CN102031369B - Method for extracting uranium by using ion exchange fixed tower under alternate Ph condition - Google Patents

Method for extracting uranium by using ion exchange fixed tower under alternate Ph condition Download PDF

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CN102031369B
CN102031369B CN2010105689506A CN201010568950A CN102031369B CN 102031369 B CN102031369 B CN 102031369B CN 2010105689506 A CN2010105689506 A CN 2010105689506A CN 201010568950 A CN201010568950 A CN 201010568950A CN 102031369 B CN102031369 B CN 102031369B
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uranium
drip washing
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resin
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CN102031369A (en
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李伟才
周根茂
刘超
邓舜勤
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Beijing Research Institute of Chemical Engineering and Metallurgy of CNNC
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Abstract

The invention relates to a method for extracting uranium by using an ion exchange fixed tower, in particular to a method for extracting uranium by using an ion exchange fixed tower under the alternate Ph condition. The method comprises the steps of absorbing uranium by barren resin and eluting the uranium-carried resin to obtain uranium, wherein the step of eluting the uranium-carried resin to obtain uranium also comprises the following stages of elution neutralization, qualified liquid elution, first barren elution and second barren elution. In the stage of elution neutralization, an alkali eluent is used to neutralize residual acid in the uranium-carried resin, and the feeding mode is lower liquid feeding; in the stage of qualified liquid elution, the feeding mode is upper liquid feeding; in the stage of first barren elution, the feeding mode is upper liquid feeding, and the effluent liquid is a first barren solution; and in the stage of second barren elution, the feeding mode is upper liquid feeding, and the effluent liquid is a second barren solution. The invention increases elution efficiency and shortens elution volume by dividing the step of eluting the uranium-carried resin to obtain uranium into the stages of elution neutralization and qualified liquid elution and by respectively using the upper liquid feeding mode and the lower liquid feeding mode.

