CN103602837A - Method for collecting scandium oxide from anatase associated scandium mineral - Google Patents
Method for collecting scandium oxide from anatase associated scandium mineral Download PDFInfo
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- CN103602837A CN103602837A CN201310509442.4A CN201310509442A CN103602837A CN 103602837 A CN103602837 A CN 103602837A CN 201310509442 A CN201310509442 A CN 201310509442A CN 103602837 A CN103602837 A CN 103602837A
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Abstract
The present invention discloses a method for collecting scandium oxide from anatase associated scandium mineral, wherein crude ore modifying and crushing, acid addition cross-flow leaching (heating and stirring), nature precipitation, supernatant extracting, replenishment of a small amount of an acid, and acid addition cross-flow leaching are performed, wherein part of the steps are repeatedly performed to increase scandium concentration in the leaching solution, and the scandium-containing mother liquid achieving the target concentration through enrichment is subjected to extraction, back extraction, precipitation and calcining to obtain high purity scandium oxide.
Description
Technical field
The invention belongs to chemical field, in particular to a kind of method of collecting Scium trioxide from anatase octahedrite association scandium ore deposit.
Background technology
The source of current domestic Scium trioxide is to extract from iron and steel tailings, flue dust or titanium pigment waste acid substantially, and source less, utilization ratio is low, and meanwhile, the grade of Scium trioxide in source, yield are unstable, and extraction conditions is harsh.In the last few years, along with the development of global materials industry, for the demand of Scium trioxide, strengthened year by year, and caused Scium trioxide price always high.It has its source in, and with regard to prior art, the extractive technique of Scium trioxide is relatively backward, and source is harsh complicated, and extraction cost is too high.
For solving from a kind of, containing directly leaching the technical problem of Scium trioxide scandium anatase octahedrite, under exacting terms, do not obtaining higher yields, be those skilled in the art's technical problem urgently to be resolved hurrily simultaneously.
Summary of the invention
The present invention relates to a kind of method of collecting Scium trioxide from anatase octahedrite association scandium ore deposit, it is characterized in that comprising the steps:
(1) raw ore is through preliminary broken, and broken median size is afterwards 20-50 order;
(2) through preliminary broken raw ore, carry out oxidizing roasting, maturing temperature is 650-750 ℃, and roasting time is 0.5-2 hour;
(3) after roasting through further pulverizing, be crushed to 90% raw ore particle diameter between 100-200 order;
(4) pulverize and add mass percent concentration to defend the acidleach of 8-12% dilution heat of sulfuric acid afterwards, acid (in 98% vitriol oil) is 1:10(mass ratio with the amount ratio of pulverized particles), in acidleach process, adopt 65-75 ℃ of steam heating, middling speed in heat-processed (40-80r/min) stirs, and churning time is 0.6-1.5 hour;
(5) pulverized particles after acidleach is transported to natural subsidence naturally cooling in settling bowl, the upper strata stillness of night filters to remove undissolved composition through further essence, lower floor obtains filtrate and filter residue containing acid leaching residue coarse filtration through filtering, filtrate is through essence filter, filter residue, through washing press filtration, is mixed to get the filtrate of three parts containing scandium filtrate;
(6) detect containing the iron level in scandium filtrate, when the content of iron is greater than 200g/L, utilize vacuum freezing crystallization to obtain ferrous sulfate crystal; When the content of iron is not more than 200g/L, adopting containing scandium filtrate replaces the dilution heat of sulfuric acid in step (4) to carry out acidleach to the raw ore after pulverizing, 98% sulfuric acid that added ore quality 5-10% before acidleach, then repeating step (4)-(6), are 50-60g scandium/ton filtrate until contain the concentration of scandium in scandium filtrate;
(7) filtrate of scandium-enriched is by extraction, and back extraction, precipitates, and calcining obtains Scium trioxide.
In a preferred embodiment of the present invention, described ferrous sulfate crystal is for the production of byproduct iron oxide red.
In a preferred embodiment of the present invention, the further preextraction anatase octahedrite of slag obtaining after the washing of the filter residue in step (5) press filtration.
In another preferred embodiment of the present invention, the Scium trioxide purity of gained 4N and more than.
In a preferred embodiment of the present invention, in described anatase octahedrite association scandium green ore, the content of TiO2 is 3-5%; The content of TiFe is 12-16%; The content of Al2O3 is 18-22%; The content of SiO2 is 35-45%; The content of Scium trioxide is 60-80g/T; The content total amount of all the other elements is less than 2%.
In another preferred embodiment of the present invention, the rate of recovery of scandium is more than 70%, preferably more than 80%.
The present invention is by this anatase octahedrite raw ore association scandium ore deposit is carried out after modification in early stage, and with a small amount of sulphuric acid soln cross-flow leaching, after heating, the solubility rate of Scium trioxide is higher, and the Scium trioxide of stripping is by several purification by liquid extraction, can obtain high-purity mangesium oxide scandium.
