CN103060581A - Method for extracting and recycling scandium in waste acid in titanium white production - Google Patents
Method for extracting and recycling scandium in waste acid in titanium white production Download PDFInfo
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Abstract
The invention discloses a method with simplified technology and high yield for extracting and recycling scandium in waste acid in titanium white production. The method is characterized by comprising the following steps of: extracting, washing, circularly extracting, re-extracting, acid-dissolving, precipitating and burning. The method is simple in technology and convenient to operate; and meanwhile, the scandium-containing organic circular extraction is adopted, so that the re-extracting time is reduced, the organic loss is reduced, the labor cost is reduced, and the scandium yield is increased.
Description
Technical field
The present invention relates to a kind of recovery method of rare earth Sc, specifically the extractive recovery method of scandium in a kind of Producing Titanium Dioxide spent acid.
Background technology
Scandium belongs to a kind of in the rare earth element, and few at the content of occurring in nature, the content of scandium in the earth's crust only has 5 * 10
-6, not only compare with other light elements and will hang down much, content also only belongs to medium in whole rare earth element, probably only has 1/10 of cerium.And the purposes of scandium is very extensive, as for having economize on electricity, long service life, the broken scandium sodium vapor lamp that the mist ability is strong, luminous efficiency is good, is used for solar photocell, gamma ray projector and is used for alloy material aspect, organic chemistry additive etc.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.
Recovery of scandium had had many research from last century since the eighties, mainly be to propose as a kind of by product from other mineral, such as 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 titanium dioxide, and the spent acid amount that one ton of titanium dioxide 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 titanium dioxides 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 to make scandium hydrolysis-sour molten-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 scandium hydroxide and oxalic acid scandium have certain solubleness, certainly will cause damage.For reclaiming trace element, be higher in the similar technology with the rate of recovery of extraction process.Be 201010230723.2 such as number of patent application, 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 extraction process that adopts and reclaims scandium in the titanium white waste acid.Its processing step is the steps such as extraction, back extraction, acid are molten, purification; The method because after the extraction not through washing, it is too high to contain in the scandium organic phase titanium content, and the titanium particle 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, the method for extracting scandium of denomination of invention red mud, disclose a kind of employing extraction-washing-back extraction-acid molten-precipitation method for extracting scandium.Washing step adopts sulfuric acid and hydrogen peroxide is mixed with the method for carrying out the single-stage washing after the washing lotion in its technique.Because in the process of preparation dilute sulphuric acid, a large amount of heat releases of meeting if add hydrogen peroxide this moment, certainly will cause the pyrolytic decomposition of hydrogen peroxide, therefore, must after the dilute sulphuric acid cooling, could add hydrogen peroxide.Like this, the washing lotion preparation is trouble, and the heat that can not effectively utilize dilute sulphuric acid to produce in process for preparation.
Number of patent application is 201210199246.7, publication number is CN102690962A, the applying date is 2012.06.18, denomination of invention be the recovery method of scandium in the Producing Titanium Dioxide waste acid water patent disclosure the recovery method of scandium of a kind of extraction-tandem washing-back extraction-oxalic acid precipitation, the method focuses on washing section to the wash-out of impurity and reduce the loss of scandium by the recycling strip liquor in the back extraction process.It is when extraction, and extracted organic phase and spent acid volume ratio are 1:10～20, and it is low to contain scandium concentration in the organic phase, increased the number of times of back extraction, and because the back extraction process is to carry out, scandium residual in the strip liquor is few under alkaline condition, therefore, this method has little significance for improving yield.
The recovery method of existing scandium all need just can obtain thick Scium trioxide through a plurality of operation stepss, and all can cause the loss of a small amount of scandium in each step, causes yield to reduce.
Summary of the invention
The extractive recovery method that the purpose of this invention is to provide scandium in the high Producing Titanium Dioxide spent acid of a kind of work simplification, yield.