Description

A kind of under the potential of hydrogen alternation condition ion-exchange fixed tower put forward the uranium method
Technical field
The invention belongs to the uranium method of putting forward of using the ion-exchange fixed tower, be specifically related to a kind of under the solution acid alkalinity alternation condition ion-exchange fixed tower put forward the uranium method.
Background technology
Adopt ion exchange method from leach liquor, to extract uranium; for the zone that does not have the particular surroundings protection to require; it generally is the kind of selecting eluent according to the characteristic of ore leach liquor that ion exchange method is carried uranium; namely from acid leaching solution, reclaim extraction uranium and adopt acid eluent, from neutrality or weakly alkaline solution, reclaim and extract uranium employing neutrality or weakly alkaline eluent.At present, China's uranium mill great majority adopt acid system to leach---anionite-exchange resin absorption---acid villaumite or acid nitrate drip washing---depositing technology.Wherein the mode of single upper feeding or lower charging is adopted in the operation of ion exchange tower, is qualifying liquid when the uranium concentration of drip washing effluent liquid is higher can reach the subsequent technique service requirements time, is called a barren solution and two barren solutions when uranium concentration drops to certain value.
---the technical process of anionite-exchange resin absorption---acid villaumite or acid nitrate drip washing---precipitation product that the employing acid system leaches, adopted acid villaumite or acid nitrate to carry out desorb owing to carry the uranium resin, in the process water working cycle, can cause chlorine root or nitrate radical constantly to accumulate, affect the absorption of follow-up ion exchange resin, and adsorption tail liquid need efflux.Strict or without the zone of receiving water body, this puies forward the relevant requirements that the uranium technical process can't reach national environmental protection for environmental protection requirement.
If adopt carbonate that the ion exchange resin that extracts uranium from acid leaching solution is carried out drip washing, can realize the process water closed cycle, but at the drip washing initial stage, the acid-base neutralisation reaction can produce a large amount of CO 2Bubble is processed improperly in actual mechanical process, can cause the damages such as pipeline, equipment, brings great potential safety hazard to production.
Summary of the invention
The object of the invention provides a kind of ion-exchange fixed tower under the potential of hydrogen alternation condition that improves elution efficiency, shortening elution volume and puies forward the method for uranium.
The technical solution adopted in the present invention is:
A kind of under the solution acid alkalinity alternation condition ion-exchange fixed tower put forward the uranium method, comprising: poor resin absorption uranium step and carry a uranium resin Elution of Uranium step, wherein:
Carrying uranium resin Elution of Uranium step comprises again successively:
The drip washing neutralization stage: use the spent acid in the alkaline eluent neutralization year uranium resin, feeding manner is lower feed liquor;
The drip washing qualifying liquid stage: feeding manner is upper feed liquor;
The one poor stage of drip washing: feeding manner is upper feed liquor, and effluent liquid is a barren solution;
The two poor stages of drip washing: feeding manner is upper feed liquor, and effluent liquid is two barren solutions.
Aforesaid a kind of under the solution acid alkalinity alternation condition ion-exchange fixed tower put forward the uranium method, wherein: described poor resin absorption uranium step adopts the ion-exchange fixed tower to reclaim uranium from acid leaching solution, feeding manner is lower feed liquor, when effluent liquid uranium concentration and stoste uranium concentration poor during at 0～20mg/L, with solution emptying in the ion-exchange fixed tower, poor resin absorption uranium step finishes.
Aforesaid a kind of under the solution acid alkalinity alternation condition ion-exchange fixed tower put forward the uranium method, wherein: described poor resin absorption uranium step adopts the mode of a plurality of ion-exchange fixed tower series connection to carry out.
Aforesaid a kind of under the solution acid alkalinity alternation condition ion-exchange fixed tower put forward the uranium method, wherein: in the described two poor stages of drip washing, when drip washing effluent liquid uranium concentration during less than 0.2g/L, drip washing finishes, the solution in the emptying ion-exchange fixed tower.
Aforesaid a kind of under the solution acid alkalinity alternation condition ion-exchange fixed tower put forward the uranium method, wherein: in described drip washing neutralization stage, when the pH of effluent liquid value was in 2.5～8.0, the drip washing neutralization stage finished to enter the drip washing qualifying liquid stage.
Aforesaid a kind of under the solution acid alkalinity alternation condition ion-exchange fixed tower put forward the uranium method, wherein: in the described drip washing qualifying liquid stage, adopt to contain CO 3 2-Eluent or a barren solution of last tower make eluent and carry out drip washing to carrying a uranium resin.
Aforesaid a kind of under the solution acid alkalinity alternation condition ion-exchange fixed tower put forward the uranium method, wherein: adopt in the one poor stage of described drip washing to contain CO 3 2-Eluent or two barren solutions of last tower make eluent and carry out drip washing to carrying a uranium resin.
Aforesaid a kind of under the solution acid alkalinity alternation condition ion-exchange fixed tower put forward the uranium method, wherein: adopt in the two poor stages of described drip washing to contain CO 3 2-Eluent carry out drip washing to carrying a uranium resin.
Aforesaid a kind of under the solution acid alkalinity alternation condition ion-exchange fixed tower put forward the uranium method, wherein: in the described drip washing qualifying liquid stage, when the uranium concentration of effluent liquid was reduced to 1～10g/L, the described drip washing qualifying liquid stage finished, and enters the one poor stage of drip washing.
Aforesaid a kind of under the solution acid alkalinity alternation condition ion-exchange fixed tower put forward the uranium method, wherein: in the described one poor stage of drip washing, when the uranium concentration of effluent liquid was reduced to 0.5～1g/L, the one poor stage of described drip washing finished, and enters the two poor stages of drip washing.
The invention has the beneficial effects as follows:
1. the present invention is by dividing drip washing neutralization stage and drip washing qualifying liquid stage in carrying uranium resin Elution of Uranium step, and feed liquor and upper feed liquor mode are descended in employing respectively, help the unobstructed discharge of a large amount of gases of production in the ion exchange tower, can avoid in lessivation, producing " dead angle " owing to gas blocks up, and help to improve elution efficiency, shorten elution volume.
2. the present invention has improved the effect of adsorption uranium by the mode that adopts the multitower series connection in poor resin absorption uranium step.
3. the present invention by distinguishing four-stage at specified range point, helps to improve elution efficiency in carrying uranium resin Elution of Uranium step, shortens elution volume.
