CN103849764A - Method for extracting uranium from acidic, high-specific-gravity or low-concentration uranium ore extraction solution - Google Patents
Method for extracting uranium from acidic, high-specific-gravity or low-concentration uranium ore extraction solution Download PDFInfo
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- CN103849764A CN103849764A CN201210514137.XA CN201210514137A CN103849764A CN 103849764 A CN103849764 A CN 103849764A CN 201210514137 A CN201210514137 A CN 201210514137A CN 103849764 A CN103849764 A CN 103849764A
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Abstract
The invention relates to hydrometallurgical extraction technology of uranium and aims at providing a method for extracting uranium from acidic, high-specific-gravity or low-concentration uranium ore extraction solution, to overcome the difficult concentration problem of an acidic, high-specific-gravity or low-concentration uranium solution, so as to improve the yield and reduce the cost. According to the method provided by the invention, tri-fatty amine is used as an extractant to extract an acidic, high-specific-gravity or low-concentration complicated uranium solution, polyhydric alcohol is used as an additive to perfect the physical properties of the extractant, and the effect of extracting uranium from the acidic, high-specific-gravity or low-concentration uranium ore extraction solution is good.
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, how low-grade, multicomponent refractory mineral need to be exploited processing again, thereby causes in uranium ore extraction stoste uranium concentration generally lower, and composition becomes increasingly complex.Except containing conventional SO
4 2-, outside the impurity such as iron, phosphorus, aluminium, manganese, vanadium, calcium, magnesium, silicon, molybdenum, also contain 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, less for the research of acid, large proportion or lower concentration uranium ore extraction stoste concentration technique specially, become the technical bottleneck that restricts production capacity.
Concentrated employing ion exchange process and the extraction process of China's most of uranium ore extraction stoste.Ion exchange method be mainly applicable to relatively large enterprise from low uranium concentration, contain a large amount of impurity uranium ore extraction stoste extract high concentration uranium, extraction process is mainly applicable to the uranium ore extraction stoste of medium and small sized enterprises and higher concentration.From the viewpoint of economic benefit, the boundary that the applicable uranium ore of ion exchange method and extraction process extracts original liquid concentration is 1g/L.But ion exchange method equipment complexity, spoilage is high, labour intensity is large, and there is the problems such as processing wastewater, discharging any waste liquor amount be excessive, and in neutralization, transformation process, there are a large amount of metals to return to stockyard, the main technique rate of recovery and heap leaching rate had a strong impact on, for example a large amount of Na
2sO
4return the crystallization of dump leaching field, affect stockyard leaching yield.In the time extracting original liquid concentration lower than 1g/L, extraction point is compared slow, and organic solvent consumption is larger, in the time processing acidity, large proportion or lower concentration uranium ore extraction stoste, should not adopt.This becomes extraction cells operation and processes the difficulties in acid, large proportion or lower concentration extraction stoste.
Extraction agent is the key issue of abstraction technique.From 1945 tributylphosphate (TBP) first as since uranium extraction agent, be widely used as by countries in the world the extraction agent that in core combustion aftertreatment, thorium, uranium separate so far.But due to TPB self-defect, people find more preferably substitute and synergist always, to reach the object of further raising extracting power.But extraction agent of the prior art just uranium ore single for composition, higher concentration extracts stoste, but often has research and the report of experimental basis and application example for the processing of acid, large proportion or lower concentration extraction stoste.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 costs, and improves the object of production capacity.
Summary of the invention
The object of the invention is the concentrated problem of difficulty for acid, large proportion or lower concentration uranium solution, provide a kind of from acid, large proportion or lower concentration uranium ore extraction stoste the method for Extraction of Uranium, to improve production capacity and to reduce costs.
