CN102154560A - Method for separating and extracting uranium and thorium from superior molten slag - Google Patents
Method for separating and extracting uranium and thorium from superior molten slag Download PDFInfo
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- CN102154560A CN102154560A CN2011101381420A CN201110138142A CN102154560A CN 102154560 A CN102154560 A CN 102154560A CN 2011101381420 A CN2011101381420 A CN 2011101381420A CN 201110138142 A CN201110138142 A CN 201110138142A CN 102154560 A CN102154560 A CN 102154560A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention relates to the field of hydrometallurgy, in particular to a method for separating enriched uranium and thorium from rare earth superior molten slag. In the method for separating the enriched uranium and thorium from the superior molten slag, disclosed by the invention, the technical scheme for performing alkaline leaching on the superior molten slag, performing acid leaching on precipitated uranium and separating precipitated thorium is adopted, so that the precipitate of uranyl and precipitate of thorium are obtained respectively. Due to the adoption of a separation technology of stepwise leaching and precipitating, complete separation of thorium and uranium is realized, the equipment and process flow are simple, the operation is convenient, raw material are readily available, and the environmental pollution is reduced.
Description
Technical field
The present invention relates to the hydrometallurgy field, specifically be a kind of from the excellent molten slag of rare earth the method for separating enriched uranium and thorium.
Background technology
Excellent molten slag is the solid waste of monazite after extracting main rare earth element, because this excellent molten slag contains multiple radioelement such as a large amount of uranium, thorium, often is deposited in the environment with the waste form, gives that physical environment and people are healthy to bring very big harm.The main chemical compositions of excellent molten slag is the oxyhydroxide of amphoteric metal oxyhydroxide and thorium, uranium and dissolved mineral not, excellent molten slag can access the mixture of thorium and uranium after leaching, extracting and separating, usually adopt the acid leaching-extraction technology to come the mixture of Separation of Thorium, uranium at present, the main step gathers: 1, nitrate leaching dissolving, in leaching equipment, excellent molten slag is soaked dissolving with aqueous nitric acid; 2, solid-liquid separation: separate the thoriated that removal of impurities obtains and the mixed liquor of uranium and other metals through solid-liquid; 3, extraction: extract the pregnant solution of thorium and uranium with extraction liquid (mixture of TBP and kerosene) from above-mentioned mixed liquor, extraction phase is the pregnant solution of thorium and uranium, and extracting phase is other metal enrichment liquid; 4, back extraction: the hydroxide mixture that is settled out thorium and uranium with low ammonia soln from the extraction phase of the pregnant solution of above-mentioned thorium and uranium.In extraction process, Th (NO
3)
4Generate Th (NO3) with TBP
42TBP, uranium nitrate and TBP generate UO
2(NO
3)
22TBP is extracted and enters extraction phase.Because the nitrate of thorium and uranium has close physicochemical property, in pickling liquor, extract the normally thorium that obtains and the mixture of uranium, and the mixture of this thorium and uranium there is not usually practical value still can only to be positioned in the environment with the form of solid waste.The main drawback that the separation method of this leaching extraction exists is:
1. product is impure, and uranium and thorium still exist with form of mixtures, and product need be proceeded purification processes, and industrial utilization is worth low.
2. in the acid leaching-extraction process, should use nitric acid, use kerosene and ammoniacal liquor again, the use of these industrial chemicals brings pollution and makes equipment often be in the deep-etching state to environment.
3. along with extraction is carried out, thorium is constantly transferred to the organic extraction mutually from water with uranium, the content of aqueous phase thorium and uranium is reduced significantly, thereby make rate of extraction slack-off, the content of the mixture of thorium and uranium is lower in the gained extraction phase, concentration can not reach capacity, the concentration that reaches capacity must increase the spissated load of subsequent evaporation, not only the comprehensive recovery of thorium and uranium is low, and follow-up refine process feed liquid treatment capacity is also very big, if will realize the production that cleans of zero release, then the processing cost height then can not aggravate environmental pollution as if treated;
4. separating technology complexity, the equipment that should leach has extraction equipment again, also needs back extraction equipment simultaneously, and the production capacity of equipment is low;
5. leaching, rate of extraction and efficient in the existing sepn process are low, and economic benefit and social benefit are not high.