4. the present invention is by adopting a barren solution of last tower and two barren solutions to make eluent in drip washing qualifying liquid stage and one poor stage of drip washing, efficient and effect that can Effective Raise ion-exchange.
Description of drawings
Fig. 1 be provided by the invention a kind of under the potential of hydrogen alternation condition ion-exchange fixed tower carry the schema of uranium method;
Fig. 2 is that ion-exchange ADSORPTION IN A FIXED BED and drip washing pipeline are arranged synoptic diagram;
Among Fig. 2: 1,2 ...., the 8th, the ion-exchange fixed tower; The 9th, lower fluid inlet valve; The 10th, upper fluid inlet valve; Dotted line represents the string pipe, and the line expression shares pipe.
Embodiment
Below in conjunction with drawings and Examples a kind of method that the ion-exchange fixed tower is carried uranium under the potential of hydrogen alternation condition of the present invention is introduced:
As shown in Figure 1, a kind of method that the ion-exchange fixed tower is carried uranium under the potential of hydrogen alternation condition is divided following step:
(1) poor resin absorption uranium step: adopt the ion-exchange fixed tower from acid leaching solution, to reclaim uranium, the acid leaching solution feeding manner is lower feed liquor, resin adsorbs the uranium in the acid leaching solution, in this process, when the effluent liquid uranium concentration after upon adsorption is basic identical with the stoste uranium concentration before the absorption (both concentration differences are when 0～20mg/L), can think that ion exchange resin absorption is saturated, and with solution emptying in the ion exchange tower, in order to drip washing.
In the present embodiment, this step adopts 3 towers series connection absorption, take 1,2, No. 3 tower as the example narration: at first adsorb stoste (namely being acid leaching solution) and enter the tower internal adsorption from No. 1 tower bottom, No. 1 tower adsorption tail liquid shares pipe by adsorbing, absorption string tower pipe enters the tower internal adsorption from No. 2 tower bottoms, No. 2 tower adsorption tail liquids share pipe by adsorbing, absorption string tower pipe enters the tower internal adsorption from No. 3 tower bottoms, and No. 3 adsorption tail liquids share pipe and directly enter the outer comb of adsorption tail liquid by adsorbing.Also can according to circumstances change the quantity of columns in series, when the quantity of columns in series was more, tail washings concentration was lower, and adsorption effect is better.
(2) carry uranium resin Elution of Uranium step:
1) drip washing neutralization stage: owing to carry uranium resin (or being ion exchange resin) system for acid, at the drip washing initial stage, (contain CO with alkaline mother liquor of precipitation of ammonium 3 2-Eluent with sodium hydroxide) resin is carried out drip washing, in and remaining spent acid in the resin, feeding manner is lower feed liquor, makes the acid-base neutralisation reaction produce a large amount of CO 2Bubble is conducive to efflux (discharging from the vent valve of ion-exchange fixed tower cat head).Find that by the drip washing test neutralization stage in the lessivation is to the transition in qualifying liquid stage, the pH value of its effluent liquid can change (pH rises to 2.5～8.0), therefore is easier to control transformation point.
2) the drip washing qualifying liquid stage: after the drip washing neutralization stage finishes, adopt to contain CO 3 2-Eluent carry out drip washing to carrying a uranium resin, feeding manner changes upper feed liquor into by original lower feed liquor.The uranium concentration of effluent liquid is higher (to reach 10～30g/L), and CO 3 2-Concentration is lower (to be reached 20～30g/L) and is the drip washing qualifying liquid.
3) the one poor stage of drip washing: when the uranium concentration of effluent liquid is reduced to 1～10g/L, effluent liquid is a barren solution of current tower, and feeding manner is upper feed liquor during drip washing; Employing contains CO 3 2-Eluent carry out drip washing to carrying a uranium resin.
4) the two poor stages of drip washing: when the uranium concentration of effluent liquid is reduced to 0.5～1g/L, adopt to contain CO 3 2-Eluent carry out drip washing to carrying a uranium resin, feeding manner is upper feed liquor, effluent liquid is two barren solutions of current tower.Treat that drip washing effluent liquid uranium concentration is down to below the 0.2g/L, drip washing finishes, and the solution in the emptying ion exchange tower, in order to absorption.
As shown in Figure 2, usually adopt the mode of a plurality of ion-exchange fixed tower series connection in carrying uranium resin Elution of Uranium step, then in the drip washing qualifying liquid stage, a rear tower can adopt a barren solution of last tower to make eluent; In the one poor stage of drip washing, a rear tower can adopt two barren solutions of last tower to make eluent.
At first open the lower fluid inlet valve 9 of each ion-exchange fixed tower, alkaline mother liquor of precipitation of ammonium is entered from tower bottom carry out acid-base neutralisation in the tower; The structure of described ion-exchange fixed tower is those skilled in the art's common practise;
After the neutralization stage of each tower finishes, close lower fluid inlet valve 9, meanwhile open upper fluid inlet valve 10, one barren solution of last tower enters from cat head by the shared pipe of drip washing (line among Fig. 2) as eluent carries out drip washing to carrying a uranium resin, this stage is the drip washing qualifying liquid stage, because there is not its last tower in No. 1 tower, thereby the eluent that uses is the CO that contains of external world's adding 3 2-Eluent;
To any tower, when the uranium concentration of effluent liquid was reduced to 1～10g/L, this tower entered the one poor stage of drip washing, use two barren solutions of last tower as eluent, feeding manner is upper feeding, because there is not its last tower in No. 1 tower, thereby the eluent that uses is the CO that contains of external world's adding 3 2-Eluent;
To any tower, when the uranium concentration of effluent liquid was reduced to 0.5～1g/L, this tower entered the two poor stages of drip washing, adopted to contain CO 3 2-Eluent carry out drip washing to carrying a uranium resin, feeding manner is upper feed liquor;
When the effluent liquid uranium concentration is down to below the 0.2g/L, drip washing finishes, the solution in the emptying ion exchange tower.Certainly, those skilled in the art also can change according to the uranium concentration that will obtain the uranium concentration value of each weight break point.But above-mentioned value range can obtain larger effluent liquid uranium concentration under shorter drip washing time and less elution volume.
The drip washing test has been carried out respectively in lower charging behind single upper feeding, single lower charging, the first upper feeding, the results are shown in following table:
Table 1 drip washing test-results
Figure BDA0000035567380000071
From above result as can be known, adopt the feed liquor mode of first upper feeding, rear lower charging, use less accumulative total elution volume can make liquid uranium flow out fast (be that effluent liquid uranium peak value is large, end value is little), help to improve elution efficiency, shorten the drip washing time and reduce elution volume.

