CN116411185A - Adsorption and desaturation process of anion resin under neutral leaching condition of sandstone uranium deposit - Google Patents
Adsorption and desaturation process of anion resin under neutral leaching condition of sandstone uranium deposit Download PDFInfo
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- CN116411185A CN116411185A CN202111656774.6A CN202111656774A CN116411185A CN 116411185 A CN116411185 A CN 116411185A CN 202111656774 A CN202111656774 A CN 202111656774A CN 116411185 A CN116411185 A CN 116411185A
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- 238000001179 sorption measurement Methods 0.000 title claims abstract description 228
- 238000002386 leaching Methods 0.000 title claims abstract description 127
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 title claims abstract description 124
- 229910052770 Uranium Inorganic materials 0.000 title claims abstract description 114
- 238000000034 method Methods 0.000 title claims abstract description 91
- 239000011347 resin Substances 0.000 title claims abstract description 58
- 229920005989 resin Polymers 0.000 title claims abstract description 58
- 230000007935 neutral effect Effects 0.000 title claims abstract description 25
- 150000001450 anions Chemical class 0.000 title claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 152
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000003860 storage Methods 0.000 claims description 62
- 239000003795 chemical substances by application Substances 0.000 claims description 55
- 239000000243 solution Substances 0.000 claims description 47
- 230000001131 transforming effect Effects 0.000 claims description 43
- 239000003480 eluent Substances 0.000 claims description 26
- 230000009466 transformation Effects 0.000 claims description 23
- 238000005406 washing Methods 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- 125000000129 anionic group Chemical group 0.000 claims description 8
- 238000005520 cutting process Methods 0.000 claims description 5
- 239000011550 stock solution Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 2
- 238000005065 mining Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 238000002791 soaking Methods 0.000 abstract description 2
- 238000010586 diagram Methods 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 3
- 230000033558 biomineral tissue development Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 239000006004 Quartz sand Substances 0.000 description 2
- 230000001351 cycling effect Effects 0.000 description 2
- 238000009854 hydrometallurgy Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012797 qualification Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- -1 uranium ions Chemical class 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
- C22B60/02—Obtaining thorium, uranium, or other actinides
- C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
- C22B60/0217—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes
- C22B60/0252—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries
- C22B60/0265—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries extraction by solid resins
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/02—Apparatus therefor
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention belongs to the technical field of water metallurgy treatment of uranium mining from sandstone uranium mine field leaching, and particularly relates to an adsorption and desaturation process of anion resin under a sandstone uranium deposit neutral leaching condition. According to the adsorption and re-saturation process of the anion resin under the neutral leaching condition of the sandstone uranium deposit, under the condition of the neutral leaching process, the process in the prior art is additionally provided with the step of circularly soaking the adsorption saturated resin by the qualified uranium-depleted liquid, so that the resin capacity is further improved, and the effect of leaching the qualified uranium-depleted liquid in the next step is achieved.
Description
Technical Field
The invention belongs to the technical field of water metallurgy treatment of uranium mining from sandstone uranium mine field leaching, and particularly relates to an adsorption and desaturation process of anion resin under a sandstone uranium deposit neutral leaching condition.
Background
In sandstone uranium mine mountain with high chloride and high mineralization degreeIn the mining process, CO is adopted 2 +O 2 The process for extracting uranium by neutral leaching of gas comprises the steps of adsorbing uranium ions in leaching liquid by adopting weak-alkaline anion resin; with the increase of the service life of the resin, the adsorption capacity of the resin is gradually reduced due to factors such as the influence of impurity ions in the leaching liquid on the resin, and the uranium concentration of the qualified production liquid is further reduced. Finally, the hydrometallurgical process efficiency is affected to be reduced, and the raw material consumption is increased. Therefore, the adsorption and desaturation process is introduced to solve the problems of low adsorption capacity of resin and low uranium concentration of leaching qualified liquid.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a resin adsorption and re-saturation process of weak alkaline anion resin under the neutral leaching conditions of high chloride and high mineralization, and solves the problem of low uranium concentration in qualified production liquid caused by low resin adsorption capacity.