The present invention adopts following technical scheme to realize its goal of the invention, at extraction-washing section, contains the organic characteristics that greatly reduce through washing rear impurity content of scandium by utilization, will contain the organic extraction section that is back to of scandium and again extract.This method both can improve the scandium content in the organic phase, had reduced again the foreign matter content in the organic phase, had reduced simultaneously the back extraction number of times, had avoided the too much loss of scandium, thereby reached the purpose that improves yield, simplifies technique;
The extractive recovery method of scandium in a kind of Producing Titanium Dioxide spent acid, it may further comprise the steps:
⑴ extraction: in extraction tank, adopt P204-TBP-kerosene extraction agent through 1 grade～6 grades extractions to the Producing Titanium Dioxide waste acid water, the volume ratio of extraction agent and spent acid is 1:5～30, mixing time is 5min～20min, obtains containing the scandium organic phase, scandium concentration＜1mg/L in the raffinate;
⑵ washing: the scandium organic phase that contains that step ⑴ obtains is washed with the hydrogen peroxide that sulfuric acid and the concentration of 2mol/L～4mol/L is 27 ﹪, and the volume ratio that contains scandium organic phase and sulfuric acid is 1:1/3～3, and the hydrogen peroxide add-on is 1 ﹪～10 ﹪ of sulfuric acid volume;
⑶ cycling extraction: will contain the scandium organic phase as extraction agent repeating step ⑴ and step ⑵ after the step ⑵ washing, regularly detect the concentration of scandium in the raffinate, until scandium concentration＞2mg/L in the raffinate;
⑷ back extraction: the scandium organic phase that contains that step ⑶ obtains is used the sodium hydroxide solution back extraction in reactor;
⑸ molten, the precipitation of acid: the strip liquor that step ⑷ is obtained filters to get scandium hydroxide alkali cake, and scandium hydroxide alkali cake with hydrochloric acid or sulfuric acid dissolution, after the filtration, is obtained the oxalic acid scandium with oxalic acid precipitation;
⑹ calcination: the oxalic acid scandium calcination in retort furnace with step ⑸ obtains obtains Scium trioxide.
The present invention is in step ⑵, described washing is washed through 10 grades～20 grades tandems for containing the scandium organic phase, the volume ratio that contains scandium organic phase and sulfuric acid is 1:1/3～3, the hydrogen peroxide add-on is 1 ﹪～10 ﹪ of sulfuric acid volume, the first step adds and contains the scandium organic phase, last step adds sulfuric acid, and for being avoids the excessive decomposition of hydrogen peroxide in whipping process, the interval adds hydrogen peroxide between penultimate stage is to the 8th grade reciprocal.
Be further to reclaim the scandium in raffinate and the washing lotion, the present invention when repeating step ⑴ and step ⑵, adds blank organic phase as extraction agent in extraction and the washing first step in step ⑶, and described blank organic phase is 1 ﹪ that contains the scandium organic phase～50 ﹪.
Be to reduce the number of times of press filtration, the present invention in step ⑷, after two-phase clarification layering, upper blank organic phase in the siphon reactor, continue in reactor, to add with blank organic equal volume contain the scandium organic phase, and repeating step ⑷ 2 times～5 times.
Be further purification Scium trioxide, the present invention is in step ⑸, and the solution that scandium hydroxide alkali cake is obtained after with hydrochloric acid or sulfuric acid dissolution extracts again with blank organic phase, after, the filtration molten through washing, back extraction, acid, obtains the oxalic acid scandium with oxalic acid precipitation.
Because adopt technique scheme, the present invention has realized goal of the invention preferably, its technique is simple, and is easy to operate, contains the extraction of scandium organic cycle owing to adopt, and reduced the number of times of back extraction, also reduced organic loss, reduced cost of labor, improved the yield of scandium.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1:
The extractive recovery method of scandium in a kind of Producing Titanium Dioxide spent acid, it may further comprise the steps:
⑴ extraction: in extraction tank, adopt P204-TBP-kerosene extraction agent through 1 grade～6 grades extractions to the Producing Titanium Dioxide waste acid water, the volume ratio of extraction agent and spent acid is 1:5～30, mixing time is 5min～20min, obtains containing the scandium organic phase, scandium concentration＜1mg/L in the raffinate;
Scandium concentration is 15.68mg/L in the present embodiment raw material titanium white waste acid, and titanium concentration is 6.92g/L.In the 50L extraction tank through 1 grade of extraction, calculate by volume, getting two (2-ethylhexyl phosphoric acid) P204 is 6 ﹪～15 ﹪ (present embodiment is 12 ﹪), tributyl phosphate TBP is 4 ﹪～6 ﹪ (present embodiment is 6 ﹪), all the other are kerosene, the volume ratio of extraction agent and spent acid is 1:10, and mixing time is 10min, obtains containing the scandium organic phase; It is 0.97 ㎎/L that raffinate contains scandium, and the scandium percentage extraction is 93.8 ﹪.
