CN102690962A - Method for recovering scandium in waste acidic water from titanium dioxide production - Google Patents
Method for recovering scandium in waste acidic water from titanium dioxide production Download PDFInfo
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- CN102690962A CN102690962A CN2012101992467A CN201210199246A CN102690962A CN 102690962 A CN102690962 A CN 102690962A CN 2012101992467 A CN2012101992467 A CN 2012101992467A CN 201210199246 A CN201210199246 A CN 201210199246A CN 102690962 A CN102690962 A CN 102690962A
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Abstract
The invention discloses a method for recovering scandium in waste acidic water from titanium dioxide production, which is simple in washing liquid preparation and convenient to use. The method is characterized by comprising the following steps of extraction, washing, back extraction, acidic dissolution, oxalic acid precipitation and scorching. The method is simple in process and convenient to operate, dilute sulphuric acid and hydrogen peroxide are respectively added in a cascade washing process, so that the washing liquid is maintained at a certain temperature to facilitate titanium elution in the washing process, and the hydrogen peroxide is prevented from being decomposed massively at high temperature in an acidic medium, meanwhile, in several stages after feeding of hydrogen peroxide, an organic phase washed with hydrogen peroxide is further washed with pure sulphuric acid, and free hydrogen peroxide is washed for recycle so as to reduce the loss of hydrogen peroxide; and in addition, in the back extraction process, a back extraction solution is retained in a reaction kettle for repeated back extraction, so that the frequency of filter pressing is reduced, a process is simplified and the loss of Sc is reduced.
Description
Technical field
The present invention relates to a kind of recovery method of REE scandium, the recovery method of scandium in specifically a kind of Producing Titanium Dioxide waste acid water.
Background technology
Scandium belongs to a kind of in the REE, and few at the content of occurring in nature, the content of scandium in the earth's crust has only 5 * 10
-6, not only compare and will hang down much with other light elements, content also only belongs to mediumly in whole REE, probably has only 1/10 of cerium.And the purposes of scandium is very extensive, as be used to have economize on electricity, long service life, the broken scandium sodium vapor lamp that the mist ability is strong, luminous efficiency is good, be used for solar photocell, gamma ray projector and be used for alloy material aspect, organic chemistry additive or the like.Because its content is rare, so extraction process is very complicated, and cost is higher, so price is also expensive, just uses as additive in most fields, is described as magical condiment.
The extraction of scandium had had many research from last century since the eighties, mainly be from other mineral, to propose as a kind of by product, like rare-earth mineral, schreyerite, ilmenite, bauxite and tungsten ore etc.
It mainly all is to use sulfuric acid process that China's titanium powder plant is produced white titanium pigment, and the spent acid amount that one ton of white titanium pigment of every production produces is 5m
3～6m
3, wherein contain the Sc amount and be 10g/ m
3～20 g/ m
3, per ten thousand tons of white titanium pigments can produce the spent acid that contains 500 ㎏～1200 ㎏ Sc, have considerable recovery value.The recovery technology of existing Sc has repeatedly transfers pH value that scandium hydrolysis-acid is dissolved-hydrolysis; Reach the progressively purpose of separating impurity; This method impurity separation efficiency is low; Scium trioxide purity after the process multistep is separated, repeatedly oxalic acid precipitation is purified is low, and because Scium trihydroxide and oxalic acid scandium all have certain solubleness, certainly will cause damage.For reclaiming trace element, be higher in the similar technology with the recovery of extraction process.Like number of patent application is 201010230723.2, and publication number is CN 102127641A, and the applying date is 2010.07.20, and denomination of invention is that the recovery method of scandium titanium in the titanium dioxide wastewater discloses a kind of scandium that adopts in the extraction process recovery titanium white waste acid.Its process step is steps such as extraction, back extraction, acid are dissolved, purification; This method because after the extraction not through washing, titanium content is too high in the load organic phases, and the titanium particle that goes out of hydrolysis is too thin with this understanding, cause filter or speed of filter pressing extremely slow, not easy to operate, and product purity is low.