The technical scheme of the invention is as follows:
an adsorption and desaturation process of anion resin under the neutral leaching condition of sandstone uranium deposit, comprising the following steps:
step one: adsorption of
The adsorption process adopts a mode of connecting two adsorption towers in series for adsorption, namely, raw liquid sequentially flows through an adsorption first tower and an adsorption last tower from a raw liquid pool and flows into a tail liquid pool; the first adsorption tower and the last adsorption tower are both upper liquid inlet and lower liquid outlet; when the first adsorption tower is saturated, the first adsorption tower is separated from the adsorption process and is transferred to a second re-saturation process;
at this time, a new standby adsorption tower is connected in series behind the original adsorption tail tower, and two towers of a new round are connected in series for adsorption; in the new round of adsorption process, the last adsorption tower of the previous round becomes an adsorption head tower, and the new standby adsorption tower becomes an adsorption tail tower;
step two: re-saturation
Carrying out re-saturation treatment on the saturated adsorption tower separated from the first step, namely an adsorption head tower;
the pre-stored depleted uranium solution is placed in a depleted liquid storage tank, an adsorption tower is connected with the depleted liquid storage tank, and the adsorption tower adopts a mode of feeding liquid from the lower inlet to the upper outlet, so that the depleted uranium solution is arranged in the depleted liquid storage tank and the adsorption towerCirculating in between, and re-adsorbing; when the uranium concentration of the liquid inlet and the liquid outlet of the adsorption tower is less than or equal to X 1 g/L (preferably X 1 =0.1), stop cycling;
driving the solution in the adsorption tower into a raw liquid pool through compressed air until the solution is pressed to be dry, and taking the resin in the adsorption tower after saturated and re-adsorbed to analyze uranium-containing capacity;
step three: transformation type
Carrying out transformation treatment on the adsorption tower which completes the re-saturation process in the second step;
the transforming agent is placed in a transforming agent storage tank, an adsorption tower is connected with the transforming agent storage tank, and the adsorption tower adopts a mode of feeding liquid from bottom to top so that the transforming agent circulates between the transforming agent storage tank and the adsorption tower for transforming; when the acidity of the liquid inlet and the liquid outlet of the adsorption tower reach the same value and X 2 g/L~X 3 g/L (preferably X 2 =13,X 3 =16), stop cycling, complete transformation;
step four: rinsing
The adsorption towers after the third step are completed for standby, three adsorption towers, namely a leaching head tower, a leaching middle tower and a leaching tail tower, are prepared, and the leaching process is carried out;
placing the eluent in a eluent storage tank; the eluent storage tank is connected with the first eluting tower, three towers are connected in series for eluting, and the eluent of each adsorption tower adopts an up-in and down-out mode; the liquid discharged from the leaching end tower is uranium qualified liquid; the liquid discharged from the leaching end tower reaches X 4 ~X 5 Cubic meter time (preferably X 4 =36,X 5 =38), complete rinsing;
finally, cutting out a leaching head tower, and using compressed air to hydraulically press residual solution in the leaching head tower into a leaching agent storage tank for preparing leaching agent; after the first leaching tower is separated, a new leaching process is started; in the new leaching process, the middle leaching tower of the previous round is changed into the first leaching tower of the new round, the last leaching tower of the previous round is changed into the middle leaching tower of the new round, and then the new adsorption tower which completes the transformation process of the third step is accessed as the last leaching tower;
step five: washing
Pumping clear water and water into the adsorption tower after washingStep one, tail liquid in the tail liquid pool is used for washing solution entrained in the adsorption tower resin; washing liquid, namely the liquid outlet of the washed adsorption tower, enters the liquid pool of the first step; when the uranium concentration of the washing liquid is less than or equal to X 6 mg/L, pH value is greater than X 7 Time (preferably X 6 =1,X 7 =5.0), washing was completed, and the adsorption column was used as an adsorption backup column.
As a preferable scheme: in the first step, the method comprises the following operations: the judgment basis of the saturation of the first adsorption tower is as follows: the uranium concentration of the tail liquid of the first tower of the adsorption is more than or equal to the uranium concentration of the stock solution, or the uranium concentration of the tail liquid of the last tower of the adsorption is more than or equal to 1mg/L; and (3) after the adsorption primary tower is separated from the adsorption process, taking saturated resin of the adsorption primary tower to analyze the uranium content capacity of the saturated resin.
