CN106507827B - A kind of ion exchange with water closed cycle puies forward uranium technique - Google Patents
A kind of ion exchange with water closed cycle puies forward uranium techniqueInfo
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- CN106507827B CN106507827B CN200910124356.5A CN200910124356A CN106507827B CN 106507827 B CN106507827 B CN 106507827B CN 200910124356 A CN200910124356 A CN 200910124356A CN 106507827 B CN106507827 B CN 106507827B
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- uranium
- resin
- solution
- exchange
- elution
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Abstract
The present invention provides a kind of ion exchange with water closed cycle and puies forward uranium technique, and which is first leached to uranium ore with acid lixiviant;Then ion exchange absorption is carried out to leachate using weak-base anion-exchange resin, obtains loading uranium resin and adsorption tail liquid;Drip washing is carried out to loading uranium resin, is reclaimed from leacheate and is obtained uranium product.Which is processed as follows to loading uranium resin:(1) drip washing is carried out in the alkaline solution of 0.5~1.5mol/L using total carbonate or magnesium hydrogen salt concentration to loading uranium resin;(2) the uranium-bearing drip washing qualifying liquid of gained after drip washing is precipitated with NaOH;The chilled machine cooling of all mother liquor of precipitation of ammonium is returned after removing sulfate and prepares eluent.The present invention proposes uranium technological process to conventional ion exchange and is improved, chlorine root or nitrate anion are not introduced in load uranium anion exchange resin lessivation, avoid adversely affecting technological process, while process water closed cycle is realized, so as to reach the requirement of environmental protection.
Description
Technical field
The present invention relates to process water Circulation Process of Materials around Circuit, and in particular to a kind of ion of use water closed cycle
Exchange process puies forward uranium technique.
Background technology
Most of China's uranium mill leaches --- anion exchange resin absorption --- acid chlorine using acid system
Salt or acidic nitric salt elution --- depositing technology.
Uranium is extracted from acid leaching solution using anion exchange method, saturated resin typically uses 1mol/L sulphur
Acid solution or acid villaumite or acidic nitric salt are desorbed as eluent.
During due to being desorbed using acid villaumite or acidic nitric salt, although elution efficiency is high, body is desorbed
Product is small, but chlorine root or nitrate anion can be introduced in whole technological process, and during process cycles not
Disconnected accumulation, can influence the absorption of subsequent ion exchanger resin, and causing adsorption tail liquid to need, part is outer to arrange, it is impossible to
Make process water closed cycle, a large amount of radioactivity technique waste waters of generation not only waste water resource, to periphery
Environment and water system also result in pollution, and especially environmental protection has caused the great attention of countries in the world in recent years,
When making strippant using acidic nitric salt or chloride, its Industrial Wastewater Treatment is complicated, need to set up one whole
Cover industrial plants.In addition, chlorion or nitrate anion are strong to the corrosivity of equipment in acid condition, equipment
Decay resistance requires to protrude, and economic input is than larger.
The content of the invention
Uranium technique is put forward it is an object of the invention to provide a kind of ion-exchange with water closed cycle, its is right
Conventional ion exchange proposes uranium technological process and is improved, that is, is carrying uranium anion exchange resin lessivation not
Introduce chlorine root or nitrate anion, it is to avoid technological process is adversely affected, while realizing that process water is closed
Road is circulated, so as to reach the requirement of environmental protection.