Number of patent application is 200610054136.6, and publication number is CN 1844421A, and the applying date is 2006.03.17, and the method for extracting scandium of denomination of invention red mud discloses a kind of employing extraction-washing-back extraction-acid and dissolved-sedimentary method for extracting scandium.Washing step adopts sulfuric acid and ydrogen peroxide 50 is mixed with the method for carrying out the single-stage washing after the washing lotion in its technology.Because in the process of preparation dilute sulphuric acid, a large amount of heat releases of meeting if add ydrogen peroxide 50 this moment, certainly will cause the pyrolytic decomposition of ydrogen peroxide 50, therefore, must treat to add ydrogen peroxide 50 after the dilute sulphuric acid cooling.Like this, the washing lotion preparation is trouble, and the heat that can not effectively utilize dilute sulphuric acid in process for preparation, to be produced.
Summary of the invention
The recovery method that the purpose of this invention is to provide scandium in a kind of washing lotion preparation Producing Titanium Dioxide waste acid water simple, easy to use.
The present invention adopts following technical scheme to realize its goal of the invention, and its process step is that cascade extraction-tandem washing-back extraction-acid is dissolved-oxalic acid precipitation-calcination.Adopt cascade extraction to reclaim the scandium in the spent acid, classification adds dilute sulphuric acid and ydrogen peroxide 50, the impurity such as titanium in the wash-out organic phase in the tandem washing process.Simultaneously, the organic phase after the washing is carried out the single-stage back extraction, and strip liquor is kept somewhere recycling in the reaction kettle.
The recovery method of scandium in a kind of Producing Titanium Dioxide waste acid water, it may further comprise the steps:
⑴ extraction: in extraction tank, adopt P204-TBP-kerosene extraction agent through 3 grades～6 grades cascade extractions to the Producing Titanium Dioxide waste acid water, the volume ratio of extraction agent and spent acid is 1:5～30, and mixing time is 10min～30min, and the scandium percentage extraction is 90 ﹪～99 ﹪;
⑵ washing: the load organic phases that step ⑴ is obtained uses the sulfuric acid of 1mol/L～3mol/L and ydrogen peroxide 50 that concentration is 27 ﹪ to be washing composition; Through 10 grades～20 grades tandem washings; Load organic phases and vitriolic volume ratio are 1:1/3～3, and the ydrogen peroxide 50 add-on is 1 ﹪～10 ﹪ of sulfuric acid volume, first step loading organic phase; Last step adds sulfuric acid, adds ydrogen peroxide 50 at penultimate stage one or more levels in to the 8th grade reciprocal;
⑶ back extraction: toward the interior sodium hydroxide solution that adds 1mol/L～4mol/L of reaction kettle; Be warming up to 40 ℃～80 ℃; The load organic phases that step ⑵ obtains is sent into reaction kettle, and the volume ratio of load organic phases and sodium hydroxide solution is 1:1/2～3, stirs back extraction; Time is 10 min～30min, clarification;
⑷ acid is dissolved: the strip liquor that step ⑶ is obtained is crossed and is filtered rich scandium alkali cake, and rich scandium alkali cake dissolves in the reaction kettle internal heating with 1mol/L～6mol/L sulfuric acid or hydrochloric acid, and boils the abundant hydrolysis of titanium is separated out, and press filtration gets scandium sulfate or Scium trichloride solution;
⑸ oxalic acid precipitation: the solution that step ⑷ is obtained precipitates with 1 ﹪～5 ﹪ oxalic acid solutions, gets granular oxalic acid scandium;
⑹ calcination: the oxalic acid scandium that step ⑸ is obtained is in 800 ℃～1000 ℃ following calcinations, purity be the Scium trioxide of 99.0 ﹪～99.99 ﹪.
The present invention makes full use of excessive ydrogen peroxide 50, in step ⑵, between penultimate stage is to the 8th grade reciprocal, adds ydrogen peroxide 50 at interval.
