mud added, then add 300 liters, water, add 120 liters, spent acid, under normal pressure, 42 DEG C of conditions, transform 40 minutes, then filter.Filter residue adds 1m
3after retort, add 100 premium on currency, start and stir after pulp, add 280 liters, spent acid by 10 liters/min of speed, react 80 minutes, after filtration, filtrate adds 38 liters of activator liquid, stirring reaction 30 minutes, filter, filtrate extracts, and back extraction is dissolved and removes titanium 2 hours 103 DEG C of hydrolysis, after filtering, filtrate is carried out reextraction, back extraction again after washing impurity-removing, back extraction slag dissolves with 6mol/L hydrochloric acid again, and filtrate adds oxalic acid precipitation at 75 DEG C, throw out adds after water washing 900 DEG C of calcinings, obtains the scandium oxide of purity 96.2%.
Claims (3)
1. a method of extracting scandium under atmospheric low-temperature from titanium white waste acid and Bayer process red mud, is characterized in that, comprises the steps:
(1) red mud transforms
In device has the acid-proof reaction groove of mechanical stirrer, add the Bayer process red mud after sizing mixing, under stirring, slowly adding water and titanium white waste acid, additional proportion is red mud: water: spent acid=1:2～6:0.8～1.2; Temperature of reaction is 20～45 DEG C, after 40～50 minutes reaction times, filters, and transforms a filtrate part and returns to uses of sizing mixing of red mud of lower cycle, and conversion slag enters step (2);
(2) acid-leaching reaction
In device has the acid-proof reaction groove of mechanical stirrer, add and transform slag and add after aquation slurry, under stirring, slowly inject titanium white waste acid by 10ml/min, additional proportion is red mud: water: spent acid=1:1:2.8; Temperature of reaction is 20～45 DEG C, reacts after 60～80 minutes and filters, the leach liquor that must be 10～15mg/L containing scandium; Acidleach residue send slag field to store up;
(3) activation treatment
In leach liquor: activator liquid=10:1 ratio, in leach liquor, add the activator liquid containing polyethers 0.5～5%, under normal temperature, stir after 30 minutes and filter, after filtering, residue send slag field to store up, and activation filtrate is sent to extraction;
(4) organic extractant phase
Organic extractant phase is with di-(2-ethylhexyl)phosphoric acid (P204), methyl phenyl ketone, 260
#sulfonated kerosene=16:4:80 makes organic extractant, in the ratio of O/A=1:5～10, activation filtrate is extracted, and extraction time 10～30 minutes, obtains being rich in scandium, titanium organic phase;
(5) alkali lye back extraction
NaOH solution using concentration as 2～3.5mol/L is as strip liquor, with mixing containing adding in back extraction case together with scandium, titanium organic phase of above-mentioned steps (4) gained, 20～30 minutes back extraction time is separated scandium, titanium from organic phase, and obtaining back extraction slag is scandium, titanium enriched substance;
(6) acid-soluble hydrolysis
The dissolve with hydrochloric acid solution back extraction slag that the acid-soluble hydrolysis of back extraction slag is is under agitation 1.5～3mol/L by concentration, keep 100～105 DEG C of boilings of solution 2.0～3.0 hours, titanium in solution is carried out after thermal hydrolysis is realized the separation of scandium titanium obtaining rich titanium slag, rich titanium slag is as the raw material that reclaims titanium dioxide, and the scandium solution that contains after heavy titanium is used as extraction fluid;
(7) reextraction
Reextraction is with di-(2-ethylhexyl)phosphoric acid (P204), 260
#sulfonated kerosene=20:80 makes organic extractant, and in the ratio of O/A=1:8～10, to sinking extracting containing scandium solution after titanium, extraction time 10～30 minutes, obtains being rich in scandium organic phase;
(8) removal of impurities
Removal of impurities is that compound concentration is the hydrochloric acid soln of 5～10mol/L, is rich in scandium organic phase in the ratio washing of O/A=1～1.5:1, washing time 10～20 minutes, and the impurity in organic phase is removed in eccysis, obtains impure few rich scandium organic phase;
(9) secondary back extraction
The NaOH solution that rich scandium organic phase after removal of impurities is 2～3.5mol/L by concentration is made reverse-extraction agent, carries out secondary counter extraction, 20～30 minutes back extraction time, obtains secondary back extraction slag;
(10) dissolving with hydrochloric acid-oxalic acid precipitation-calcining
Compound concentration is the dissolve with hydrochloric acid solution secondary back extraction slag of 6mol/L, after dissolving, adjust pH to 1.5～2.5, be heated to 60～90 DEG C, add solid oxalic acid to carry out precipitin reaction, 30～60 minutes reaction times, obtain oxalic acid scandium throw out after filtration, washing, dry and be placed in 800～900 DEG C of retort furnaces and calcine 2～3 hours, obtain the Scium trioxide of purity > 93%.
