CN103849764B - The method of Extraction of Uranium from acid, large proportion or lower concentration uranium ore extraction stoste - Google Patents
The method of Extraction of Uranium from acid, large proportion or lower concentration uranium ore extraction stoste Download PDFInfo
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- CN103849764B CN103849764B CN201210514137.XA CN201210514137A CN103849764B CN 103849764 B CN103849764 B CN 103849764B CN 201210514137 A CN201210514137 A CN 201210514137A CN 103849764 B CN103849764 B CN 103849764B
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Abstract
The present invention relates to uranium hydrometallurgy abstraction technique, object is for the concentrated problem of acid, proportion or lower concentration uranium solution greatly difficulty, provides a kind of method of Extraction of Uranium from acid, large proportion or lower concentration uranium ore extraction stoste, to improve production capacity and to reduce costs.The present invention is that extraction agent extracts acid, large proportion or the complicated uranium solution of lower concentration with Trifatty amine, take polyvalent alcohol as the physicals that additive improves extraction agent, respond well for Extraction of Uranium from acid, large proportion or lower concentration, large proportion or lower concentration extraction stoste.<!--1-->
Description
Technical field
The present invention relates to uranium hydrometallurgy abstraction technique field, be specifically related to a kind of method to Extraction of Uranium in acid, large proportion or low concentration solution.
Background technology
Along with the development of China's nuclear energy, the demand of natural uranium is continued to increase.Because of the decline of uranium ore grade, more how low-grade, multicomponent refractory mineral needs again to exploit processing, thus it is general lower to cause uranium ore to extract uranium concentration in stoste, and composition becomes increasingly complex.Except the SO containing routine
4 2-, iron, phosphorus, aluminium, manganese, vanadium, calcium, magnesium, silicon, outside the impurity such as molybdenum, also containing certain humic acids, organism, heavy metal oxide etc.Wherein, acid, large proportion or lower concentration are the principal features of this type of uranium ore extraction stoste.At present, the research specially for acid, large proportion or lower concentration uranium ore extraction stoste concentration technique is less, becomes the technical bottleneck of restriction production capacity.
The concentrated employing ion exchange process of China's major part uranium ore extraction stoste and extraction process.Ion exchange method be mainly applicable to relatively large enterprise from low uranium concentration, containing a large amount of impurity uranium ore extraction stoste extract high concentration uranium, extraction process be mainly applicable to medium and small sized enterprises and higher concentration uranium ore extraction stoste.From the viewpoint of economic benefit, the boundary of the uranium ore extraction original liquid concentration that ion exchange method and extraction process are suitable for is 1g/L.But ion exchange method equipment is complicated, spoilage is high, labour intensity is large, and there is the problems such as processing wastewater, discharging any waste liquor amount be excessive, and neutralize, have a large amount of metal to return to stockyard in transformation process, the main technique rate of recovery and heap leaching rate are had a strong impact on, such as a large amount of Na
2sO
4return the crystallization of dump leaching field, affect stockyard leaching yield.When extracting original liquid concentration lower than 1g/L, extraction point is compared slow, and organic solvent consumption is comparatively large, should not adopt when processing acid, large proportion or lower concentration uranium ore extraction stoste.This makes extraction cells operate becomes the difficulties processed in acid, large proportion or lower concentration extraction stoste.
Extraction agent is the key issue of abstraction technique.From 1945 tributylphosphate (TBP) be used as first since uranium extraction agent, be widely used as by countries in the world the extraction agent that in core combustion aftertreatment, thorium, uranium are separated so far.But due to TPB self-defect, people find more preferably substitute and synergist always, to reach the object improving extracting power further.But extraction agent of the prior art just uranium ore that is single for composition, higher concentration extracts stoste, for acid, that proportion or lower concentration extraction stoste greatly process but often has experimental basis and application example research and report.The new abstraction technique of China's hydrometallurgical process of uranium an urgent demand can replace traditional ion exchange process, particularly extracts stoste concentration technique, reduces labor intensity to reach, and reduces production cost, improves the object of production capacity.
Summary of the invention
The object of the invention is for the concentrated problem of acid, proportion or lower concentration uranium solution greatly difficulty, provide a kind of method of Extraction of Uranium from acid, large proportion or lower concentration uranium ore extraction stoste, to improve production capacity and to reduce costs.