As a preferable scheme: the second step comprises the following operations:
carrying out re-saturation treatment on the saturated adsorption tower separated from the first step, namely an adsorption head tower;
pre-storing a depleted uranium solution, wherein the uranium concentration of the depleted uranium solution is less than or equal to 25.0g/L; the volume ratio of the uranium-depleted solution in the lean solution storage tank to the resin in the adsorption tower is 2:1; connecting an adsorption tower with a lean solution storage tank, circulating the lean uranium solution between the lean solution storage tank and the adsorption tower through a chemical pump by adopting a mode of feeding liquid from bottom to top, and re-adsorbing; after the depleted uranium solution circulates for 12 hours between the depleted solution storage tank and the adsorption tower, taking the inlet liquid and the outlet liquid of the adsorption tower every 2 hours for measuring the uranium concentration, and stopping the circulation when the uranium concentrations of the inlet liquid and the outlet liquid of the adsorption tower are less than or equal to 0.1 g/L;
and driving the solution in the adsorption tower into a raw liquid pool through compressed air until the solution is pressed to dryness, and taking the resin in the adsorption tower after saturated and re-adsorbed to analyze the uranium content capacity.
As a preferable scheme: step three, the method comprises the following operations:
carrying out transformation treatment on the adsorption tower which completes the re-saturation process in the second step;
qualified liquid with uranium concentration less than or equal to 8.0g/L and industrial hydrochloric acid are mixed according to a volume ratio of 16m 3 :3.0~3.5m 3 The mixture is prepared into a transforming agent, the transforming agent is placed in a transforming agent storage tank, and the acidity of the transforming agent after preparation is 65g/L; connecting the adsorption tower with a transforming agent storage tank for absorbingThe auxiliary tower adopts a lower inlet and upper outlet liquid inlet mode, and a transforming agent is circulated between a transforming agent storage tank and an adsorption tower through a chemical pump to transform; after the transforming agent circulates between the transforming agent storage tank and the adsorption tower for 8 hours, when the acidity of the inlet liquid and the outlet liquid of the adsorption tower reach the same, and the circulation is stopped at 13.0 g/L-16.0 g/L, and transformation is completed.
As a preferable scheme: step four, the method comprises the following operations:
the adsorption towers after the third step are completed for standby, three adsorption towers, namely a leaching head tower, a leaching middle tower and a leaching tail tower, are prepared, and the leaching process is carried out;
clean water is adopted as eluent and is placed in an eluent storage tank; the eluent storage tank is connected with the first eluting tower, three towers are connected in series for eluting, the eluent of each adsorption tower adopts an up-in and down-out mode, and the liquid inlet linear speed of the eluent is controlled to be 0.8 m/h-1.0 m/h;
the liquid discharged from the leaching end tower is uranium qualified liquid: when the uranium concentration of the uranium qualified liquid is more than or equal to 25.0g/L, the finished product is obtained; when the uranium concentration of the uranium qualified liquid is less than or equal to 8.0g/L and less than 25.0g/L, conveying the uranium qualified liquid with the concentration to a lean liquid storage tank; when the uranium concentration of the uranium qualified liquid is less than 8.0g/L, preparing a transformation agent by using the uranium qualified liquid with the concentration; the liquid outlet of the leaching end tower reaches 36-38 m 3 When the leaching is finished;
finally, cutting out a leaching head tower, and using compressed air to hydraulically press residual solution in the leaching head tower into a leaching agent storage tank for preparing leaching agent; after the first leaching tower is separated, a new leaching process is started; in the new leaching process, the middle leaching tower of the previous round is changed into the first leaching tower of the new round, the last leaching tower of the previous round is changed into the middle leaching tower of the new round, and then the adsorption tower which completes the three transformation process of the step is accessed to be used as the last leaching tower.
The beneficial effects of the invention are as follows:
the invention provides an adsorption and resaturation process of anion resin under the neutral leaching condition of sandstone uranium deposit, which solves the problem of low uranium concentration in qualified liquid produced due to low adsorption capacity of resin by realizing resin adsorption and resaturation of weak alkaline anion resin under the neutral leaching condition of high chloride and high mineralization, improves the saturated resin capacity and the uranium concentration in qualified liquid by more than 50%, and saves the consumption of raw materials by more than 10%.