2. the method for extracting scandium under atmospheric low-temperature according to claim 1 from titanium white waste acid and Bayer process red mud, is characterized in that: the temperature of reaction of step (1), (2) is to carry out at 25～33 DEG C.
3. under atmospheric low-temperature according to claim 1, from titanium white waste acid and Bayer process red mud, extract the method for scandium, it is characterized in that: the pickling liquor of step (3) need first add i.e. 0.5～5% polyethers solution activation treatment of activator liquid, then carries out scandium extraction.
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Cited By (7)
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| CN104498723A (en) * | 2014-12-16 | 2015-04-08 | 湖南稀土金属材料研究院 | Method for extracting scandium oxide from titanium slag chlorinated waste salt |
| CN104651619A (en) * | 2015-03-17 | 2015-05-27 | 湖南东方钪业股份有限公司 | Method for separating and recovering scandium in stable zirconia ceramic wastes containing scandium and rare earth |
| CN108722422A (en) * | 2017-04-21 | 2018-11-02 | 中国石油化工股份有限公司 | A kind of method of red mud activation modification and application |
| CN109280770A (en) * | 2018-11-27 | 2019-01-29 | 中南大学 | A method of recycling scandium and titanium from the immersion liquid of metatitanic acid containing scandium |
| CN109563566A (en) * | 2016-08-30 | 2019-04-02 | 住友金属矿山株式会社 | The recovery method of scandium |
| CN110358937A (en) * | 2019-07-02 | 2019-10-22 | 广西大学 | A method of the selective enrichment scandium from titanium white waste acid and red mud |
| CN110436600A (en) * | 2019-08-21 | 2019-11-12 | 天津理工大学 | A kind of method that red mud disposes production Ti-enriched slag and water purification agent with ferrous waste acid jointly |
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| CN104498723A (en) * | 2014-12-16 | 2015-04-08 | 湖南稀土金属材料研究院 | Method for extracting scandium oxide from titanium slag chlorinated waste salt |
| CN104651619A (en) * | 2015-03-17 | 2015-05-27 | 湖南东方钪业股份有限公司 | Method for separating and recovering scandium in stable zirconia ceramic wastes containing scandium and rare earth |
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| CN108722422A (en) * | 2017-04-21 | 2018-11-02 | 中国石油化工股份有限公司 | A kind of method of red mud activation modification and application |
| CN108722422B (en) * | 2017-04-21 | 2020-10-30 | 中国石油化工股份有限公司 | Red mud activation modification method and application |
| CN109280770A (en) * | 2018-11-27 | 2019-01-29 | 中南大学 | A method of recycling scandium and titanium from the immersion liquid of metatitanic acid containing scandium |
| CN110358937A (en) * | 2019-07-02 | 2019-10-22 | 广西大学 | A method of the selective enrichment scandium from titanium white waste acid and red mud |
| CN110436600A (en) * | 2019-08-21 | 2019-11-12 | 天津理工大学 | A kind of method that red mud disposes production Ti-enriched slag and water purification agent with ferrous waste acid jointly |
| CN110436600B (en) * | 2019-08-21 | 2022-04-01 | 天津理工大学 | Method for producing titanium-rich slag and water purifying agent by jointly treating red mud and iron-containing waste acid |
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Application publication date: 20141029 |