The technical solution used in the present invention is: a kind of method of Extraction of Uranium from acid, large proportion or lower concentration uranium solution, in turn includes the following steps:
A method for Extraction of Uranium from acid, large proportion or lower concentration uranium solution, in turn includes the following steps:
Step one: the acquisition of extraction stoste: fine ore granularity being less than 8mm is banked up, adopts dense H after many heap series connection
2sO
4carry out dump leaching, make pH of leaching solution be 0.8 ~ 1.5, leaching cycle is 120 days, and the leach liquor that collection obtains is as extraction stoste;
Step 2: organic phase makes the transition: be that the Trifatty amine of 0.1 ~ 0.18mol/L is extraction agent, take polyvalent alcohol as additive with concentration, by Trifatty amine: polyvalent alcohol: sulfonated kerosene is that 15:10:180 is mixed into organic phase with volume ratio, then be the H of 70 ~ 80g/L according to organic phase and mass concentration
2sO
4be in a ratio of 4/1 ~ 6/1, duration of contact is that 3 ~ 5min carries out static phase-splitting, collects the organic phase obtained;
Step 3: extraction: extraction stoste is added in the organic phase made the transition, be in a ratio of 1/4 ~ 1/7 according to the organic phase that makes the transition with extraction stoste and carry out two-phase mixtures, duration of contact is 1 ~ 3min, and temperature of reaction is 13 ~ 40 DEG C, obtains saturated organic phase after static phase-splitting;
Step 4: repeating one or many counter-current extraction to the saturated organic phase that step 3 obtains according to step 3, can be twice, three times, four times or five times;
Step 5: washing: be in a ratio of 4/1 ~ 6/1 according to saturated organic phase and service water, duration of contact is that 3 ~ 5min service water washs saturated organic phase;
Step 6: strip: be the NaOH of 15 ~ 25g/L and the Na of 60 ~ 80g/L with mass concentration
2cO
3mixing solutions as strippant, be in a ratio of 6/1 ~ 9/1 according to saturated organic phase with extraction stoste and strip according to method in step 3 to the saturated organic phase after wash, duration of contact is 3 ~ 4min, and temperature of reaction is 13 ~ 40 DEG C, and what collection obtained contains U aqueous phase.
To take Trifatty amine as extraction agent extract acid, large proportion or the complicated uranium solution of lower concentration in the present invention, take polyvalent alcohol as the physicals that additive improves extraction agent, respond well for Extraction of Uranium from acid, large proportion or lower concentration extraction stoste.Step one compared with ion-exchange, cost-saving 30 ~ 45%, the rate of recovery improves 2 ~ 3%, and production capacity improves 2.5 ~ 3.5%; The aqueous phase that step 3 extraction stoste obtains after extraction is raffinate, and raffinate returns to stockyard for again preparing spray agent, and wherein uranium concentration drops to 10mg/L by 100mg/L, Na
2sO
4content is less than ion exchange method greatly, can not cause stockyard in winter surface Na in subsequent processes
2sO
4the accumulation of crystallization.Therefore can accelerate leaching process, shorten period of heap leaching.Meanwhile, can improve the quality of products.
Embodiment
Be further described below in conjunction with the method for specific embodiment to a kind of Extraction of Uranium from acid, large proportion or lower concentration uranium solution of the present invention.
Embodiment 1
1 grade of transition, 4 stage countercurrent extractions, 1 grade of washing, 1 grade of test of stripping is carried out in 250mL separating funnel.