⑵ washing: the scandium organic phase that contains that step ⑴ obtains is washed with the hydrogen peroxide that sulfuric acid and the concentration of 2mol/L～4mol/L is 27 ﹪, and the volume ratio that contains scandium organic phase and sulfuric acid is 1:1/3～3, and the hydrogen peroxide add-on is 1 ﹪～10 ﹪ of sulfuric acid volume;
The sulphuric acid soln of present embodiment preparation 3mol/L and the hydrogen peroxide washing lotion that volume is sulfuric acid 5% to contain scandium organic phase and washing lotion volume ratio as 2:1, are warming up to 60 ℃ and carry out the single-stage washing, survey TiO in the washing lotion
2Concentration is 5.44g/L, and the titanium eluting rate is 75.6 ﹪.
⑶ cycling extraction: will contain the scandium organic phase as extraction agent repeating step ⑴ and step ⑵ after the step ⑵ washing, regularly detect the concentration of scandium in the raffinate, until scandium concentration＞2mg/L in the raffinate;
For reducing the back extraction number of times, reduce organic loss, reduce cost of labor, present embodiment contains the scandium organic phase as extraction agent repeating step ⑴ and step ⑵, coextraction spent acid 20m after with step ⑵ washing
3, the concentration that detects scandium in the raffinate is 2.47mg/L, stops extraction; Obtain being rich in the organic phase 400L of scandium, extracted organic phase and spent acid volume ratio are 1:50, have greatly improved the concentration of scandium in the organic phase, have reduced the number of times of back extraction.
Utilization of the present invention contains the characteristics that the scandium organic phase greatly reduces through washing rear impurity content, the scandium organic phase that contains after the washing is returned the extraction tank re-extract, both made scandium obtain enrichment, reduced the foreign matter content in the organic phase, simultaneously, reduced again subsequent step---the number of times of back extraction, saved manpower and materials, avoid the too much loss of scandium, thereby improved the yield of scandium.
⑷ back extraction: the scandium organic phase that contains that step ⑶ obtains is used the sodium hydroxide solution back extraction in reactor;
Present embodiment adds the 2.0mol/L sodium hydroxide solution in the reactor, is warming up to 50 ℃, the enrichment that step ⑶ is obtained the organic phase of scandium send into reactor, the volume ratio that contains scandium organic phase and sodium hydroxide solution is 1:2, stirring back extraction 20min.
⑸ molten, the precipitation of acid: the strip liquor that step ⑷ is obtained filters to get scandium hydroxide alkali cake, and scandium hydroxide alkali cake with hydrochloric acid or sulfuric acid dissolution, after the filtration, is obtained the oxalic acid scandium with oxalic acid precipitation;
The strip liquor that present embodiment obtains step ⑷ filters to get scandium hydroxide alkali cake, and scandium hydroxide alkali cake is complete with the dissolving with hydrochloric acid of 1mol/L, after the filtration, precipitates with the oxalic acid solution of 10 ﹪ and to obtain the oxalic acid scandium.
⑹ calcination: the oxalic acid scandium calcination in retort furnace with step ⑸ obtains obtains Scium trioxide.
Present embodiment places in the retort furnace oxalic acid scandium in 950 ℃ of calcinations, and obtaining total amount is the Scium trioxide 360g of 94.6 ﹪, yield 70.83 ﹪.
Embodiment 2:
Present embodiment is in step ⑴, and scandium concentration is 15.68mg/L in the raw material titanium white waste acid, and titanium concentration is 6.92g/L.In the 50L extraction tank, through 3 grades of extractions, obtain containing the scandium organic phase; It is 0.83 ㎎/L that raffinate contains scandium, and the scandium percentage extraction is 94.7 ﹪.
The present invention is in step ⑵, described washing is washed through 10 grades～20 grades tandems for containing the scandium organic phase, the volume ratio that contains scandium organic phase and sulfuric acid is 1:1/3～3, the hydrogen peroxide add-on is 1 ﹪～10 ﹪ of sulfuric acid volume, the first step adds and contains the scandium organic phase, last step adds sulfuric acid, and for taking full advantage of excessive hydrogen peroxide, the interval adds hydrogen peroxide between penultimate stage is to the 8th grade reciprocal.
Present embodiment is in step ⑵, containing the scandium organic phase washs through 10 grades of tandems, the volume ratio that contains scandium organic phase and sulfuric acid is 1:1, the hydrogen peroxide add-on is 5 ﹪ of sulfuric acid volume, the first step adds and contains the scandium organic phase, last step adds sulfuric acid, and for taking full advantage of excessive hydrogen peroxide, the interval adds hydrogen peroxide between penultimate stage is to the 8th grade reciprocal; Survey TiO in the remaining liquid of the first step
2Concentration is 6.18g/L, and the titanium eluting rate is 85.8 ﹪.