Summary of the invention
In order to overcome the deficiency of existing isolation technique, the invention provides a kind of from excellent molten slag the method for separation and Extraction uranium, thorium, its realizes separating fully of thorium and uranium, shortens the separating technology route, improves velocity of separation and efficient, reduces cost and reduces environmental pollution.
The objective of the invention is to realize by following approach: a kind of from excellent molten slag the method for separation and Extraction uranium, thorium, its processing step is as follows: is that 1000: 50～100: 2000 ratio is put in the tank reactor with excellent molten slag, alkali and water in ratio of quality and the number of copies, stir logical carbonic acid gas down, the red-tape operati temperature is at 40～100 ℃, the pH value is 8～11, through 4～12 hours leaching, left standstill 6～8 hours, separate obtaining alkali immersion liquid and solid phase;
Described alkali immersion liquid is a uranyl tricarbonate solution, adds dilute hydrochloric acid and regulates alkali immersion liquid pH value to 6～8, adds phosphoric acid salt again, and phosphatic dosage is 8～10 times that alkali soaks uranium content in the solution, obtains uranyl phosphate salt product UO
2HPO
4.4H
2O;
Be that 150～350: 1000～2000 ratio joins alkali to sulfuric acid, water and soaks in the solid phase of separating in ratio of quality and the number of copies, the red-tape operati temperature is at 60～140 ℃, leaching time 4～8 hours, left standstill 4～12 hours, separate obtaining pickling liquor and insoluble solid formation, pickling liquor is thorium enriched thorium sulfate solution; In pickling liquor, regulate pH value to 6.0, obtain thorium hydroxide throw out Th (OH) with alkali
4
Further, it is still formula container that described alkali soaks equipment, and it comprises whipping appts and heating unit; Described whipping appts is a mechanical stirring device; Heating unit is that the combination of any or they in steam heater, the electric heater unit all can.
Further, it is a kind of in sodium hydroxide, potassium hydroxide and the yellow soda ash that alkali soaks with alkali, or their combination.
Further, it is 60～80 ℃ that alkali soaks service temperature, and the operating time, alkali soaked the pH value between 9～10 at 6～8 hours, and time of repose was at 4～6 hours.
Further, phosphoric acid salt is any of tricresyl phosphate sodium salt, perlate salt, or their combination.
Further, in the acidleach process, the vitriolic dosage is 250～280 by ratio of quality and the number of copies, and it is 6～8 hours that acidleach is stirred, and time of repose is 6～8 hours, and service temperature is 90～110 ℃.
Further, the pH value of precipitation thorium is controlled between 5.5～6.
Further, precipitation thorium alkali is any of caustic soda, soda ash, or their combination.
The present invention is a kind of, and the method employing alkali of separation and Extraction uranium, thorium soaks from excellent molten slag, uranium is extracted in acidleach step by step, thorium technology, uranium in the excellent molten slag is leached in different processes with thorium and purify, thereby make that uranium and the thorium separated are not to exist with form of mixtures, the uranium product that obtains is the uranyl phosphate salt hydrate, purity is more than 63%, the product of thorium is to occur with oxygen Thorotrast form, and purity is more than 85%.
Compare with existing uranium, thorium isolation technique, this method has following advantage:
1. technology is simple, and is easy to operate.Separating technology of the present invention comprises simple procedures such as leaching, separatory and precipitation, only needs to adopt simple leaching, filter plant, need not other equipment in the production process, and is easy to operate.
2. has environment friendly.Handled raw material is to have alpha-contamination rare earth waste, can obtain having products such as nuclear industry fuel uranium and thorium again, makes resource obtain regeneration; Leach simultaneously and precipitate and be mostly to adopt mineral acid and mineral alkali, waste water that obtains and solid waste provide condition as long as just can be discharged in the environment through simple neutralizing treatment for realizing zero release cleaned industry production.