Drawings
FIG. 1 is a schematic diagram of an adsorption process;
in FIG. 1, 101-a raw liquid pool, 102-an adsorption process chemical pump, 103-a first tower, 104-a last tower and 105-a tail liquid pool;
FIG. 2 is a schematic diagram of a re-saturation process and a inversion process;
in FIG. 2, 201-lean liquid storage tank, 202-transforming agent storage tank, 203-resaturation and transforming process chemical pump, 204-adsorption tower;
FIG. 3 is a schematic diagram of a rinsing process;
in FIG. 3, 301-eluent reservoir, 302-chemical pump, 303-first column, 304-middle column, 305-last column, 306-pass liquid reservoir;
FIG. 4 is a schematic diagram of the structure of an adsorption tower;
in fig. 4, 401-adsorption tower base, 402-manhole, 403-tower body, 404-compressed air pipeline, 405-leachate inlet, 406-DN40 exhaust valve, 407-resin, 408-40 mesh gauze, 409-water cap, 410-quartz sand, 411-filter plate, 412-liquid outlet;
FIG. 5 is a schematic diagram of the structure of the eluent reservoir;
in fig. 5, 501-can top interface, DN50 flange, 502-can top interface, DN150 flange, 503-can top interface, 60cm x 70cm, 504-can bottom interface, DN40 flange;
FIG. 6 is a schematic diagram of the structure of a transfer agent reservoir and a qualification liquid reservoir;
in fig. 6: 601-can top interface, DN flange, 602-can top interface, DN40 flange, 603-can top interface, DN600 flange, 604-can bottom interface, DN80 flange, 605-can top interface, DN80 flange.
Detailed Description
The adsorption and desaturation process of the anionic resin under neutral leaching conditions of sandstone uranium deposit according to the present invention is described in detail below with reference to the accompanying drawings and examples.
According to the adsorption and re-saturation process of the anion resin under the neutral leaching condition of the sandstone uranium deposit, under the condition of the neutral leaching process, the process in the prior art is additionally provided with the step of circularly soaking the adsorption saturated resin by the qualified uranium-depleted liquid, so that the resin capacity is further improved, and the effect of leaching the qualified uranium-depleted liquid in the next step is achieved.
The invention relates to an adsorption and desaturation process of anion resin under the neutral leaching condition of sandstone uranium deposit, which comprises the following steps:
step one: and (5) adsorption.
As shown in fig. 1, the adsorption process adopts a mode of connecting two adsorption towers of a compact fixed bed in series for adsorption, namely, raw liquid sequentially flows through an adsorption first tower and an adsorption last tower from a raw liquid pool and flows into a tail liquid pool. The first adsorption tower and the last adsorption tower are both upper liquid inlet and lower liquid outlet. And when the uranium concentration of the tail liquid of the first adsorption tower is more than or equal to the uranium concentration of the stock solution, or when the uranium concentration of the tail liquid of the last adsorption tower is more than or equal to 1mg/L, the first adsorption tower is saturated, the first adsorption tower is separated from the adsorption process and is transferred to the second re-saturation process, and meanwhile, the saturated resin of the first adsorption tower is taken to analyze the uranium content capacity of the first adsorption tower.
At this time, a new standby adsorption tower is connected in series behind the original adsorption tail tower, and two towers of a new round are connected in series for adsorption. In the new round of adsorption process, the last adsorption tower of the previous round becomes an adsorption head tower, and the new standby adsorption tower becomes an adsorption tail tower.
Step two: and (5) re-saturating.
And (3) carrying out re-saturation treatment on the saturated adsorption tower (namely the original adsorption head tower) separated from the first step.