Because the present invention adopts cross-flow acidleach repeatedly, after the acidleach factor repeatedly that affects in leaching liquid is rejected, pickling liquor can leach repeatedly, thereby improves constantly Scium trioxide concentration in immersion liquid, has reduced cost and the technology difficulty of follow-up purification by liquid extraction and has saved sulfuric acid and water simultaneously.First main innovation part of the present invention is by modification, by a large amount of active, viscous substance modifications in mineral, suppresses " objectionable impurities " in mineral and reacts with pickling liquor, and the while has been improved the leaching yield of scandium element to a great extent.
The present invention, by suppressing the stripping of " objectionable impurities ", has simplified the composition in immersion liquid, greatly for follow-up Sc extraction work is laid a good foundation.
Accompanying drawing explanation
Fig. 1: the method schematic diagram of collecting Scium trioxide from anatase octahedrite association scandium ore deposit;
Fig. 2: the filtrate of scandium-enriched is passed through extraction, back extraction, precipitation, the processing schematic diagram of calcining: wherein extraction agent is p204(p507) and TBP.Organic phase after back extraction is by regeneration (dilution heat of sulfuric acid washing), reusable after reclaiming.Waste residue composition is the impurity such as iron, aluminium, silicon, titanium.
Specific embodiments
Raw ore is a kind of anatase octahedrite association scandium ore deposit mineral, and its results of elemental analyses is as shown in the table.
Concrete treatment process comprises the steps:
(1) raw ore is through preliminary broken, and broken median size is afterwards 20-50 order;
(2) through preliminary broken raw ore, carry out oxidizing roasting, maturing temperature is 700 ℃, and roasting time is 1 hour;
(3) after roasting through further pulverizing, be crushed to 90% raw ore particle diameter between 100-200 order;
(4) pulverize and add dilution heat of sulfuric acid (10%) acidleach afterwards, acid (in 98% vitriol oil) is 1:10(mass ratio with the amount ratio of pulverized particles), in acidleach process, adopt 70 ℃ of steam heating, middling speed in heat-processed (60r/min) stirs, and churning time is 1 hour;
(5) pulverized particles after acidleach is transported to natural subsidence in settling bowl (the not free restriction of sedimentation, is separated into standard substantially with solid-liquid.Temperature is drop temperature, naturally cooling), the upper strata stillness of night filters to remove undissolved composition through further essence, lower floor obtains filtrate and filter residue containing acid leaching residue coarse filtration through filtering, filtrate is through essence filter, filter residue, through washing (consumption of water is about 1T filter residue water consumption 1T) press filtration, is mixed to get the filtrate of three parts containing scandium filtrate; The further preextraction anatase octahedrite of slag obtaining after filter residue washing press filtration;
(6) detect containing the iron level in scandium filtrate, when the content of iron is greater than 200g/L, (vacuum tightness is 0.1MPa to utilize vacuum freezing crystallization, temperature is reduced to 10-15 ℃ from 70-80 ℃) obtain ferrous sulfate crystal, when the content of iron is not more than 200g/L, adopting containing scandium filtrate replaces the dilution heat of sulfuric acid in step (4) to carry out acidleach to the raw ore after pulverizing, the sulfuric acid that added ore quality 5-10% before I acidleach, then repeating step (4)-(6), are 50-60g scandium/ton filtrate until contain the concentration of scandium in scandium filtrate;
(7) ferrous sulfate is for the production of byproduct iron oxide red; The filtrate of scandium-enriched is by extraction, and back extraction, precipitates, and calcining (please specifically supplementing technological process and the condition of above-mentioned 4 steps), can obtain highly purified Scium trioxide, with respect to original ore deposit soil, obtains 4N high-purity mangesium oxide scandium yield and is about 70%-80%.
According to sand town, Qinglong County, Guizhou Province anatase octahedrite, scandium ore deposit, calculate, in raw ore per ton, the average grade of Scium trioxide is 70g, adopts 10T raw ore, approximately uses the 2T98% vitriol oil, can obtain 4N Scium trioxide 0.5Kg.Owing to extracting Scium trioxide in acid solution, (extraction agent can be recycled substantially can not expend extraction agent.) raw material expends and be mainly sulfuric acid.Through data, calculate, using the present invention to extract Scium trioxide and produce 4N High-purity Sc Oxide cost can be controlled between per kilogram 9000-12000 unit substantially, on (in October, 2013) market, the price maintenance of 4N Scium trioxide, at 25000-30000 unit per kilogram, is used the present invention from having very large economic worth containing leaching Scium trioxide scandium anatase octahedrite at present.
In addition, utilize method of the present invention, the yield of scandium is up to 80%, and sulfuric acid, water can farthest recycle, and meanwhile, byproduct has also been accomplished sufficient recycling, has reduced the waste of resource.
The above, be only the specific embodiment of the present invention, but protection scope of the present invention is not limited to this, and any variation of expecting without creative work or replacement, within all should being encompassed in protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain that claims were limited.