The method of a kind of Extraction of Uranium from acid, large proportion or lower concentration uranium solution of the present invention, in turn includes the following steps:
Step one: the acquisition of extraction stoste: fine ore granularity being less than 8mm is banked up, will pile with placed in series more, adopt dense H after 7 heap series connection
2sO
4spray from head heap, the leach liquor of bottom collection acquisition is piled by head, Xia Dui top is sprayed again with leach liquor, carry out successively, each heap pH of leaching solution is made to be 0.8 ~ 1.5, collect the leach liquor of tail heap bottom acquisition as extraction stoste, leaching cycle is 120 days, and in the extraction stoste of acquisition, the mass concentration of each element is U:1.7gL
-1; ∑ Fe:12.20gL
-1; Fe
2+: 4.60gL
-1; SiO
2: 0.24gL
-1; Al:2.79gL
-1; MnO:0.30gL
-1; MoO
3: 0.50gL
-1; CaO:2.80gL
-1; MgO:24.90gL
-1; SO
4 2-: 198.20gL
-1; PH:1.09; Redox potential is 404mv; Proportion is 1.456;
Step 2: organic phase makes the transition: take concentration as the Trifatty amine of 0.148mol/L be extraction agent, take volume fraction as the polyvalent alcohol of 4.4% be additive, by Trifatty amine: polyvalent alcohol: sulfonated kerosene is mixed into organic phase with volume ratio 15:10:180, then be the H of 70 ~ 80g/L according to organic phase and mass concentration
2sO
4be in a ratio of 5/1, duration of contact is that 3min carries out static phase-splitting, collects the organic phase obtained;
Step 3: extraction: extraction stoste is added in the organic phase made the transition, be in a ratio of 1/4 according to the organic phase that makes the transition with extraction stoste and carry out two-phase mixtures with magnetic stirrer in 250mL ground Erlenmeyer flask, duration of contact is 3min, temperature of reaction is 15 DEG C, obtains saturated organic phase with after the static phase-splitting of 250mL separating funnel;
Step 4: according to step 3, four counter-current extractions are repeated to the saturated organic phase that step 3 obtains;
Step 5: washing: be in a ratio of 5/1 according to saturated organic phase and service water, duration of contact is that 3min service water washs saturated organic phase;
Step 6: strip: take mass concentration as NaOH:22g/L and Na
2cO
3: the mixing solutions of 66g/L is as strippant, and be in a ratio of 6/1 according to saturated organic phase with extraction stoste and strip according to method in step 3 to the saturated organic phase after wash, duration of contact is 3min, and temperature of reaction is 15 DEG C, and what collection obtained contains U aqueous phase.
This test is carried out under room temperature 15 DEG C of conditions, and in saturated organic phase, U mass concentration is: 6.78g/L, U:2mg/L in raffinate, U:20mg/L in wash water, and turn one's coat middle U:31.88g/L, U:390mg/L in lean organic phase.
Embodiment 2
1 grade of transition, 5 stage countercurrent extractions, 1 grade of washing, 1 grade of test of stripping is carried out in 250mL separating funnel.
The method of a kind of Extraction of Uranium from acid, large proportion or lower concentration uranium solution of the present invention, in turn includes the following steps:
Step one: the acquisition of extraction stoste: fine ore granularity being less than 8mm is banked up, will pile with placed in series more, adopt dense H after 7 heap series connection
2sO
4spray from head heap, the leach liquor of bottom collection acquisition is piled by head, spray agent as lower heap continues spray, carry out successively, each heap pH of leaching solution is made to be 0.8 ~ 1.5, collect the leach liquor of tail heap bottom acquisition as extraction stoste, leaching cycle 120 days, the extraction stoste of acquisition consists of: U:510mgL
-1; ∑ Fe:9.41gL
-1; Fe
2+: 2.50gL
-1; SiO
2: 1.44gL
-1; Al:0.84gL
-1; MnO:0.10gL
-1; MoO
3: 0.90gL
-1; CaO:3.84gL
-1; MgO:22.35gL
-1; SO
4 2-: 200.51gL
-1; PH:1.88; Redox potential 398mv; Proportion 1.386;
Step 2: organic phase makes the transition: take concentration as the Trifatty amine of 0.108mol/L be extraction agent, take volume fraction as the polyvalent alcohol of 4.6% be additive, by Trifatty amine: polyvalent alcohol: sulfonated kerosene is mixed into organic phase with volume ratio 15:10:180, then be the H of 70 ~ 80g/L according to organic phase and mass concentration
2sO
4be in a ratio of 5/1, duration of contact is that 3min carries out static phase-splitting, collects the organic phase obtained;
Step 3: extraction: extraction stoste is added in the organic phase made the transition, be in a ratio of 1/6 according to the organic phase that makes the transition with extraction stoste and carry out two-phase mixtures with magnetic stirrer in 250mL ground Erlenmeyer flask, duration of contact is 3min, temperature of reaction is 15 DEG C, obtains saturated organic phase with after the static phase-splitting of 250mL separating funnel;
Step 4: according to step 3, five extractions are repeated to the saturated organic phase that step 3 obtains;
Step 5: washing: be in a ratio of 5/1 according to saturated organic phase and service water, duration of contact is that 3min service water washs saturated organic phase;
Step 6: strip: take mass concentration as NaOH:17g/L and Na
2cO
3: the mixing solutions of 70g/L is as strippant, and be in a ratio of 6/1 according to saturated organic phase with extraction stoste and strip according to method in step 3 to the saturated organic phase after wash, duration of contact is 3min, and temperature of reaction is 15 DEG C, and what collection obtained contains U aqueous phase.