The technical solution used in the present invention is: a kind of from acid, large proportion or lower concentration uranium solution the method for Extraction of Uranium, in turn include 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 1: the acquisition of extraction stoste: the fine ore that granularity is less than to 8mm is banked up, adopts dense H after many heap series connection
2sO
4carry out dump leaching, making pH of leaching solution is 0.8～1.5, and leaching cycle is 120 days, collects the leach liquor obtaining as extraction stoste;
Step 2: organic phase makes the transition: the Trifatty amine take concentration as 0.1～0.18 mol/L is as extraction agent, take polyvalent alcohol as additive, by Trifatty amine: polyvalent alcohol: sulfonated kerosene is mixed into organic phase take volume ratio as 15:10:180, then the H that is 70～80g/L according to organic phase and mass concentration
2sO
4be in a ratio of 4/1～6/1, be that 3～5min carries out static phase-splitting duration of contact, collects the organic phase obtaining;
Step 3: extraction: extraction stoste is added in the organic phase having made the transition, be in a ratio of 1/4～1/7 and carry out two-phase and mix with extracting stoste according to the organic phase that makes the transition, be 1～3min duration of contact, and temperature of reaction is 13～40 ℃, obtains saturated organic phase after static phase-splitting;
Step 4: the saturated organic phase that step 3 is obtained repeats one or many counter-current extraction 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, be that 3～5min service water washs saturated organic phase duration of contact;
Step 6: strip: the NaOH take mass concentration as 15～25 g/L and the Na of 60～80 g/L
2cO
3mixing solutions as strippant, be in a ratio of 6/1～9/1 pair of saturated organic phase after washing according to saturated organic phase with extraction stoste and strip according to method in step 3, be 3～4min duration of contact, temperature of reaction is 13～40 ℃, collect obtain containing U water.
The present invention extracts acid, large proportion or the complicated uranium solution of lower concentration take Trifatty amine as extraction agent, improves the physicals of extraction agent take polyvalent alcohol as additive, respond well for Extraction of Uranium from acid, large proportion or lower concentration extraction stoste.Step 1 is compared with ion-exchange, cost-saving 30～45%, and the rate of recovery has improved 2～3%, and production capacity has improved 2.5～3.5%; The water 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
Below in conjunction with specific embodiment to the present invention a kind of from acid, large proportion or lower concentration uranium solution the method for Extraction of Uranium be further described.
Embodiment 1
In 250mL separating funnel, carry out 1 grade of transition, 4 stage countercurrent extractions, 1 grade of washing, 1 grade of test of stripping.
Of the present invention a kind of from acid, large proportion or lower concentration uranium solution the method for Extraction of Uranium, in turn include the following steps:
Step 1: the acquisition of extraction stoste: the fine ore that granularity is less than to 8mm is banked up, will pile with pipeline series connection more, after 7 heap series connection, adopt dense H
2sO
4start spray from head heap, pile bottom by head and collect the leach liquor obtaining, spray Xia Dui top with leach liquor again, carry out successively, making each heap pH of leaching solution is 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 transition: the Trifatty amine take concentration as 0.148 mol/L is as extraction agent, polyvalent alcohol take volume fraction as 4.4% are as additive, by Trifatty amine: polyvalent alcohol: sulfonated kerosene is mixed into organic phase with volume ratio 15:10:180, then the H that is 70～80g/L according to organic phase and mass concentration
2sO
4be in a ratio of 5/1, be that 3min carries out static phase-splitting duration of contact, collects the organic phase obtaining;
Step 3: extraction: extraction stoste is added in the organic phase having made the transition, be in a ratio of 1/4 according to the organic phase that makes the transition with extraction stoste carries out two-phase with magnetic stirrer and mixes in 250mL ground Erlenmeyer flask, be 3min duration of contact, temperature of reaction is 15 ℃, with obtaining saturated organic phase after the static phase-splitting of 250mL separating funnel;
Step 4: the saturated organic phase that step 3 is obtained repeats counter-current extraction four times according to step 3;
Step 5: washing: be in a ratio of 5/1 according to saturated organic phase and service water, be that 3min service water washs saturated organic phase duration of contact;
Step 6: strip: take mass concentration as NaOH:22 g/L and Na
2cO
3: the mixing solutions of 66 g/L, as strippant, is in a ratio of 6/1 pair of saturated organic phase after washing according to saturated organic phase with extraction stoste and strips according to method in step 3, and be 3min duration of contact, and temperature of reaction is 15 ℃, and what collection obtained contains U water.
This test is carried out under 15 ℃ of conditions of room temperature, and in saturated organic phase, U mass concentration is: 6.78g/L, U:2mg/L in raffinate, U:20mg/L in wash water, the middle U:31.88g/L that turns one's coat, U:390mg/L in lean organic phase.
Embodiment 2
In 250 mL separating funnels, carry out 1 grade of transition, 5 stage countercurrent extractions, 1 grade of washing, 1 grade of test of stripping.