3. quality product height.The present invention has carried out separating fully to isolated uranium, thorium in the excellent molten slag, and the target product that obtains is highly purified uranyl deposited salt and thorium hydroxide, has reduced the treatment capacity of material in the follow-up refining step.
4. raw material is easy to get.The raw material that the present invention relates to is industry inorganic acid alkali commonly used, and handled raw material is again to have alpha-contamination rare earth waste, and raw material is cheap and easy to get.
Following table is the content of excellent molten slag each element before and after present method is handled, and data come from the analyzing and testing report of nuclear industry 230 Institute of Analysis of institute in the table.
Embodiment
The present invention a kind of from excellent molten slag the method for separation and Extraction uranium, thorium, its processing step is as follows: is that 1000: 50～100: 2000 ratio is put in the tank reactor with excellent molten slag, alkali and water in ratio of quality and the number of copies, stir logical carbonic acid gas down, the red-tape operati temperature is at 40～100 ℃, the pH value is 8～11, through 4～12 hours leaching, left standstill 6～8 hours, separate obtaining alkali immersion liquid and solid phase;
Described alkali immersion liquid is a uranyl tricarbonate solution, adds dilute hydrochloric acid and regulates alkali immersion liquid pH value to 6～8, adds phosphoric acid salt again, and phosphatic dosage is 8～10 times that alkali soaks uranium content in the solution, obtains uranyl phosphate salt product UO
2HPO
4.4H
2O;
Be that 150～350: 1000～2000 ratio joins alkali to sulfuric acid, water and soaks in the solid phase of separating in ratio of quality and the number of copies, the red-tape operati temperature is at 60～140 ℃, leaching time 4～8 hours, left standstill 4～12 hours, separate obtaining pickling liquor and insoluble solid formation, pickling liquor is thorium enriched thorium sulfate solution; In pickling liquor, regulate pH value to 6.0, obtain thorium hydroxide throw out Th (OH) with alkali
4
Further, it is a kind of in sodium hydroxide, potassium hydroxide and the yellow soda ash that alkali soaks with alkali, or their combination.
Further, it is 60～80 ℃ that alkali soaks service temperature, and the operating time, alkali soaked the pH value between 9～10 at 6～8 hours, and time of repose was at 4～6 hours.
Further, phosphoric acid salt is any of tricresyl phosphate sodium salt, perlate salt, or their combination.
Further, in the acidleach process, the vitriolic dosage is 250～280 by ratio of quality and the number of copies, and it is 6～8 hours that acidleach is stirred, and time of repose is 6～8 hours, and service temperature is 90～110 ℃.
Further, the pH value of precipitation thorium is controlled between 5.5～6.
Further, precipitation thorium alkali is any of caustic soda, soda ash, or their combination.
Embodiment 1:
With excellent molten waste residue 1000g, the water of 2000g joins in the reactor, adds 50g sodium hydroxide while stirring, add the logical carbonic acid gas in back, 80 ℃ of red-tape operati temperature, pH value are 10, stir and left standstill 8 hours after 8 hours, emit supernatant liquid in reactor, the solid phase slag places the acidleach pond; Logical carbonic acid gas makes clear liquid pH value a little less than 6.5 in clear liquid, adds Sodium phosphate dibasic then, stirs and leaves standstill 4 hours after one hour, filters and obtains high purity xanchromatic uranyl phosphate product; The water that in the acidleach pond of solid phase slag, adds 1500g, stir and add the sulfuric acid of 250g then, temperature is controlled at 100 ℃, reacted 4 hours, left standstill 10 hours after adding the water stirred for several minute of 1000g again, emit pickling liquor, hydro-oxidation sodium is in leaching liquid, control pH value is filtered and is obtained highly purified thorium hydroxide 6.0.