The present invention is for reducing the number of times of press filtration, and in step ⑶, after the clarification, upper blank organic phase in the siphon reaction kettle continues in reaction kettle, to add the load organic phases with blank organic equal volume, and repeating step ⑶ 2 times～5 times.
Because adopt technique scheme, the present invention has realized goal of the invention preferably, its technology is simple, and is easy to operate; Add dilute sulphuric acid and ydrogen peroxide 50 in the tandem washing process respectively, not only make washing lotion keep certain temperature to help the wash-out of titanium in the washing process, avoided a large amount of decomposition of ydrogen peroxide 50 in high temperature and acidic medium, simultaneously; After the ydrogen peroxide 50 charging what, the organic phase after ydrogen peroxide 50 washing has been passed through the bright sulfur acid elution again, and the free ydrogen peroxide 50 is washed recycling; Reduced the loss of ydrogen peroxide 50, and in the back extraction process, strip liquor is kept somewhere repetition back extraction in the reaction kettle; Reduce the number of times of press filtration, simplified technology, reduced the loss of Sc.
Embodiment
Below in conjunction with embodiment the present invention is described further.
Embodiment 1:
The recovery method of scandium in a kind of Producing Titanium Dioxide waste acid water, it may further comprise the steps:
⑴ extraction: it is 15.68 ㎎/L that the raw material titanium white waste acid contains scandium concentration; In extraction tank, adopt two (2-ethylhexyl phosphoric acid) P204-tributyl phosphate TBP-kerosene extraction agent through 3 grades～6 grades (present embodiment is 3 grades) cascade extractions to the Producing Titanium Dioxide waste acid water, by volume is calculated, and P204 is 6 ﹪～15 ﹪ (present embodiment is 6 ﹪); TBP is 4 ﹪～6 ﹪ (present embodiment is 6 ﹪); All the other are kerosene, and the volume ratio of extraction agent and spent acid is 1:5～30, (present embodiment is 1:10); Mixing time is 10min～30min (present embodiment is 10min); It is 0.83 ㎎/L that raffinate contains scandium, and the scandium percentage extraction is 90 ﹪～99 ﹪ (present embodiment is 94.7 ﹪), obtains containing the load organic phases of scandium;
⑵ washing: the load organic phases that step ⑴ is obtained is a washing composition with the ydrogen peroxide 50 that sulfuric acid and the concentration of 1mol/L～3mol/L (present embodiment is 2mol/L) is 27 ﹪; Through 10 grades～20 grades (present embodiment is 10 grades) tandem washings; Load organic phases and vitriolic volume ratio are 1:1/3～3 (present embodiment is 1:1); The ydrogen peroxide 50 add-on is 1 ﹪～10 ﹪ (present embodiment is 5 ﹪) of sulfuric acid volume; First step loading organic phase, last step adds sulfuric acid, adds ydrogen peroxide 50 (present embodiment adds ydrogen peroxide 50 in level third from the bottom) at penultimate stage one or more levels in to the 8th grade reciprocal; Survey TiO in the surplus liquid of the first step
2Concentration is 6.18g/L, and the titanium eluting rate is 85.8 ﹪;
⑶ back extraction: toward the interior sodium hydroxide solution that adds 1mol/L～4mol/L (present embodiment is 2mol/L) of reaction kettle; Be warming up to 40 ℃～80 ℃ (present embodiment is 40 ℃); The load organic phases that step ⑵ obtains is sent into reaction kettle, and the volume ratio of load organic phases and sodium hydroxide solution is 1:1/2～3 (present embodiment is 1:1/2), stirs back extraction; Time is 10 min～30min (present embodiment is 20min), clarification;
The present invention is the number of times of minimizing press filtration, and in step ⑶, after the clarification, upper blank organic phase in the siphon reaction kettle continues toward the load organic phases of the interior adding of reaction kettle with blank organic equal volume, and repeating step ⑶ 2 times～5 times (present embodiment is 2 times);
⑷ acid is dissolved: the strip liquor that step ⑶ is obtained is crossed and is filtered rich scandium alkali cake; Rich scandium alkali cake dissolves in the reaction kettle internal heating with 1mol/L～6mol/L (present embodiment is 1mol/L) sulfuric acid or hydrochloric acid (present embodiment is a sulfuric acid); And boil the abundant hydrolysis of titanium is separated out, press filtration gets scandium sulfate or Scium trichloride solution (present embodiment is a scandium sulfate solution);
⑸ oxalic acid precipitation: the solution that step ⑷ is obtained precipitates with 1 ﹪～5 ﹪ (present embodiment is 5 ﹪) oxalic acid solution, gets granular oxalic acid scandium;
⑹ calcination: with oxalic acid scandium calcination under 800 ℃～1000 ℃ (present embodiment is 900 ℃) that step ⑸ obtains, getting purity is the Scium trioxide of 99.0 ﹪～99.99 ﹪ (present embodiment is 99.9 ﹪).