Of the present invention a kind of from acid, large proportion or lower concentration uranium solution the method for Extraction of Uranium, in turn include the following steps:
Step 1: the acquisition of extraction stoste: the fine ore that granularity is less than to 8mm is banked up, will pile with pipeline series connection more, after 7 heap series connection, adopt dense H
2sO
4start spray from head heap, pile bottom by head and collect the leach liquor obtaining, spray agent as lower heap continues spray, carry out successively, making each heap pH of leaching solution is 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 transition: the Trifatty amine take concentration as 0.108 mol/L is as extraction agent, polyvalent alcohol take volume fraction as 4.6% are as additive, by Trifatty amine: polyvalent alcohol: sulfonated kerosene is mixed into organic phase with volume ratio 15:10:180, then the H that is 70～80g/L according to organic phase and mass concentration
2sO
4be in a ratio of 5/1, be that 3min carries out static phase-splitting duration of contact, collects the organic phase obtaining;
Step 3: extraction: extraction stoste is added in the organic phase having made the transition, be in a ratio of 1/6 according to the organic phase that makes the transition with extraction stoste carries out two-phase with magnetic stirrer and mixes in 250mL ground Erlenmeyer flask, be 3min duration of contact, temperature of reaction is 15 ℃, with obtaining saturated organic phase after the static phase-splitting of 250mL separating funnel;
Step 4: the saturated organic phase that step 3 is obtained repeats five extractions according to step 3;
Step 5: washing: be in a ratio of 5/1 according to saturated organic phase and service water, be that 3min service water washs saturated organic phase duration of contact;
Step 6: strip: take mass concentration as NaOH:17 g/L and Na
2cO
3: the mixing solutions of 70g/L, as strippant, is in a ratio of 6/1 pair of saturated organic phase after washing according to saturated organic phase with extraction stoste and strips according to method in step 3, and be 3min duration of contact, and temperature of reaction is 15 ℃, and what collection obtained contains U water.
This test is carried out under the condition of 15 ℃ of room temperatures, U mass concentration: 3.03g/L in saturated organic phase, U:2mg/L in raffinate, U:23mg/L in wash water, the middle U:13.70g/L that turns one's coat, U:279mg/L in lean organic phase.
Compared with prior art, beneficial effect of the present invention is:
(1) reduce labour intensity
With respect 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) save material reagent
Trifatty amine extraction process using Trifatty amine as extraction agent, has not only reduced labour intensity, also reduces acid-base reaction frequently, has reduced raw-material consumption.
1. alkaline consumption.Compared with ion-exchange, one ton of product Trifatty amine extraction process of every production can be saved NaOH 56.5%, saves NaHCO
366.7%, calculate according to annual 85 tons of products, can save 123.6 ten thousand yuan;
2. acid consumption.The every tower of ion exchange tower can be saved 0.5t sulfuric acid, within 1 year, can save 210t, saves and is worth ten thousand yuan/t=320,000 yuan, 210t × 0.15.
3. reduce resin loses, save every year economic worth 400,000.
(3) raising of the rate of recovery
Prior art intermediate ion exchange process is soaked return difference > 5%, adopts technical solution of the present invention can reach 3%, by producing resultant metal 85t per year, and the rate of recovery 85%, year metal 3t that reclaim, are worth 2,100,000 yuan more.Approximately 3,570,000 yuan of annual incomes after transformation.
(4) value to 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 operation requirement, the moisture < 30% of product, and U > 60%, meets user's requirement.
(5) arrange outward without processing wastewater
Trifatty amine extraction process has really been realized zero outer putting of processing wastewater.Per diem milling capacity 300T, qualifying liquid 300m is leached in daily output
3calculate: slag is moisture 10% band 30 m that leak 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 was brought water < 5m into
3/ day.So heap leaching solution reduces water yield > heap leaching solution and increases the water yield, can not produce unnecessary waste water.In addition, because product is moisture 30%, saltcake (Na
2sO
410H
2o) moisture 10%, so the anti-dosage+precipitation of mother liquor amount < dosage can not produce unnecessary waste water.
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 possessing those of ordinary skills, can also under the prerequisite that does not depart from aim of the present invention, make a variety of changes.
Claims (10)
1. for an extraction agent for acid, large proportion or lower concentration uranium solution Extraction of Uranium, comprise that concentration is the Trifatty amine of 0.1～0.18 mol/L and the polyvalent alcohol that volume fraction is 44%～46%.