Embodiment 2:
With excellent molten waste residue 1000g, the water of 2000g joins in the reactor, adds 50g yellow soda ash while stirring, add the logical carbonic acid gas in back, 80 ℃ of red-tape operati temperature, pH value are 8.5, stir and left standstill 8 hours after 8 hours, emit supernatant liquid in reactor, the solid phase slag places the acidleach pond; Logical carbonic acid gas makes clear liquid pH value a little less than 6.5 in clear liquid, adds tertiary sodium phosphate then, stirs and leaves standstill 4 hours after one hour, filters and obtains high purity xanchromatic uranyl phosphate product; The water that in the acidleach pond of solid phase slag, adds 1500g, stir and add the sulfuric acid of 300g then, temperature is controlled at 95 ℃, reacted 4 hours, left standstill 6 hours after adding the water stirred for several minute of 1000g again, emit pickling liquor, hydro-oxidation sodium is in leaching liquid, control pH value is filtered and is obtained highly purified thorium hydroxide 6.0.
Embodiment 3:
With excellent molten waste residue 1000g, the water of 2000g joins in the reactor, add 25g sodium hydroxide and 30g yellow soda ash while stirring, add the logical carbonic acid gas in back, 80 ℃ of red-tape operati temperature, pH value are 9, stir to leave standstill 8 hours after 8 hours, emit supernatant liquid in reactor, the solid phase slag places the acidleach pond; Logical carbonic acid gas makes clear liquid pH value a little less than 6.5 in clear liquid, adds Sodium phosphate dibasic then, stirs and leaves standstill 4 hours after one hour, filters and obtains high purity xanchromatic uranyl phosphate product; The water that in the acidleach pond of solid phase slag, adds 1500g, stir and add the sulfuric acid of 250g then, temperature is controlled at 110 ℃, reacted 4 hours, left standstill 8 hours after adding the water stirred for several minute of 1000g again, emit pickling liquor, hydro-oxidation sodium is in leaching liquid, control pH value is filtered and is obtained highly purified thorium hydroxide 6.0.
Embodiment of the present invention are a lot; can't be exhaustive; as long as adopt alkali to soak and acidleach associating proceed step by step uranium and isolating all technical schemes of thorium, all belong to protection scope of the present invention, especially protect and utilize from excellent molten slag material that alkali soaks, the technical scheme of pickling process SEPARATION OF URANIUM, thorium.
Claims (7)
1. the method for separation and Extraction uranium, thorium from an excellent molten slag, it is characterized in that: its processing step is as follows: is that 1000: 50～100: 2000 ratio is put in the tank reactor with excellent molten slag, alkali and water in ratio of quality and the number of copies, stir logical carbonic acid gas down, the red-tape operati temperature is at 40～100 ℃, the pH value is 8～11, through 4～12 hours leaching, left standstill 6～8 hours, separate obtaining alkali immersion liquid and solid phase;
Described alkali immersion liquid is a uranyl tricarbonate solution, adds dilute hydrochloric acid and regulates alkali immersion liquid pH value to 6～8, adds phosphoric acid salt again, and phosphatic dosage is 8～10 times that alkali soaks uranium content in the solution, obtains uranyl phosphate salt product UO
2HPO
4.4H
2O;
Be that 150～350: 1000～2000 ratio joins alkali to sulfuric acid, water and soaks in the solid phase of separating in ratio of quality and the number of copies, the red-tape operati temperature is at 60～140 ℃, leaching time 4～8 hours, left standstill 4～12 hours, separate obtaining pickling liquor and insoluble solid formation, pickling liquor is thorium enriched thorium sulfate solution; In pickling liquor, regulate pH value to 6.0, obtain thorium hydroxide throw out Th (OH) with alkali
4
2. as claimed in claim 1 a kind of from excellent molten slag the method for separation and Extraction uranium, thorium, it is characterized in that: it is a kind of in sodium hydroxide, potassium hydroxide and the yellow soda ash that alkali soaks with alkali, or their combination.
3. as claimed in claim 1 a kind of from excellent molten slag the method for separation and Extraction uranium, thorium, it is characterized in that: it is 60～80 ℃ that alkali soaks service temperature, the operating time, alkali soaked the pH value between 9～10 at 6～8 hours, time of repose was at 4～6 hours.
4. as claimed in claim 1 a kind of from excellent molten slag the method for separation and Extraction uranium, thorium, it is characterized in that: phosphoric acid salt is any of tricresyl phosphate sodium salt, perlate salt, or their combination.