The present invention adopts the mode that adds respectively dilute sulphuric acid and hydrogen peroxide at washing section, simplified the washing lotion process for preparation, make washing lotion keep certain temperature to be conducive to the wash-out of titanium in the washing process, the a large amount of decomposition of hydrogen peroxide in high temperature and acidic medium have been avoided, effectively utilized again the heat that produces in the dilute sulphuric acid process for preparation, simultaneously, after the hydrogen peroxide charging what, organic phase after the hydrogen peroxide washing has been passed through again the bright sulfur acid elution, free hydrogen peroxide is washed recycling, reduced the loss of hydrogen peroxide, with the hydrogen peroxide of minute quantity, wash-out most impurity.
Present embodiment will contain the scandium organic phase as extraction agent repeating step ⑴ and step ⑵, coextraction spent acid 20m after the step ⑵ washing in step ⑶
3, the concentration that detects scandium in the raffinate is 2.28mg/L, stops extraction; Obtain being rich in the organic phase 300L of scandium, extracted organic phase is 1:67 with spent acid actual volume ratio.
Contain the scandium organic phase and after back extraction, molten, the precipitation of acid, calcination, obtain the Scium trioxide 350g that total amount is 95.8 ﹪, yield 69.73 ﹪.Remaining with embodiment 1.
Embodiment 3:
For further reclaiming the scandium in raffinate and the washing lotion, the present invention when repeating step ⑴ and step ⑵, adds blank organic phase as extraction agent in extraction and the washing first step in step ⑶, described blank organic phase is 1 ﹪ that contains the scandium organic phase～50 ﹪, and present embodiment is 2 ﹪.
Present embodiment in step ⑶ during cycling extraction, coextraction spent acid 20m
3, the concentration that detects scandium in the raffinate is 2.12mg/L, stops extraction; Obtain being rich in the organic phase 330L of scandium, extracted organic phase is 1:61 with spent acid actual volume ratio.
Contain the scandium organic phase and after back extraction, molten, the precipitation of acid, calcination, obtain the Scium trioxide 370g that total amount is 95.1 ﹪, yield 73.3 ﹪.Remaining with embodiment 2.
Embodiment 4:
Present embodiment in step ⑶ during cycling extraction, coextraction spent acid 20m
3, the concentration that detects scandium in the raffinate is 2.22mg/L, stops extraction; Obtain being rich in the organic phase 330L of scandium, extracted organic phase is 1:61 with spent acid actual volume ratio.
For reducing the number of times of press filtration, the present invention in step ⑷, after two-phase clarification layering, upper blank organic phase in the siphon reactor, continue in reactor, to add with blank organic equal volume contain scandium organic phase and repeating step ⑷ 2 times～5 times (present embodiment is 3 times).
In the back extraction process of the present invention, the recycling of anti-liquid, repeatedly again press filtration after the extraction has reduced the number of times of press filtration, has also reduced the loss of scandium.
Strip liquor filters to get scandium hydroxide alkali cake, obtains the Scium trioxide 375g that total amount is 94.9 ﹪, yield 74.01 ﹪ after, precipitation molten through acid, the calcination.Remaining with embodiment 2,3.
Embodiment 5:
Present embodiment in step ⑶ during cycling extraction, coextraction spent acid 20m
3, the concentration that detects scandium in the raffinate is 2.18mg/L, stops extraction; Obtain being rich in the organic phase 330L of scandium, extracted organic phase is 1:61 with spent acid actual volume ratio.
Be further purification Scium trioxide, the present invention is in step ⑸, and the solution that scandium hydroxide alkali cake is obtained after with hydrochloric acid or sulfuric acid dissolution extracts again with blank organic phase, after, the filtration molten through washing, back extraction, acid, obtains the oxalic acid scandium with oxalic acid precipitation.
Present embodiment is in step ⑸, scandium hydroxide alkali cake is complete with the dissolving with hydrochloric acid of 1mol/L, again extract with blank organic phase again, molten through washing, back extraction, acid, filter after, oxalic acid solution precipitation with 10 ﹪ obtains the oxalic acid scandium, the oxalic acid scandium obtains the Scium trioxide 340g that total amount is 97.6 ﹪, yield 69.13 ﹪ after calcination.Remaining with embodiment 2,3,4.
