CN116351480A - D231-YT anion exchange resin detoxification process - Google Patents
D231-YT anion exchange resin detoxification process Download PDFInfo
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- CN116351480A CN116351480A CN202111618432.5A CN202111618432A CN116351480A CN 116351480 A CN116351480 A CN 116351480A CN 202111618432 A CN202111618432 A CN 202111618432A CN 116351480 A CN116351480 A CN 116351480A
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- 238000001784 detoxification Methods 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000003957 anion exchange resin Substances 0.000 title claims abstract description 22
- 239000011347 resin Substances 0.000 claims abstract description 68
- 229920005989 resin Polymers 0.000 claims abstract description 68
- 238000001179 sorption measurement Methods 0.000 claims abstract description 26
- 238000002386 leaching Methods 0.000 claims abstract description 19
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 10
- 229910052770 Uranium Inorganic materials 0.000 claims abstract description 7
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 claims abstract description 7
- 231100000331 toxic Toxicity 0.000 claims abstract description 5
- 230000002588 toxic effect Effects 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims description 66
- 238000004140 cleaning Methods 0.000 claims description 21
- 238000002360 preparation method Methods 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 238000001704 evaporation Methods 0.000 claims description 9
- 230000008020 evaporation Effects 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 230000009466 transformation Effects 0.000 claims description 4
- 239000000729 antidote Substances 0.000 claims description 3
- 238000005056 compaction Methods 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 239000003440 toxic substance Substances 0.000 abstract description 5
- 238000009854 hydrometallurgy Methods 0.000 abstract description 4
- 231100000614 poison Toxicity 0.000 abstract description 4
- 125000000524 functional group Chemical group 0.000 abstract description 3
- 238000011065 in-situ storage Methods 0.000 abstract description 3
- 229910052742 iron Inorganic materials 0.000 abstract description 3
- 238000005065 mining Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 238000011112 process operation Methods 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000000921 elemental analysis Methods 0.000 description 2
- 231100000572 poisoning Toxicity 0.000 description 2
- 230000000607 poisoning effect Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 230000001131 transforming effect Effects 0.000 description 1
- -1 uranyl ions Chemical class 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J49/00—Regeneration or reactivation of ion-exchangers; Apparatus therefor
- B01J49/50—Regeneration or reactivation of ion-exchangers; Apparatus therefor characterised by the regeneration reagents
- B01J49/57—Regeneration or reactivation of ion-exchangers; Apparatus therefor characterised by the regeneration reagents for anionic exchangers
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Environmental & Geological Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention belongs to CO 2 +O 2 The technical field of hydrometallurgy post-treatment engineering of an in-situ leaching uranium mining process, and particularly relates to a D231-YT anion exchange resin detoxification process. A D231-YT anion exchange resin detoxification process comprises the following steps: step 1: preparing detoxification reagent; step 2: preparing detoxification resin; step 3: detoxification of the resin; step 4: and (5) preparing the detoxication resin by adsorption. The invention has the remarkable effects that: the developed resin detoxification formula is used for carrying out detoxification process operation on toxic substances such as Fe, al, ca, si and macromolecular organic matters on the toxic resin, separating the toxic substances from resin functional groups, and recovering the adsorption performance of the resin so as to improve the hydrometallurgical benefit.
Description
Technical Field
The invention belongs to CO 2 +O 2 The technical field of hydrometallurgy post-treatment engineering of an in-situ leaching uranium mining process, and particularly relates to a D231-YT anion exchange resin detoxification process.
Background
In CO 2 +O 2 In the in-situ leaching uranium mining hydrometallurgy post-treatment process, along with the gradual exchange behavior of uranyl ions in the leaching liquid and counter ions on a resin exchange group, the preliminary enrichment of metal uranium from liquid phase to solid phase is realized. In the ion exchange process, other forms of anions are often adsorbed strongly as useful components, and also occupy a part of functional groups, or small molecular inorganic salts are subjected to local pH condition change to cause sedimentation phenomenon in resin pores to block pore channels, and conventional eluent and converting agent cannot completely remove the substances, so that the substances are accumulated continuously until the resin exchange performance is obviously influenced, and the phenomena of reduced adsorption capacity, prolonged adsorption time and the like, namely resin poisoning, are mainly shown. The degradation benefit of hydrometallurgy is seriously reduced and the process is uncontrolled directly after resin poisoning.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a D231-YT anion exchange resin detoxification process.