Claims (6)
1. a method of collecting Scium trioxide from anatase octahedrite association scandium ore deposit, is characterized in that comprising the steps:
(1) raw ore is through preliminary broken, and broken median size is afterwards 20-50 order;
(2) through preliminary broken raw ore, carry out oxidizing roasting, maturing temperature is 650-750 ℃, and roasting time is 0.5-2 hour;
(3) after roasting through further pulverizing, be crushed to 90% raw ore particle diameter between 100-200 order;
(4) pulverize and add mass percent concentration to defend the acidleach of 8-12% dilution heat of sulfuric acid afterwards, acid (in 98% vitriol oil) is 1:10(mass ratio with the amount ratio of pulverized particles), in acidleach process, adopt 65-75 ℃ of steam heating, middling speed in heat-processed (40-80r/min) stirs, and churning time is 0.6-1.5 hour;
(5) pulverized particles after acidleach is transported to natural subsidence naturally cooling in settling bowl, the upper strata stillness of night filters to remove undissolved composition through further essence, lower floor obtains filtrate and filter residue containing acid leaching residue coarse filtration through filtering, filtrate is through essence filter, filter residue, through washing press filtration, is mixed to get the filtrate of three parts containing scandium filtrate;
(6) detect containing the iron level in scandium filtrate, when the content of iron is greater than 200g/L, utilize vacuum freezing crystallization to obtain ferrous sulfate crystal; When the content of iron is not more than 200g/L, adopting containing scandium filtrate replaces the dilution heat of sulfuric acid in step (4) to carry out acidleach to the raw ore after pulverizing, 98% sulfuric acid that added ore quality 5-10% before acidleach, then repeating step (4)-(6), are 50-60g scandium/ton filtrate until contain the concentration of scandium in scandium filtrate;
(7) filtrate of scandium-enriched is by extraction, and back extraction, precipitates, and calcining obtains Scium trioxide.
2. method according to claim 1, described ferrous sulfate crystal is for the production of byproduct iron oxide red.
3. method according to claim 1, the further preextraction anatase octahedrite of slag obtaining after the filter residue washing press filtration in step (5).
4. according to the method described in claim 1-3 any one, the Scium trioxide purity of gained 4N and more than.
5. according to the method described in claim 1-3 any one, in described anatase octahedrite association scandium green ore, the content of TiO2 is 3-5%; The content of TiFe is 12-16%; The content of Al2O3 is 18-22%; The content of SiO2 is 35-45%; The content of Scium trioxide is 60-80g/T raw ore; The content total amount of all the other elements is less than 2%.
6. method according to claim 5, the rate of recovery of scandium is more than 70%, preferably more than 80%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106378252A (en) * | 2016-09-29 | 2017-02-08 | 中国地质科学院矿产综合利用研究所 | Beneficiation and enrichment method for primary scandium ore |
| CN106868325A (en) * | 2017-01-22 | 2017-06-20 | 北京有色金属研究总院 | A kind of method of scandium-enriched in hydrochloric acid leaching ilmenite production rich-titanium material flow |
| CN110129590A (en) * | 2019-05-29 | 2019-08-16 | 中南大学 | A method of extracting scandium from the concentrate of hornblend containing scandium |
| CN113046580A (en) * | 2021-03-12 | 2021-06-29 | 中国恩菲工程技术有限公司 | Scandium extraction pretreatment system and treatment method of scandium-containing solution |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102312090A (en) * | 2011-09-10 | 2012-01-11 | 吉林吉恩镍业股份有限公司 | Process for extracting scandium from ore containing scandium through pressure leaching |
| CN102653820A (en) * | 2012-04-24 | 2012-09-05 | 包头稀土研究院 | Method for extracting scandium from baiyuneboite tailings |
| CN103194609A (en) * | 2013-04-23 | 2013-07-10 | 桃江瑞龙金属新材料有限责任公司 | Method for preparing scandium oxide by using rough scandium extracted from waste acid water of titanium dioxide as raw material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102312090A (en) * | 2011-09-10 | 2012-01-11 | 吉林吉恩镍业股份有限公司 | Process for extracting scandium from ore containing scandium through pressure leaching |
| CN102653820A (en) * | 2012-04-24 | 2012-09-05 | 包头稀土研究院 | Method for extracting scandium from baiyuneboite tailings |
| CN103194609A (en) * | 2013-04-23 | 2013-07-10 | 桃江瑞龙金属新材料有限责任公司 | Method for preparing scandium oxide by using rough scandium extracted from waste acid water of titanium dioxide as raw material |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106378252A (en) * | 2016-09-29 | 2017-02-08 | 中国地质科学院矿产综合利用研究所 | Beneficiation and enrichment method for primary scandium ore |
| CN106868325A (en) * | 2017-01-22 | 2017-06-20 | 北京有色金属研究总院 | A kind of method of scandium-enriched in hydrochloric acid leaching ilmenite production rich-titanium material flow |
| CN106868325B (en) * | 2017-01-22 | 2019-06-18 | 北京有色金属研究总院 | A kind of method that hydrochloric acid leaching ilmenite produces scandium-enriched in rich-titanium material process |
| CN110129590A (en) * | 2019-05-29 | 2019-08-16 | 中南大学 | A method of extracting scandium from the concentrate of hornblend containing scandium |
| CN113046580A (en) * | 2021-03-12 | 2021-06-29 | 中国恩菲工程技术有限公司 | Scandium extraction pretreatment system and treatment method of scandium-containing solution |
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