5. as claimed in claim 1 a kind of from excellent molten slag the method for separation and Extraction uranium, thorium, it is characterized in that: in the acidleach process, the vitriolic dosage is 250～280 by ratio of quality and the number of copies, and it is 6～8 hours that acidleach is stirred, time of repose is 6～8 hours, and service temperature is 90～110 ℃.
6. as claimed in claim 1 a kind of from excellent molten slag the method for separation and Extraction uranium, thorium, it is characterized in that: the pH value of precipitation thorium is controlled between 5.5～6.
7. as claimed in claim 1 a kind of from excellent molten slag the method for separation and Extraction uranium, thorium, it is characterized in that: precipitation thorium alkali is any of caustic soda, soda ash, or their combination.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103014358A (en) * | 2012-11-27 | 2013-04-03 | 益阳鸿源稀土有限责任公司 | Treatment method of tailings after separation and recovery of monazite slag |
| CN103014333A (en) * | 2012-11-27 | 2013-04-03 | 益阳鸿源稀土有限责任公司 | Separation and recovery method of uranium, thorium and rare earth in monazite slag |
| CN104485148A (en) * | 2014-11-18 | 2015-04-01 | 中国科学院福建物质结构研究所 | High-efficient method of extracting uranyl ions from water |
| CN106367590A (en) * | 2015-07-22 | 2017-02-01 | 永州市湘江稀土有限责任公司 | Monazite ore comprehensive utilization and recovery process |
| CN106555054A (en) * | 2015-09-29 | 2017-04-05 | 中国科学院上海应用物理研究所 | A kind of separation and recovery method of thorium and uranium |
| CN117695844A (en) * | 2024-02-05 | 2024-03-15 | 北京先通国际医药科技股份有限公司 | Method for extracting decay daughter of thorium element |
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| CN101012502A (en) * | 2007-02-05 | 2007-08-08 | 扬州大学 | Method for separating enriched uranium, thorium mixture and rare earth from preferred slag |
| WO2008108888A2 (en) * | 2006-10-05 | 2008-09-12 | Holden Charles S | Separation of radium and rare earth elements from monazite |
-
2011
- 2011-05-26 CN CN2011101381420A patent/CN102154560A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008108888A2 (en) * | 2006-10-05 | 2008-09-12 | Holden Charles S | Separation of radium and rare earth elements from monazite |
| CN101012502A (en) * | 2007-02-05 | 2007-08-08 | 扬州大学 | Method for separating enriched uranium, thorium mixture and rare earth from preferred slag |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103014358A (en) * | 2012-11-27 | 2013-04-03 | 益阳鸿源稀土有限责任公司 | Treatment method of tailings after separation and recovery of monazite slag |
| CN103014333A (en) * | 2012-11-27 | 2013-04-03 | 益阳鸿源稀土有限责任公司 | Separation and recovery method of uranium, thorium and rare earth in monazite slag |
| CN103014333B (en) * | 2012-11-27 | 2014-04-09 | 益阳鸿源稀土有限责任公司 | Separation and recovery method of uranium, thorium and rare earth in monazite slag |
| CN103014358B (en) * | 2012-11-27 | 2014-05-21 | 益阳鸿源稀土有限责任公司 | Treatment method of tailings after separation and recovery of monazite slag |
| CN104485148A (en) * | 2014-11-18 | 2015-04-01 | 中国科学院福建物质结构研究所 | High-efficient method of extracting uranyl ions from water |
| CN106367590A (en) * | 2015-07-22 | 2017-02-01 | 永州市湘江稀土有限责任公司 | Monazite ore comprehensive utilization and recovery process |
| CN106555054A (en) * | 2015-09-29 | 2017-04-05 | 中国科学院上海应用物理研究所 | A kind of separation and recovery method of thorium and uranium |
| CN106555054B (en) * | 2015-09-29 | 2019-08-13 | 中国科学院上海应用物理研究所 | A kind of separation and recovery method of thorium and uranium |
| CN117695844A (en) * | 2024-02-05 | 2024-03-15 | 北京先通国际医药科技股份有限公司 | Method for extracting decay daughter of thorium element |
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Application publication date: 20110817 |