Realize the technical scheme of the object of the invention:A kind of ion-exchange with water closed cycle puies forward uranium technique,
It is first leached with acid lixiviant to uranium ore;Then using weak-base anion-exchange resin to leaching
Go out liquid and carry out ion exchange absorption, obtain load uranium resin and adsorption tail liquid;Load uranium resin is drenched
Wash, reclaimed from leacheate and obtain uranium product.It is handled load uranium resin as follows:
(1) total carbonate or magnesium hydrogen salt concentration are used in 0.5~1.5mol/L alkali to load uranium resin
Property solution eluted, the alkaline solution consumption volume is 6~12 times of resin bed volumes, during elution contact
Between be 30~60min, elution terminal uranium concentration is within 0.3g/L, to obtain depleted uranium resin and uranium-bearing elution
Qualifying liquid;
(2) the uranium-bearing elution qualifying liquid of gained after elution is precipitated with NaOH, precipitates terminal
PH=12~14, obtain sodium diuranate uranium product and mother liquor of precipitation of ammonium;All chilled machine coolings of mother liquor of precipitation of ammonium
Remove to return after sulfate to 0~10 DEG C and prepare eluent.
A kind of ion-exchange with water closed cycle as described above puies forward uranium technique, alkaline molten described in it
Liquid uses Na2CO3Solution, NaHCO3Solution, K2CO3Solution, KHCO3Solution, (NH4)2CO3
Solution, NH4HCO3Solution, (NH4)2CO3With NH4HCO3Mixed solution, Na2CO3With NaHCO3
Mixed solution or K2CO3Solution and KHCO3Mixed solution.
A kind of ion-exchange with water closed cycle as described above puies forward uranium technique, and it is to obtained by elution
Depleted uranium resin is directly made the transition with adsorption tail liquid, and adsorption tail liquid consumption volume is 3~6 times of resin bed volumes, is connect
The time of touching is 5~20min, and transition terminal is pH=1.5~2.0;Transition tail washings directly returns to leaching process
Prepare leaching agent.
A kind of ion-exchange with water closed cycle as described above puies forward uranium technique, its weak base used
Property anion exchange resin include polystyrene, acrylic acid series, phenolic aldehyde system, epoxy, vinylpyridine system,
Ureaformaldehyde system or vinyl chloride weak-base anion-exchange resin.
Effect of the invention is that:
In the present invention reclaims the technique of uranium using weak-base anion-exchange resin from acid leaching solution,
Suitable eluent is selected, it (adsorbed, elute, make the transition and is sunk in whole ion exchange process
Shallow lake mother liquor is returned and used) in do not introduce other impurities ion.The alkaline matter such as carbonate or bicarbonate is made
The technical requirements of process water closed cycle in uranium removal process can be met for eluent, the eluent
Elution efficiency is high, can obtain the few elution qualifying liquid of impurity content.
Present invention process flow is compared with former flow:(1) influence ion exchange resin absorption property is not entered
Other ions (such as chlorine root or nitrate anion);(2) poor resin need not individually prepare transition agent and be made the transition
With transition equipment, using the poor resin of spent acid transition of adsorption tail liquid, technique is simple, and adsorption tail liquid need not
Outer row;(3) due to other ions without influence subsequent ion exchanger resin absorption property in mother liquor of precipitation of ammonium,
Preparation eluent can be all returned to, without outer row.
Brief description of the drawings
Fig. 1 conventional process flows and present invention process flow contrast schematic diagram.
Embodiment
A kind of ion of use water closed cycle of the present invention is handed over specific embodiment below in conjunction with the accompanying drawings
The method of changing puies forward uranium technique and is further described.
Embodiment 1
As shown in figure 1, a kind of ion-exchange with water closed cycle of the present invention carries uranium technique tool
Body step is as follows:
(I) Uranium Ores are leached using sulfuric acid solution as leaching agent;
(II) using D301 resins (polystyrene weak-base anion-exchange resin) to above-mentioned leachate
Ion exchange absorption is carried out, load uranium resin and adsorption tail liquid is obtained;
(III) adsorption tail liquid, which is returned, leaches process preparation leaching agent;
Load uranium resin is handled as follows:
1.5mol/L Na are used to load uranium resin2CO3Solution is eluted, the alkaline solution consumption body
Product is 6 times of resin bed volumes, and elution time of contact is 30min, and elution terminal uranium concentration is 0.3g/L, is obtained
To depleted uranium resin and uranium-bearing elution qualifying liquid;
The uranium-bearing elution qualifying liquid of gained after elution is precipitated with solid NaOH, terminal is precipitated
PH=12, obtains sodium diuranate uranium and mother liquor of precipitation of ammonium;All mother liquor of precipitation of ammonium (mainly contain Na2CO3With
Na2SO4) chilled machine is cooled to 0 DEG C, most Na in solution2SO4Precipitation, removes Na2SO4,
Supernatant can directly return to preparation eluent.