This test is carried out under the condition of room temperature 15 DEG C, U mass concentration: 3.03g/L in saturated organic phase, U:2mg/L in raffinate, U:23mg/L in wash water, and turn one's coat middle U:13.70g/L, U:279mg/L in lean organic phase.
Compared with prior art, beneficial effect of the present invention is:
(1) labour intensity is reduced
Relative to ion exchange process, the present invention adopts extraction process, can greatly reduce maintenance of equipment expense, and simplifies the operation, reduces labor intensity.
(2) material agents is saved
Trifatty amine extraction process using Trifatty amine as extraction agent, not only reduces labour intensity, also reduces acid-base reaction frequently, reduces raw-material consumption.
1. alkaline consumption.Compared with ion-exchange, often produce one ton of product Trifatty amine extraction process and can save NaOH56.5%, save NaHCO
366.7%, calculate according to annual 85 tons of products, 123.6 ten thousand yuan can be saved;
2. acid consumption.The every tower of ion exchange tower can save 0.5t sulfuric acid, within 1 year, can save 210t, saves and is worth the ten thousand yuan/t=32 in 210t × 0.15 ten thousand yuan.
3. resin loss is reduced, annual saving economic worth 400,000.
(3) raising of the rate of recovery
Prior art ion exchange methods leaching return difference > 5%, adopts technical solution of the present invention to reach 3%, and by annual output resultant metal 85t, the rate of recovery 85%, year many Footwall drift 3t, is worth 2,100,000 yuan.Annual income about 3,570,000 yuan after transformation.
(4) to the value of full technique
Raffinate returns to stockyard for again preparing spray agent, and wherein uranium concentration drops to 10mg/L by 100mg/L, and surface, stockyard in winter can not add up a thick layer of Na simultaneously
2sO
4.Therefore can accelerate leaching process, shorten period of heap leaching.Meanwhile, product meets next step procedure calls, and product moisture < 30%, U > 60%, meets user's requirement.
(5) arrange outward without processing wastewater
Trifatty amine extraction process really achieve processing wastewater zero outside put.Per diem milling capacity 300T, qualifying liquid 300m is leached in daily output
3calculate: slag moisture 10%, be with the 30m that leakes water
3/ day, washing full bring into water be about stoste 5%, about 15m
3/ d; Transition, liquid reusable edible, also can join agent transition with raffinate, and transition, liquid brought water < 5m into
3/ day.So heap leaching solution reduces water yield > heap leaching solution increase the water yield, unnecessary waste water can not be produced.In addition, due to product moisture 30%, saltcake (Na
2sO
410H
2o) moisture 10%, so mother liquor amount < anti-dosage+precipitation dosage, unnecessary waste water can not be produced.
Above to embodiments of the invention to being explained in detail, above-mentioned embodiment is only optimum embodiment of the present invention, but the present invention is not limited to above-described embodiment, in the ken that those of ordinary skill in the art possess, can also make a variety of changes under the prerequisite not departing from present inventive concept.
Claims (9)
1.-kind from acid, large proportion or lower concentration uranium solution the method for Extraction of Uranium, in turn include the following steps:
Step one: the acquisition of extraction stoste: the rear dense H of Bian of fine ore many heaps series connection granularity being less than 8 millimeters
2sO
4carry out dump leaching, make pH of leaching solution be 0.8 ~ 1.5, leaching cycle is 120 days, and the leach liquor that collection obtains is as extraction stoste;
Step 2: organic phase makes the transition: be that the Trifatty amine of 0.1 ~ 0.18mol/L is extraction agent, take polyvalent alcohol as additive with mass concentration, by Trifatty amine: polyvalent alcohol: sulfonated kerosene is that 15:10:180 is mixed into organic phase with volume ratio, then be the H of 70 ~ 80g/L according to organic phase and mass concentration
2sO
4be in a ratio of 4/1 ~ 6/1, duration of contact is carry out static phase-splitting in 3 ~ 5 minutes, collects the organic phase obtained;
Step 3: extraction: extraction stoste is added in the organic phase made the transition, be in a ratio of 1/4 ~ 1/7 according to the organic phase that makes the transition with extraction stoste and carry out two-phase mixtures, duration of contact is 1 ~ 3 minute, and temperature of reaction is 13 ~ 40 DEG C, obtains saturated organic phase after static phase-splitting;
Step 4: according to step 3, one or many counter-current extraction is repeated to the saturated organic phase that step 3 obtains;
Step 5: washing: be in a ratio of 4/1 ~ 6/1 according to saturated organic phase and service water, duration of contact is wash saturated organic phase with service water for 3 ~ 5 minutes;
Step 6: strip: with the Na of the NaOH of mass concentration 15 ~ 25g/L and 60 ~ 80g/L
2cO
3mixing solutions as strippant, be in a ratio of 6/1 ~ 9/1 according to saturated organic phase with extraction stoste and strip according to method in step 3 to the saturated organic phase after wash, duration of contact is 3 ~ 4 minutes, and temperature of reaction is 13 ~ 40 DEG C, and what collection obtained contains U aqueous phase.