As shown in fig. 2 (in the re-saturation process, the inlet and outlet valves of the transforming agent storage tank in fig. 2 are closed and do not participate in circulation), pre-stored uranium-depleted solution (the uranium concentration is less than or equal to 25.0 g/L) is placed in a lean solution storage tank, and the volume ratio of the uranium-depleted solution in the lean solution storage tank to resin in the adsorption tower is controlled to be about 2:1; the adsorption tower is connected with the lean liquid storage tank, the adsorption tower adopts a mode of feeding liquid from the lower inlet to the upper outlet, and the lean uranium solution is circulated between the lean liquid storage tank and the adsorption tower through the chemical pump for re-adsorption. After the depleted uranium solution circulates for 12 hours between the depleted solution storage tank and the adsorption tower, the inlet liquid and the outlet liquid of the adsorption tower are taken every 2 hours to be used for measuring the uranium concentration, and when the uranium concentration of the inlet liquid and the uranium concentration of the outlet liquid of the adsorption tower are less than or equal to 0.1g/L, the circulation is stopped.
And driving the solution in the adsorption tower into a stock solution tank shown in fig. 1 through compressed air until the solution is pressed dry, and taking the resin in the adsorption tower after saturated re-adsorption to analyze the uranium content.
Step three: and (5) transformation.
And (3) carrying out transformation treatment on the adsorption tower which completes the step two of the re-saturation process.
As shown in FIG. 2 (in the adsorption process, the inlet and outlet valves of the lean liquid storage tank in FIG. 2 are closed and do not participate in circulation), qualified liquid with uranium concentration less than or equal to 8.0g/L and industrial hydrochloric acid are added according to the volume ratio of 16m 3 :3.0~3.5m 3 The mixture is prepared into a transforming agent, the transforming agent is placed in a transforming agent storage tank, and the acidity of the transforming agent after preparation is 65g/L; the adsorption tower is connected with the transforming agent storage tank, adopts a mode of feeding liquid from the lower inlet to the upper outlet, and circulates the transforming agent between the transforming agent storage tank and the adsorption tower through a chemical pump for transformation. After the transforming agent circulates between the transforming agent storage tank and the adsorption tower for 8 hours, when the acidity of the inlet liquid and the outlet liquid of the adsorption tower reach the same, and the circulation is stopped at 13.0 g/L-16.0 g/L, and transformation is completed.
Step four: and (5) leaching.
And 3, finishing the adsorption tower after the step three for standby, and finishing three adsorption towers, namely a leaching head tower, a leaching middle tower and a leaching tail tower, and entering a leaching procedure.
As shown in fig. 3, clean water is used as the eluent and is placed in the eluent storage tank; the eluent storage tank is connected with the first eluting tower, three towers are connected in series for eluting, the eluent of each adsorption tower adopts an up-in and down-out mode, and the liquid inlet linear speed of the eluent is controlled to be 0.8 m/h-1.0 m/h.
The liquid discharged from the leaching end tower is uranium qualified liquid: when the uranium concentration of the uranium qualified liquid is more than or equal to 25.0g/L, the finished product is obtained; when the uranium concentration of the uranium qualified liquid is less than or equal to 8.0g/L and less than 25.0g/L, conveying the uranium qualified liquid with the concentration to a lean liquid storage tank; when the uranium concentration of the uranium qualified liquid is less than 8.0g/L, preparing a transformation agent by using the uranium qualified liquid with the concentration. The liquid outlet of the leaching end tower reaches 36-38 m 3 At this time, the rinsing is completed.
Finally, cutting out the leaching head tower, and using compressed air to press residual solution in the leaching head tower into a leaching agent storage tank for preparing leaching agent. And after the first leaching tower is separated, starting a new leaching process. In the new leaching process, the middle leaching tower of the previous round is changed into the first leaching tower of the new round, the last leaching tower of the previous round is changed into the middle leaching tower of the new round, and then the adsorption tower which completes the three transformation process of the step is accessed to be used as the last leaching tower.
Step five: and (5) washing.
For the adsorption tower after washing, 200m of the adsorption tower is pumped in 3 Clear water and 400m 3 And step one, tail liquid in the tail liquid pool is used for washing solution carried in the adsorption tower resin, and washing liquid, namely liquid discharged from the washed adsorption tower enters the original liquid pool in step one. When the uranium concentration of the washing liquid is less than or equal to 1mg/L, pH value and is more than 5.0, washing is completed, and the adsorption tower is used as an adsorption standby tower.