Depleted uranium resin after elution is directly made the transition with adsorption tail liquid, the transition agent special without preparing
Made the transition.During transition, adsorption tail liquid consumption volume is 3 times of resin bed volumes, and time of contact is 5min,
Transition terminal is the CO on pH=2.0, poor resin3 2-With the H in adsorption tail liquid+Reaction production CO2Gas.
Transition tail washings directly returns to leaching process and prepares leaching agent.
Result of the test:Use 1.5mol/L Na2CO3Eluted to carrying uranium resin, with preferable elution effect
Really, qualifying liquid uranium concentration is in more than 20g/L.During whole ion exchange carries uranium, it is to avoid other
The introducing of foreign ion, finally realizes that process water closed cycle is utilized.
Embodiment 2
As shown in figure 1, a kind of ion-exchange with water closed cycle of the present invention carries uranium technique tool
Body step is as follows:
(I) Uranium Ores are leached using sulfuric acid solution as leaching agent;
(II) using D363 resins (vinyl chloride weak-base anion-exchange resin) to above-mentioned leachate
Ion exchange absorption is carried out, load uranium resin and adsorption tail liquid is obtained;
(III) adsorption tail liquid, which is returned, leaches process preparation leaching agent;
Load uranium resin is handled as follows:
0.5mol/L K are used to load uranium resin2CO3Solution is eluted, the alkaline solution consumption volume
For 12 times of resin bed volumes, elution time of contact is 60min, and elution terminal uranium concentration is 0.3g/L, is obtained
To depleted uranium resin and uranium-bearing elution qualifying liquid;
The uranium-bearing elution qualifying liquid of gained after elution is precipitated with solid NaOH, terminal is precipitated
PH=14, obtains sodium diuranate uranium and mother liquor of precipitation of ammonium;Mother liquor of precipitation of ammonium (mainly contains K2CO3And K2SO4)
Chilled machine is cooled to 10 DEG C, most K in solution2SO4Precipitation, removes K2SO4, supernatant
Preparation eluent can directly be returned.
Depleted uranium resin after elution is directly made the transition with adsorption tail liquid, the transition agent special without preparing
Made the transition.During transition, adsorption tail liquid consumption volume is 6 times of resin bed volumes, and time of contact is 20min,
Transition terminal is the CO on pH=1.5, poor resin3 2-With the H in adsorption tail liquid+Reaction production CO2Gas.
Transition tail washings directly returns to leaching process and prepares leaching agent.
Result of the test:Use 0.5mol/L K2CO3Eluted to carrying uranium resin, with preferable elution effect,
Qualifying liquid uranium concentration is in more than 20g/L.During whole ion exchange carries uranium, it is to avoid other impurities
The introducing of ion, finally realizes that process water closed cycle is utilized.