2. the method for a kind of Extraction of Uranium from acid, large proportion or lower concentration uranium solution as claimed in claim 1, is characterized in that: described step 2 to step 6 is carry out under the condition of 15 DEG C in temperature.
3. the method for a kind of Extraction of Uranium from acid, large proportion or lower concentration uranium solution as claimed in claim 1, is characterized in that: in described step one, the series connection of many heaps is 7 heaps series connection.
4. the method for a kind of Extraction of Uranium from acid, large proportion or lower concentration uranium solution as claimed in claim 1, it is characterized in that: the concentration of Trifatty amine described in step 2 is 0.15mol/L, described organic phase and mass concentration are the H of 70 ~ 80g/L
2sO
4be in a ratio of 4/1.
5. the method for a kind of Extraction of Uranium from acid, large proportion or lower concentration uranium solution as claimed in claim 1, is characterized in that: the organic phase that made the transition described in step 3 is in a ratio of 1/6 with extraction stoste and carries out two-phase mixtures, and duration of contact is 3 minutes.
6. the method for a kind of Extraction of Uranium from acid, large proportion or lower concentration uranium solution as claimed in claim 1, is characterized in that: in described step 4, the number of times of re-extract is three times, four times or five counter-current extractions.
7. the method for a kind of Extraction of Uranium from acid, large proportion or lower concentration uranium solution as claimed in claim 1, it is characterized in that: in described step 5, saturated organic phase and service water are in a ratio of 5/1, duration of contact is 3 minutes.
8. the method for a kind of Extraction of Uranium from acid, large proportion or lower concentration uranium solution as claimed in claim 1, is characterized in that: in described step 6, strippant is NaOH:22g/L and Na
2cO
3: the mixing solutions of 66g/L.
9. the method for a kind of Extraction of Uranium from acid, large proportion or lower concentration uranium solution as claimed in claim 1, is characterized in that: in described step 6, saturated organic phase is in a ratio of 6/1 with extraction stoste, and duration of contact is 3 minutes.
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| CN105567962B (en) * | 2015-12-29 | 2017-09-26 | 核工业北京化工冶金研究院 | A kind of back extraction method and device for loading uranium Trifatty amine |
| CN112553484B (en) * | 2020-09-07 | 2022-09-20 | 核工业北京化工冶金研究院 | Method for improving flow benefit of uranium extraction by triple-fatty amine leaching |
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| US4610852A (en) * | 1981-12-14 | 1986-09-09 | Hitachi, Ltd. | Process for stripping uranium |
| CN101886175A (en) * | 2010-07-02 | 2010-11-17 | 湘潭市天添矿业有限公司 | Method for producing diuranate by extracting uranium from rare earth slag containing uranium |
| CN102021330A (en) * | 2010-12-23 | 2011-04-20 | 核工业北京化工冶金研究院 | Leaching method capable of reducing leached acid consumption of uranium ores |
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2012
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4610852A (en) * | 1981-12-14 | 1986-09-09 | Hitachi, Ltd. | Process for stripping uranium |
| CN101886175A (en) * | 2010-07-02 | 2010-11-17 | 湘潭市天添矿业有限公司 | Method for producing diuranate by extracting uranium from rare earth slag containing uranium |
| CN102021330A (en) * | 2010-12-23 | 2011-04-20 | 核工业北京化工冶金研究院 | Leaching method capable of reducing leached acid consumption of uranium ores |
Non-Patent Citations (1)
| Title |
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| 用三脂肪胺从煤灰酸浸矿浆中直接萃取铀的研究与应用;付子忠等;《湿法冶金》;20090331;第28卷(第1期);41-44 * |
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