The process of the adsorption and resaturation of anionic resins under neutral leaching conditions of sandstone uranium deposits is carried out by means of the following devices of the prior art:
a. adsorption tower: as shown in fig. 4, the adsorption tower is a steel liner PO tank with a diameter of 2.5m, a total height of 7.5m and an effective height of 6m, and the components include: 401-adsorption tower base, 402-manhole, 403-tower body, 404-compressed air pipeline, 405-leachate inlet, 406-DN40 exhaust valve, 407-resin, 408-40 mesh gauze, 409-water cap, 410-quartz sand, 411-filter plate, 412-outlet, compressed air pipeline is DN40PE pipe, and the rest connecting pipes are PPR pipe, the size corresponds to the flange size.
b. A eluent reservoir: as shown in fig. 5, a steel lined PO tank of 2.5m diameter and 2m height, the components comprising: 501-a tank top interface, a DN50 flange, wherein a DN50 iron pipe is connected with a clean water pipeline; 502-a tank top exhaust port, DN150, a fan pipeline is connected; 503-tank top interface, 60cm 70cm, exhaust port; 504-tank bottom interface, DN40 flange, desorbent outlet, connected with desorbent delivery pump by DN40PPR pipe.
c. A transforming agent (qualification liquid) storage tank: as shown in fig. 6, the transforming agent storage tank and the qualified liquid storage tank are the same in structure, and are steel lining PO tanks with diameters of 2.5m and heights of 4m, and the components comprise: 601-a tank top interface, a DN40 flange, wherein a DN40 iron pipe is connected with a clean water pipeline; 602-a tank top interface, a DN40 flange, and a DN40PPR pipeline is connected with a hydrochloric acid pipeline; 603-a pot top exhaust port, DN600 flange; 604-a tank bottom interface, a DN80 flange, and an acidizing fluid outlet, which is connected with a DN80PPR pipeline; 605-tank top interface, DN80 flange, acidification circulation backwater, connected by DN80PPR pipeline.
Results of the implementation
After the process is implemented, the saturated resin capacity and the uranium qualified liquid are both greatly increased, and the residual uranium capacity of the lean resin after leaching is less than 0.8g/L, so that the requirement that the uranium capacity of the subsequent adsorption process is less than 1.0g/L is met.
Implementation results: the comparison of the adsorption process parameters before and after the process improvement of the invention is shown in Table 1:
table 1: the process of the invention is used for comparing the process parameters before and after the process is improved
As can be seen from the comparison of the prior art in Table 1 and the parameters of the invention, the improved saturated resin capacity and the qualified liquid uranium concentration are greatly increased, and the unit consumption of chemical raw materials is obviously reduced.
The capacity of the saturated resin is increased by 122.98% compared with the capacity of the saturated resin before improvement, the uranium concentration of the qualified liquid is increased by 69.39% compared with the uranium concentration of the qualified liquid before application, and the volume of the qualified liquid after precipitation is reduced by 41.67%, the unit consumption of hydrochloric acid is reduced by 13.11% and the unit consumption of caustic soda flakes is reduced by 33.85% due to the fact that the uranium concentration of the qualified liquid is greatly increased after the saturated re-adsorption process is applied. The adsorption performance of the resin is not affected before and after the saturated re-adsorption process is applied, and all parameters are controlled within the process instruction range.
The application of the adsorption and desaturation technology of the anion resin under the neutral leaching condition of the sandstone uranium deposit is also described in detail in the embodiment of the invention. The above embodiment is the best example of uranium hydrometallurgy fixed bed saturation re-adsorption under the weak alkaline neutral leaching condition, but the control parameters can be changed under the conditions of different weak alkaline anions and different leachate treatment without departing from the spirit of the invention, and any modification, equivalent replacement, improvement and the like which are within the spirit and principle of the invention are all within the protection scope of the patent of the invention.