Claims (6)
1. the extractive recovery method of scandium in the Producing Titanium Dioxide spent acid is characterized in that it may further comprise the steps:
⑴ extraction: in extraction tank, adopt P204-TBP-kerosene extraction agent through 1 grade～6 grades extractions to the Producing Titanium Dioxide waste acid water, the volume ratio of extraction agent and spent acid is 1:5～30, mixing time is 5min～20min, obtains containing the scandium organic phase, scandium concentration＜1mg/L in the raffinate;
⑵ washing: the scandium organic phase that contains that step ⑴ obtains is washed with the hydrogen peroxide that sulfuric acid and the concentration of 2mol/L～4mol/L is 27 ﹪, and the volume ratio that contains scandium organic phase and sulfuric acid is 1:1/3～3, and the hydrogen peroxide add-on is 1 ﹪～10 ﹪ of sulfuric acid volume;
⑶ cycling extraction: will contain the scandium organic phase as extraction agent repeating step ⑴ and step ⑵ after the step ⑵ washing, regularly detect the concentration of scandium in the raffinate, until scandium concentration＞2mg/L in the raffinate;
⑷ back extraction: the scandium organic phase that contains that step ⑶ obtains is used the sodium hydroxide solution back extraction in reactor;
⑸ molten, the precipitation of acid: the strip liquor that step ⑷ is obtained filters to get scandium hydroxide alkali cake, and scandium hydroxide alkali cake with hydrochloric acid or sulfuric acid dissolution, after the filtration, is obtained the oxalic acid scandium with oxalic acid precipitation;
⑹ calcination: the oxalic acid scandium calcination in retort furnace with step ⑸ obtains obtains Scium trioxide.
2. the extractive recovery method of scandium in the Producing Titanium Dioxide spent acid according to claim 1, it is characterized in that in step ⑵, described washing is washed through 10 grades～20 grades tandems for containing the scandium organic phase, the volume ratio that contains scandium organic phase and sulfuric acid is 1:1/3～3, the hydrogen peroxide add-on is 1 ﹪～10 ﹪ of sulfuric acid volume, the first step adds and contains the scandium organic phase, and last step adds sulfuric acid, and the interval adds hydrogen peroxide between penultimate stage is to the 8th grade reciprocal.
3. the extractive recovery method of scandium in the Producing Titanium Dioxide spent acid according to claim 1 is characterized in that in step ⑶, when repeating step ⑴ and step ⑵, adds blank organic phase as extraction agent in extraction and the washing first step.
4. the extractive recovery method of scandium in the Producing Titanium Dioxide spent acid according to claim 3 is characterized in that blank organic phase is 1 ﹪ that contains the scandium organic phase～50 ﹪.
5. the extractive recovery method of scandium in the Producing Titanium Dioxide spent acid according to claim 1, it is characterized in that in step ⑷, after two-phase clarification layering, upper blank organic phase in the siphon reactor, continue in reactor, to add with blank organic equal volume contain the scandium organic phase, and repeating step ⑷ 2 times～5 times.
6. the extractive recovery method of scandium in the Producing Titanium Dioxide spent acid according to claim 1, it is characterized in that in step ⑸, the solution that scandium hydroxide alkali cake is obtained after with hydrochloric acid or sulfuric acid dissolution extracts again with blank organic phase, molten through washing, back extraction, acid, filter after, obtain the oxalic acid scandium with oxalic acid precipitation.
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| 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 |
| CN103667748A (en) * | 2013-12-30 | 2014-03-26 | 贵州鑫亚矿业有限公司 | Method for preparing purified scandium from crude scandium enriched in raw anatase and serving as raw material |
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| 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 |
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| 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 |
| CN103667748A (en) * | 2013-12-30 | 2014-03-26 | 贵州鑫亚矿业有限公司 | Method for preparing purified scandium from crude scandium enriched in raw anatase and serving as raw material |
| CN106399685A (en) * | 2015-07-28 | 2017-02-15 | 永州市湘江稀土有限责任公司 | Uranium, iron, thorium and rare earth extraction and separation process |
| CN106399685B (en) * | 2015-07-28 | 2019-06-25 | 永州市湘江稀土有限责任公司 | A kind of uranium, iron, thorium, rare-earth extraction separating process |
| 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 |
| CN109266870A (en) * | 2018-09-28 | 2019-01-25 | 中国恩菲工程技术有限公司 | The method for extracting scandium oxide |
| CN114262806A (en) * | 2021-12-13 | 2022-04-01 | 先导薄膜材料（广东）有限公司 | Method for recycling scandium and zirconium from waste solid oxide fuel cell |
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Application publication date: 20130424 |