The present invention is employed in the mode that washing section adds dilute sulphuric acid and ydrogen peroxide 50 respectively, has both simplified the washing lotion process for preparation, has effectively utilized the heat that produces in the dilute sulphuric acid process for preparation again; Use the ydrogen peroxide 50 of minute quantity simultaneously, wash-out the impurity of 70 ﹪～90 ﹪, and in the back extraction process; The washing lotion recycling; Press filtration again after the extraction has repeatedly reduced the number of times of press filtration, has also reduced the loss of scandium.
Embodiment 2:
In step ⑵; To use 2mol/L sulfuric acid and concentration be that the ydrogen peroxide 50 of 27 ﹪ is washing composition to the scandium load organic phases that contains that step ⑴ is obtained; Through 15 grades of tandem washings, load organic phases and vitriolic volume ratio are 1:1/2, and the ydrogen peroxide 50 add-on is 4 ﹪ of sulfuric acid volume; First step loading organic phase, last step adds sulfuric acid; For avoiding the decomposition of ydrogen peroxide 50 in the whipping process; The present invention is multistage adding ydrogen peroxide 50 between penultimate stage is to the 8th grade reciprocal; Simultaneously, for making full use of excessive ydrogen peroxide 50, the present invention adds ydrogen peroxide 50 at interval between penultimate stage is to the 8th grade reciprocal; Present embodiment adds ydrogen peroxide 50 for the 6th grade at fourth from the last level, inverse, surveys TiO in the surplus liquid of the first step
2Concentration is 5.87g/L, and eluting rate is 81.5 ﹪;
In step ⑶, in reaction kettle, add the 2.5mol/L sodium hydroxide solution, be warming up to 50 ℃; The load organic phases that step ⑵ obtains is sent into reaction kettle, and the volume ratio of load organic phases and sodium hydroxide solution is 1:2, stirs back extraction 20min; Reduce the number of times of press filtration, after the clarification, upper blank organic phase in the siphon reaction kettle; Continue in reaction kettle, to add the load organic phases with blank organic equal volume, and repeating step ⑶ 3 times;
Surplus with embodiment 1.
Embodiment 3:
In step ⑷, the strip liquor that step ⑶ is obtained is crossed and is filtered rich scandium alkali cake, and rich scandium alkali cake, and boils the abundant hydrolysis of titanium is separated out in the dissolving of reaction kettle internal heating with the hydrochloric acid of 2mol/L, and press filtration gets Scium trichloride solution;
Surplus with embodiment 1.