Claims (7)
1. An adsorption and desaturation process of anion resin under the neutral leaching condition of sandstone uranium deposit, which is characterized in that: the method comprises the following steps:
step one: adsorption of
The adsorption process adopts a mode of connecting two adsorption towers in series for adsorption, namely, raw liquid sequentially flows through an adsorption first tower and an adsorption last tower from a raw liquid pool and flows into a tail liquid pool; the first adsorption tower and the last adsorption tower are both upper liquid inlet and lower liquid outlet; when the first adsorption tower is saturated, the first adsorption tower is separated from the adsorption process and is transferred to a second re-saturation process;
at this time, a new standby adsorption tower is connected in series behind the original adsorption tail tower, and two towers of a new round are connected in series for adsorption; in the new round of adsorption process, the last adsorption tower of the previous round becomes an adsorption head tower, and the new standby adsorption tower becomes an adsorption tail tower;
step two: re-saturation
Carrying out re-saturation treatment on the saturated adsorption tower separated from the first step, namely an adsorption head tower;
placing pre-stored depleted uranium solution in a depleted liquid storage tank, connecting an adsorption tower with the depleted liquid storage tank, and enabling the depleted uranium solution to circulate between the depleted liquid storage tank and the adsorption tower by adopting a lower inlet and upper outlet liquid inlet mode for the adsorption tower to re-adsorb; when the uranium concentration of the liquid inlet and the liquid outlet of the adsorption tower is less than or equal to X 1 g/L, stopping circulation;
driving the solution in the adsorption tower into a raw liquid pool through compressed air until the solution is pressed to be dry, and taking the resin in the adsorption tower after saturated and re-adsorbed to analyze uranium-containing capacity;
step three: transformation type
Carrying out transformation treatment on the adsorption tower which completes the re-saturation process in the second step;
the transforming agent is placed in a transforming agent storage tank, an adsorption tower is connected with the transforming agent storage tank, and the adsorption tower adopts a mode of feeding liquid from bottom to top so that the transforming agent circulates between the transforming agent storage tank and the adsorption tower for transforming; when the acidity of the liquid inlet and the liquid outlet of the adsorption tower reach the same value and X 2 g/L~X 3 Stopping circulation and finishing transformation when g/L is carried out;
step four: rinsing
The adsorption towers after the third step are completed for standby, three adsorption towers, namely a leaching head tower, a leaching middle tower and a leaching tail tower, are prepared, and the leaching process is carried out;
placing the eluent in a eluent storage tank; the eluent storage tank is connected with the first eluting tower, three towers are connected in series for eluting, and the eluent of each adsorption tower adopts an up-in and down-out mode; the liquid discharged from the leaching end tower is uranium qualified liquid; the liquid discharged from the leaching end tower reaches X 4 ~X 5 When cubic meters are used, washing is completed;
finally, cutting out a leaching head tower, and using compressed air to hydraulically press residual solution in the leaching head tower into a leaching agent storage tank for preparing leaching agent; after the first leaching tower is separated, a new leaching process is started; in the new leaching process, the middle leaching tower of the previous round is changed into the first leaching tower of the new round, the last leaching tower of the previous round is changed into the middle leaching tower of the new round, and then the new adsorption tower which completes the transformation process of the third step is accessed as the last leaching tower;
step five: washing
Pumping clear water and tail liquid in the tail liquid pool in the step one into the adsorption tower after leaching is finished, and washing solution entrained in the adsorption tower resin; washing liquid, namely the liquid outlet of the washed adsorption tower, enters the liquid pool of the first step; when the uranium concentration of the washing liquid is less than or equal to X 6 mg/L, pH value is greater than X 7 And when the washing is finished, the adsorption tower is used as an adsorption standby tower.
2. The process for the adsorption and desaturation of anionic resins under neutral leaching conditions of sandstone uranium deposits according to claim 1,
in the second step, X 1 =0.1;
In step three, X 2 =13,X 3 =16;
In step four, X 4 =36,X 5 =38;
In step five, X 6 =1,X 7 =5.0。
3. The process for the adsorption and resaturation of anionic resins under neutral leaching conditions of sandstone uranium deposits according to claim 1, characterized in that: in the first step, the method comprises the following operations:
the judgment basis of the saturation of the first adsorption tower is as follows: the uranium concentration of the tail liquid of the first tower of the adsorption is more than or equal to the uranium concentration of the stock solution, or the uranium concentration of the tail liquid of the last tower of the adsorption is more than or equal to 1mg/L.
4. The process for the adsorption and resaturation of anionic resins under neutral leaching conditions of sandstone uranium deposits according to claim 1, characterized in that: in the first step, after the adsorption first tower is separated from the adsorption process, the saturated resin of the adsorption first tower is taken to analyze the uranium content of the adsorption first tower.