2. application rights requires a method for the extraction agent Extraction of Uranium from acid, large proportion or lower concentration uranium solution described in 1, in turn includes the following steps:
Step 1: the acquisition of extraction stoste: the fine ore that granularity is less than to 8 millimeters is piled the rear dense H of employing of series connection more
2sO
4carry out dump leaching, making pH of leaching solution is 0.8～1.5, and leaching cycle is 120 days, collects the leach liquor obtaining as extraction stoste;
Step 2: organic phase makes the transition: the Trifatty amine take mass concentration as 0.1～0.18 mol/L is as extraction agent, take polyvalent alcohol as additive, by Trifatty amine: polyvalent alcohol: sulfonated kerosene is mixed into organic phase take volume ratio as 15:10:180, then the H that is 70～80g/L according to organic phase and mass concentration
2sO
4be in a ratio of 4/1～6/1, be within 3～5 minutes, to carry out static phase-splitting duration of contact, collects the organic phase obtaining;
Step 3: extraction: extraction stoste is added in the organic phase having made the transition, be in a ratio of 1/4～1/7 and carry out two-phase and mix with extracting stoste according to the organic phase that makes the transition, be 1～3 minute duration of contact, and temperature of reaction is 13～40 ℃, obtains saturated organic phase after static phase-splitting;
Step 4: the saturated organic phase that step 3 is obtained repeats one or many counter-current extraction according to step 3;
Step 5: washing: be in a ratio of 4/1～6/1 according to saturated organic phase and service water, be with service water, saturated organic phase to be washed for 3～5 minutes duration of contact;
Step 6: strip: with the NaOH of mass concentration 15～25 g/L and the Na of 60～80 g/L
2cO
3mixing solutions as strippant, be in a ratio of 6/1～9/1 pair of saturated organic phase after washing according to saturated organic phase with extraction stoste and strip according to method in step 3, be 3～4 minutes duration of contact, temperature of reaction is 13～40 ℃, collect obtain containing U water.
As claimed in claim 2 a kind of from acid, large proportion or lower concentration uranium solution the method for Extraction of Uranium, it is characterized in that: described step 2 is to carry out under the condition of 15 ℃ in temperature to step 6.
As claimed in claim 2 a kind of from acid, large proportion or lower concentration uranium solution the method for Extraction of Uranium, it is characterized in that: in described step 1, many heap series connection are 7 heaps series connection.
As claimed in claim 2 a kind of from acid, large proportion or lower concentration uranium solution the method for Extraction of Uranium, it is characterized in that: the concentration of Trifatty amine described in step 2 is 0.15mol/L, the H that described organic phase and mass concentration are 70～80g/L
2sO
4be in a ratio of 4/1.。
As claimed in claim 2 a kind of from acid, large proportion or lower concentration uranium solution the method for Extraction of Uranium, it is characterized in that: the organic phase that made the transition described in step 3 is in a ratio of 1/6 and carries out two-phase and mix with extracting stoste, and be 3 minutes duration of contact.
As claimed in claim 2 a kind of from acid, large proportion or lower concentration uranium solution the method for Extraction of Uranium, it 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.
As claimed in claim 2 a kind of from acid, large proportion or lower concentration uranium solution the method for Extraction of Uranium, it is characterized in that: in described step 5, saturated organic phase and service water are in a ratio of 5/1, be 3 minutes duration of contact.
As claimed in claim 2 a kind of from acid, large proportion or lower concentration uranium solution the method for Extraction of Uranium, it is characterized in that: in described step 6, strippant is NaOH:22 g/L and Na
2cO
3: the mixing solutions of 66 g/L.
As claimed in claim 2 a kind of from acid, large proportion or lower concentration uranium solution the method for Extraction of Uranium, it is characterized in that: in described step 6, saturated organic phase is in a ratio of 6/1 with extraction stoste, and be 3 minutes duration of contact.
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Cited By (2)
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| CN105567962A (en) * | 2015-12-29 | 2016-05-11 | 核工业北京化工冶金研究院 | Reextraction method and device of uranium loaded trifatty amine |
| CN112553484A (en) * | 2020-09-07 | 2021-03-26 | 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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| CN105567962A (en) * | 2015-12-29 | 2016-05-11 | 核工业北京化工冶金研究院 | Reextraction method and device of uranium loaded trifatty amine |
| 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 |
| CN112553484A (en) * | 2020-09-07 | 2021-03-26 | 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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