Claims (3)
1. the recovery method of scandium in the Producing Titanium Dioxide waste acid water is characterized in that it may further comprise the steps:
⑴ extraction: in extraction tank, adopt P204-TBP-kerosene extraction agent through 3 grades～6 grades cascade extractions to the Producing Titanium Dioxide waste acid water, the volume ratio of extraction agent and spent acid is 1:5～30, and mixing time is 10min～30min, and the scandium percentage extraction is 90 ﹪～99 ﹪;
⑵ washing: the load organic phases that step ⑴ is obtained uses the sulfuric acid of 1mol/L～3mol/L and ydrogen peroxide 50 that concentration is 27 ﹪ to be washing composition; Through 10 grades～20 grades tandem washings; Load organic phases and vitriolic volume ratio are 1:1/3～3, and the ydrogen peroxide 50 add-on is 1 ﹪～10 ﹪ of sulfuric acid volume, first step loading organic phase; Last step adds sulfuric acid, adds ydrogen peroxide 50 at penultimate stage one or more levels in to the 8th grade reciprocal;
⑶ back extraction: toward the interior sodium hydroxide solution that adds 1mol/L～4mol/L of reaction kettle; Be warming up to 40 ℃～80 ℃; The load organic phases that step ⑵ obtains is sent into reaction kettle, and the volume ratio of load organic phases and sodium hydroxide solution is 1:1/2～3, stirs back extraction; Time is 10 min～30min, clarification;
⑷ acid is dissolved: the strip liquor that step ⑶ is obtained is crossed and is filtered rich scandium alkali cake, and rich scandium alkali cake dissolves in the reaction kettle internal heating with 1mol/L～6mol/L sulfuric acid or hydrochloric acid, and boils the abundant hydrolysis of titanium is separated out, and press filtration gets scandium sulfate or Scium trichloride solution;
⑸ oxalic acid precipitation: the solution that step ⑷ is obtained precipitates with 1 ﹪～5 ﹪ oxalic acid solutions, gets granular oxalic acid scandium;
⑹ calcination: the oxalic acid scandium that step ⑸ is obtained is in 800 ℃～1000 ℃ following calcinations, purity be the Scium trioxide of 99.0 ﹪～99.99 ﹪.
2. the recovery method of scandium in the Producing Titanium Dioxide waste acid water according to claim 1 is characterized in that in step ⑵, between penultimate stage is to the 8th grade reciprocal, adds ydrogen peroxide 50 at interval.
3. the recovery method of scandium in the Producing Titanium Dioxide waste acid water according to claim 1; It is characterized in that in step ⑶, after the clarification, upper blank organic phase in the siphon reaction kettle; Continue in reaction kettle, to add the load organic phases with blank organic equal volume, and repeating step ⑶ 2 times～5 times.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102994756A (en) * | 2012-09-29 | 2013-03-27 | 贵州绿水青山环保科技有限公司 | Method for enriching rare earth elements from red mud |
| CN103060580A (en) * | 2013-01-11 | 2013-04-24 | 湖南宝盈新材料有限公司 | Method for separating titanium, scandium and zirconium in scandium extraction with titanium white waste acid |
| CN103060581A (en) * | 2013-01-11 | 2013-04-24 | 湖南宝盈新材料有限公司 | Method for extracting and recycling scandium in waste acid in titanium white production |
| CN103131854A (en) * | 2013-03-18 | 2013-06-05 | 广西冶金研究院 | Method for comprehensively recovering scandium and titanium by leaching red mud with titanium white waste acid |
| CN103318940A (en) * | 2013-07-05 | 2013-09-25 | 中国科学院宁波材料技术与工程研究所 | Method for extracting scandium oxide from zirconium oxychloride waste acid |
| CN103361488A (en) * | 2013-07-31 | 2013-10-23 | 湖南永利化工股份有限公司 | Recycling method of scandium in titanium white waste water |
| CN103614560A (en) * | 2013-11-25 | 2014-03-05 | 四川有色金砂选矿药剂有限公司 | Method of recycling scandium in titanium white waste acid |