Embodiment 3
As shown in figure 1, a kind of ion-exchange with water closed cycle of the present invention carries uranium technique tool
Body step is as follows:
(I) Uranium Ores are leached using sulfuric acid solution as leaching agent;
(II) using D311 resins (acrylic acid series weak-base anion-exchange resin) to above-mentioned leachate
Ion exchange absorption is carried out, load uranium resin and adsorption tail liquid is obtained;
(III) adsorption tail liquid, which is returned, leaches process preparation leaching agent;
Load uranium resin is handled as follows:
1.0mol/L (NH are used to load uranium resin4)2CO3Solution is eluted, the alkaline solution consumption
Volume is 9 times of resin bed volumes, and elution time of contact is 45min, and elution terminal uranium concentration is 0.25g/L,
Obtain depleted uranium resin and uranium-bearing elution qualifying liquid;
The uranium-bearing elution qualifying liquid of gained after elution is precipitated with NaOH, terminal pH=13 is precipitated,
Obtain sodium diuranate uranium and mother liquor of precipitation of ammonium;Mother liquor of precipitation of ammonium (mainly contains (NH4)2CO3(NH4)2SO4)
Chilled machine is cooled to 5 DEG C, most (NH in solution4)2SO4Precipitation, removes (NH4)2SO4, on
Clear liquid can directly return to preparation eluent.
Depleted uranium resin after elution is directly made the transition with adsorption tail liquid, the transition agent special without preparing
Made the transition.During transition, adsorption tail liquid consumption volume is 4.5 times of resin bed volumes, and time of contact is 12min,
Transition terminal is the CO on pH=1.8, poor resin3 2-With the H in adsorption tail liquid+Reaction production CO2Gas.
Transition tail washings directly returns to leaching process and prepares leaching agent.
Result of the test:With 1.0mol/L (NH4)2CO3Eluted to carrying uranium resin, with preferable elution
Effect, qualifying liquid uranium concentration is in more than 20g/L.During whole ion exchange carries uranium, it is to avoid its
The introducing of his foreign ion, finally realizes that process water closed cycle is utilized.
Embodiment 4
As shown in figure 1, a kind of ion-exchange with water closed cycle of the present invention carries uranium technique tool
Body step is as follows:
(I) Uranium Ores are leached using sulfuric acid solution as leaching agent;
(II) using D341 resins (vinylpyridine system weak-base anion-exchange resin) to above-mentioned leaching
Liquid carries out ion exchange absorption, obtains load uranium resin and adsorption tail liquid;
(III) adsorption tail liquid, which is returned, leaches process preparation leaching agent;
Load uranium resin is handled as follows:
0.50mol/L (NH are used to load uranium resin4)2CO3With 0.25mol/L (NH4)HCO3Mixing
Solution is eluted, and the alkaline solution consumption volume is 10 times of resin bed volumes, and elution time of contact is
30min, elution terminal uranium concentration is 0.25g/L, obtains depleted uranium resin and uranium-bearing elution qualifying liquid.
The uranium-bearing elution qualifying liquid of gained after elution is precipitated with NaOH, terminal pH=13 is precipitated,
Obtain sodium diuranate uranium and mother liquor of precipitation of ammonium;All mother liquor of precipitation of ammonium (mainly contain (NH4)2CO3With
(NH4)2SO4) chilled machine be cooled to 8 DEG C remove precipitation (NH4)2SO4, supernatant, which is returned, prepares eluent.
Depleted uranium resin obtained by elution is directly made the transition with adsorption tail liquid, adsorption tail liquid consumption volume is 5 times
Resin bed volume, time of contact is 10min, and transition terminal is pH=1.5;Transition tail washings directly returns to leaching
Go out process and prepare leaching agent.
Result of the test:With 0.50mol/L (NH4)2CO3+0.25mol/L(NH4)HCO3Enter to carrying uranium resin
Row elution, with preferable elution effect, qualifying liquid uranium concentration is in more than 20g/L.In whole ion exchange
During carrying uranium, it is to avoid the introducing of other impurities ions, finally realize that process water closed cycle is utilized.