Claims (5)

  1. One kind under the solution acid alkalinity alternation condition ion-exchange fixed tower put forward the uranium method, comprising: poor resin absorption uranium step and carry a uranium resin Elution of Uranium step is characterized in that:
    Described poor resin absorption uranium step adopts the ion-exchange fixed tower to reclaim uranium from acid leaching solution, feeding manner is lower feed liquor, poor during at 0～20mg/L when effluent liquid uranium concentration and stoste uranium concentration, with solution emptying in the ion-exchange fixed tower, poor resin absorption uranium step finishes;
    Carrying uranium resin Elution of Uranium step comprises again successively:
    Drip washing neutralization stage: use to contain CO 3 2-The spent acid in the uranium resin is carried in neutralization with the eluent of sodium hydroxide, and feeding manner is lower feed liquor; In described drip washing neutralization stage, when the pH of effluent liquid value was in 2.5～8.0, the drip washing neutralization stage finished to enter the drip washing qualifying liquid stage;
    The drip washing qualifying liquid stage: feeding manner is upper feed liquor; Employing contains CO 3 2-Eluent or a barren solution of last tower make eluent and carry out drip washing to carrying a uranium resin;
    The one poor stage of drip washing: feeding manner is upper feed liquor, and effluent liquid is a barren solution; Employing contains CO 3 2-Eluent or two barren solutions of last tower make eluent and carry out drip washing to carrying a uranium resin;
    The two poor stages of drip washing: feeding manner is upper feed liquor, and effluent liquid is two barren solutions; Employing contains CO 3 2-Eluent carry out drip washing to carrying a uranium resin.
  2. According to claim 1 a kind of under the solution acid alkalinity alternation condition ion-exchange fixed tower put forward the uranium method, it is characterized in that: described poor resin absorption uranium step adopts the mode of a plurality of ion-exchange fixed tower series connection to carry out.
  3. According to claim 1 a kind of under the solution acid alkalinity alternation condition ion-exchange fixed tower put forward the uranium method, it is characterized in that: in the described two poor stages of drip washing, when drip washing effluent liquid uranium concentration during less than 0.2g/L, drip washing finishes, the solution in the emptying ion-exchange fixed tower.
  4. According to claim 1 a kind of under the solution acid alkalinity alternation condition ion-exchange fixed tower put forward the uranium method, it is characterized in that: in the described drip washing qualifying liquid stage, when the uranium concentration of effluent liquid was reduced to 1～10g/L, the described drip washing qualifying liquid stage finished, and enters the one poor stage of drip washing.
  5. According to claim 1 a kind of under the solution acid alkalinity alternation condition ion-exchange fixed tower put forward the uranium method, it is characterized in that: in the described one poor stage of drip washing, when the uranium concentration of effluent liquid was reduced to 0.5～1g/L, the described one poor stage of drip washing finished, and enters the two poor stages of drip washing.
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CN103204601B (en) * 2013-04-23 2014-05-07 清华大学 Wastewater treatment method
CN111020190B (en) * 2019-12-10 2021-10-22 核工业北京化工冶金研究院 Process linking method for extracting uranium by two-step ion exchange method
CN112680606B (en) * 2020-12-16 2022-10-21 核工业北京化工冶金研究院 Ion exchange method for gas generation in uranium extraction process
CN114192195A (en) * 2021-12-09 2022-03-18 中核内蒙古矿业有限公司 Elution device for uranium extraction by ion exchange method and elution method of ion exchange resin

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CN101619401A (en) * 2009-07-17 2010-01-06 云南佰盾环保新技术咨询有限公司 Method for recycling uranium from uranium extraction tailings

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CN101619401A (en) * 2009-07-17 2010-01-06 云南佰盾环保新技术咨询有限公司 Method for recycling uranium from uranium extraction tailings

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