| CN106591581A (en) * | 2016-11-07 | 2017-04-26 | 中铝广西有色稀土开发有限公司 | Purification method of titanium oxide waste water regeneration scandium |
| CN106636684A (en) * | 2016-11-07 | 2017-05-10 | 中铝广西有色稀土开发有限公司 | Method for enriching scandium from titanium white wastewater |
| CN108627499A (en) * | 2018-04-13 | 2018-10-09 | 中航金属材料理化检测科技有限公司 | A kind of assay method of Boron in Titanium Alloy content |
| CN108950219A (en) * | 2018-04-03 | 2018-12-07 | 东北大学 | A kind of the step extraction and method of comprehensive utilization of titanium white waste acid valuable metal |
| CN109576493A (en) * | 2018-12-25 | 2019-04-05 | 衢州华友钴新材料有限公司 | A method of removing trace amount of titanium from cobalt liquid |
| CN115974128A (en) * | 2022-12-29 | 2023-04-18 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recycling scandium from molten salt chlorination comprehensive utilization by-product by using titanium dioxide waste acid |
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| CN1844421A (en) * | 2006-03-17 | 2006-10-11 | 汪友华 | Method for extracting scandium from red mud |
| CN102127641A (en) * | 2010-07-20 | 2011-07-20 | 湖南稀土技术开发有限公司 | Method for recovering scandium and titanium in titanium white wastewater |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102994756A (en) * | 2012-09-29 | 2013-03-27 | 贵州绿水青山环保科技有限公司 | Method for enriching rare earth elements from red mud |
| CN103060580A (en) * | 2013-01-11 | 2013-04-24 | 湖南宝盈新材料有限公司 | Method for separating titanium, scandium and zirconium in scandium extraction with titanium white waste acid |
| CN103060581A (en) * | 2013-01-11 | 2013-04-24 | 湖南宝盈新材料有限公司 | Method for extracting and recycling scandium in waste acid in titanium white production |
| CN103131854A (en) * | 2013-03-18 | 2013-06-05 | 广西冶金研究院 | Method for comprehensively recovering scandium and titanium by leaching red mud with titanium white waste acid |
| CN103318940A (en) * | 2013-07-05 | 2013-09-25 | 中国科学院宁波材料技术与工程研究所 | Method for extracting scandium oxide from zirconium oxychloride waste acid |
| CN103318940B (en) * | 2013-07-05 | 2015-05-20 | 中国科学院宁波材料技术与工程研究所 | Method for extracting scandium oxide from zirconium oxychloride waste acid |
| CN103361488A (en) * | 2013-07-31 | 2013-10-23 | 湖南永利化工股份有限公司 | Recycling method of scandium in titanium white waste water |
| CN103614560A (en) * | 2013-11-25 | 2014-03-05 | 四川有色金砂选矿药剂有限公司 | Method of recycling scandium in titanium white waste acid |
| CN106591581A (en) * | 2016-11-07 | 2017-04-26 | 中铝广西有色稀土开发有限公司 | Purification method of titanium oxide waste water regeneration scandium |
| CN106636684A (en) * | 2016-11-07 | 2017-05-10 | 中铝广西有色稀土开发有限公司 | Method for enriching scandium from titanium white wastewater |
| CN106636684B (en) * | 2016-11-07 | 2019-08-06 | 中铝广西有色稀土开发有限公司 | A method of the scandium-enriched from titanium dioxide wastewater |
| CN108950219A (en) * | 2018-04-03 | 2018-12-07 | 东北大学 | A kind of the step extraction and method of comprehensive utilization of titanium white waste acid valuable metal |
| CN108627499A (en) * | 2018-04-13 | 2018-10-09 | 中航金属材料理化检测科技有限公司 | A kind of assay method of Boron in Titanium Alloy content |
| CN109576493A (en) * | 2018-12-25 | 2019-04-05 | 衢州华友钴新材料有限公司 | A method of removing trace amount of titanium from cobalt liquid |
| CN115974128A (en) * | 2022-12-29 | 2023-04-18 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recycling scandium from molten salt chlorination comprehensive utilization by-product by using titanium dioxide waste acid |
| 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 |
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Application publication date: 20120926 |