Embodiment 5
As shown in figure 1, a kind of ion-exchange with water closed cycle of the present invention carries uranium technique tool
Body step is as follows:
(I) Uranium Ores are leached using sulfuric acid solution as leaching agent;
(II) ion exchange absorption is carried out to above-mentioned leachate using D341 weak-base anion-exchange resins,
Obtain load uranium resin and adsorption tail liquid;
(III) adsorption tail liquid, which is returned, leaches process preparation leaching agent;
Load uranium resin is handled as follows:
0.75mol/L Na are used to load uranium resin2CO3+0.50mol/L NaHCO3Solution is drenched
Wash, the alkaline solution consumption volume is 8 times of resin bed volumes, elution time of contact is 30min, elution
Terminal uranium concentration is 0.3g/L, obtains depleted uranium resin and uranium-bearing elution qualifying liquid;
The uranium-bearing elution qualifying liquid of gained after elution is precipitated with NaOH, terminal pH=13 is precipitated,
Obtain sodium diuranate uranium and mother liquor of precipitation of ammonium;All mother liquor of precipitation of ammonium (mainly contain Na2CO3And Na2SO4)
Chilled machine is cooled to 3 DEG C and removes precipitation Na2SO4, supernatant, which is returned, prepares eluent.
Depleted uranium resin obtained by elution is directly made the transition with adsorption tail liquid, adsorption tail liquid consumption volume is 4 times
Resin bed volume, time of contact is 15min, and transition terminal is pH=1.8.
Result of the test:Use 0.75mol/L Na2CO3+0.50mol/L NaHCO3Drenched to carrying uranium resin
Wash, with preferable elution effect, qualifying liquid uranium concentration is in more than 20g/L.Uranium is carried in whole ion exchange
During, it is to avoid the introducings of other impurities ions, finally realize that process water closed cycle is utilized.
Claims (4)
1. a kind of ion-exchange with water closed cycle puies forward uranium technique, it is first with acid lixiviant to uranium ore
Stone is leached;Then ion exchange absorption is carried out to leachate using weak-base anion-exchange resin,
Obtain load uranium resin and adsorption tail liquid;Load uranium resin is eluted, reclaims and obtains from leacheate
Uranium product;It is characterized in that:Load uranium resin is handled as follows:
(1) total carbonate or magnesium hydrogen salt concentration are used in 0.5~1.5mol/L alkali to load uranium resin
Property solution eluted, the alkaline solution consumption volume is 6~12 times of resin bed volumes, during elution contact
Between be 30~60min, elution terminal uranium concentration is within 0.3g/L, to obtain depleted uranium resin and uranium-bearing elution
Qualifying liquid;
(2) the uranium-bearing elution qualifying liquid of gained after elution is precipitated with NaOH, precipitates terminal
PH=12~14, obtain sodium diuranate uranium product and mother liquor of precipitation of ammonium;All chilled machine coolings of mother liquor of precipitation of ammonium
Remove to return after sulfate to 0~10 DEG C and prepare eluent.
2. a kind of ion-exchange with water closed cycle according to claim 1 puies forward uranium technique, its
It is characterised by:Described alkaline solution uses Na2CO3Solution, NaHCO3Solution, K2CO3Solution,
KHCO3Solution, (NH4)2CO3Solution, NH4HCO3Solution, (NH4)2CO3With NH4HCO3Mixing
Solution, Na2CO3With NaHCO3Mixed solution or K2CO3Solution and KHCO3Mixed solution.
3. a kind of ion-exchange with water closed cycle according to claim 1 or 2 puies forward uranium technique,
It is characterized in that:Depleted uranium resin obtained by elution is directly made the transition with adsorption tail liquid, adsorption tail liquid consumption body
Product is 3~6 times of resin bed volumes, and time of contact is 5~20min, and transition terminal is pH=1.5~2.0;
Transition tail washings directly returns to leaching process and prepares leaching agent.
4. a kind of ion-exchange with water closed cycle according to claim 1 or 2 puies forward uranium technique,
It is characterized in that:The weak-base anion-exchange resin used includes polystyrene, acrylic acid series, phenol
Aldehyde system, epoxy, vinylpyridine system, ureaformaldehyde system or vinyl chloride weak-base anion-exchange resin.
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