5. The process for the adsorption and resaturation of anionic resins under neutral leaching conditions of sandstone uranium deposits according to claim 1, characterized in that: the second step comprises the following operations:
carrying out re-saturation treatment on the saturated adsorption tower separated from the first step, namely an adsorption head tower;
pre-storing a depleted uranium solution, wherein the uranium concentration of the depleted uranium solution is less than or equal to 25.0g/L; the volume ratio of the uranium-depleted solution in the lean solution storage tank to the resin in the adsorption tower is 2:1; connecting an adsorption tower with a lean solution storage tank, circulating the lean uranium solution between the lean solution storage tank and the adsorption tower through a chemical pump by adopting a mode of feeding liquid from bottom to top, and re-adsorbing; after the depleted uranium solution circulates for 12 hours between the depleted solution storage tank and the adsorption tower, taking the inlet liquid and the outlet liquid of the adsorption tower every 2 hours for measuring the uranium concentration, and stopping the circulation when the uranium concentrations of the inlet liquid and the outlet liquid of the adsorption tower are less than or equal to 0.1 g/L;
and driving the solution in the adsorption tower into a raw liquid pool through compressed air until the solution is pressed to dryness, and taking the resin in the adsorption tower after saturated and re-adsorbed to analyze the uranium content capacity.
6. The process for the adsorption and resaturation of anionic resins under neutral leaching conditions of sandstone uranium deposits according to claim 1, characterized in that: step three, the method comprises the following operations:
carrying out transformation treatment on the adsorption tower which completes the re-saturation process in the second step;
qualified liquid with uranium concentration less than or equal to 8.0g/L and industrial hydrochloric acid are mixed according to a volume ratio of 16m 3 :3.0~3.5m 3 The mixture is prepared into a transforming agent, the transforming agent is placed in a transforming agent storage tank, and the acidity of the transforming agent after preparation is 65g/L; the method comprises the steps that an adsorption tower is connected with a transforming agent storage tank, the adsorption tower adopts a mode of feeding liquid from bottom to top, and transforming agent circulates between the transforming agent storage tank and the adsorption tower through a chemical pump for transformation; after the transforming agent circulates between the transforming agent storage tank and the adsorption tower for 8 hours, when the acidity of the inlet liquid and the outlet liquid of the adsorption tower reach the same, and the circulation is stopped at 13.0 g/L-16.0 g/L, and transformation is completed.
7. The process for the adsorption and resaturation of anionic resins under neutral leaching conditions of sandstone uranium deposits according to claim 1, characterized in that: step four, the method comprises the following operations:
the adsorption towers after the third step are completed for standby, three adsorption towers, namely a leaching head tower, a leaching middle tower and a leaching tail tower, are prepared, and the leaching process is carried out;
clean water is adopted as eluent and is placed in an eluent storage tank; the eluent storage tank is connected with the first eluting tower, three towers are connected in series for eluting, the eluent of each adsorption tower adopts an up-in and down-out mode, and the liquid inlet linear speed of the eluent is controlled to be 0.8 m/h-1.0 m/h;
the liquid discharged from the leaching end tower is uranium qualified liquid: when the uranium concentration of the uranium qualified liquid is more than or equal to 25.0g/L, the finished product is obtained; when the uranium concentration of the uranium qualified liquid is less than or equal to 8.0g/L and less than 25.0g/L, conveying the uranium qualified liquid with the concentration to a lean liquid storage tank; when the uranium concentration of the uranium qualified liquid is less than 8.0g/L, preparing a transformation agent by using the uranium qualified liquid with the concentration; the liquid outlet of the leaching end tower reaches 36-38 m 3 When the leaching is finished;
finally, cutting out a leaching head tower, and using compressed air to hydraulically press residual solution in the leaching head tower into a leaching agent storage tank for preparing leaching agent; after the first leaching tower is separated, a new leaching process is started; in the new leaching process, the middle leaching tower of the previous round is changed into the first leaching tower of the new round, the last leaching tower of the previous round is changed into the middle leaching tower of the new round, and then the adsorption tower which completes the three transformation process of the step is accessed to be used as the last leaching tower.
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