The invention is realized in the following way: a D231-YT anion exchange resin detoxification process comprises the following steps:
step 1: preparing detoxification reagent;
step 2: preparing detoxification resin;
step 3: detoxification of the resin;
step 4: and (5) preparing the detoxication resin by adsorption.
The step 1 comprises the steps of taking a transforming agent preparation tank as an antidote preparation tool, adding adsorption tail liquid into the tank, opening a stirring paddle, opening a blow-down valve at the bottom of the preparation tank, and cleaning the tank. After cleaning, closing a blow-down valve, opening a clear water inlet valve at the top of a preparation tank, opening a stirring paddle, and sequentially adding detoxification reagents according to a certain proportion: hydrochloric acid, hydrofluoric acid and hydrogen peroxide are fully stirred until the solution is uniform, and the preparation of the detoxification reagent is completed.
The D231-YT anion exchange resin detoxification process comprises the step 1, wherein in the step of adding adsorption tail liquid into a tank, the liquid level of the adsorption tail liquid is 1 meter, and the stirring time is 1 hour.
In the step 1, the clear water inlet valve at the top of the preparation tank is opened, the clear water inlet is stopped when the liquid level reaches 0.5 m of the notch, and the stirring paddle is opened.
The step 2 comprises that the toxic resin uranium adsorption tower is sent to a leaching transformation tower through a saturated resin escort tank, leaching is carried out in a three-tower series upper liquid inlet mode, after the leaching process is finished, lean liquid in the tower is compressed by using compressed air, lean resin is washed in the same liquid inlet mode by using adsorption tail liquid, after washing is finished, a compressed air inlet valve at the top of a blow-down valve at the bottom of the leaching tower is opened, liquid in the tower is emptied, and resin detoxification process preparation is finished.
In the process for detoxifying the D231-YT anion exchange resin, in the step 2, the cleaning volume is 2 times of the bed volume in the step of cleaning the lean resin by using the adsorption tail liquid.
The step 3 comprises opening a liquid inlet valve of a transfer agent pipeline of the leaching transfer tower, using the transfer agent pipeline for detoxification, opening a liquid outlet valve at the bottom of the tower, directly connecting to an evaporation tank, and using a frequency converter to regulate liquid inlet flow.
The D231-YT anion exchange resin detoxification process comprises the steps of controlling the contact time to be 24 hours in the step 3, wherein the liquid-solid ratio is 2:1, the liquid feeding mode is upper liquid feeding, and tail liquid enters an evaporation tank.
The step 4 comprises the step of pressing down the liquid in the tower in the same way after the detoxification is completed, opening a tower top tail liquid inlet valve, starting to clean the resin, and enabling the cleaning liquid to enter an evaporation tank. After the cleaning is finished, the tail liquid inlet valve is closed, the tower bottom liquid outlet valve is opened, the tower top compressed air inlet valve and the tower bottom resin transfer valve are opened, resin is transferred to the resin escort tank, and the resin is further transferred to the compaction layer at the top of the adsorption tower through the resin transfer process, so that the detoxification process is completely finished.
The D231-YT anion exchange resin detoxification process comprises the step 4, wherein a step of cleaning the resin is started, and the liquid-solid ratio is 5:1.
The invention has the remarkable effects that: the developed resin detoxification formula is used for carrying out detoxification process operation on toxic substances such as Fe, al, ca, si and macromolecular organic matters on the toxic resin, separating the toxic substances from resin functional groups, and recovering the adsorption performance of the resin so as to improve the hydrometallurgical benefit.
Drawings
FIG. 1 depicts a resin electron microscope image prior to detoxification;
FIG. 2 depicts a resin electron microscope image after detoxification;
FIG. 3 is a table of elemental analysis versus before and after detoxification of the resin;
FIG. 4 resin recovery data for adsorption performance before and after detoxification.
Detailed Description
A D231-YT anion exchange resin detoxification process comprises the following steps:
(1) Preparation of detoxification reagent
The conversion agent preparation tank is used as an antidote preparation tool, firstly, adsorption tail liquid is added into the tank, the liquid level is 1 meter, a stirring paddle is opened, stirring is carried out for 1 hour, a blow-down valve at the bottom of the preparation tank is opened, and tank cleaning is carried out. After cleaning, closing a drain valve, opening a clear water inlet valve at the top of the preparation tank, closing clear water inlet at the position of 0.5 m from the liquid level to the notch, opening a stirring paddle, and sequentially adding detoxification reagents according to a certain proportion: hydrochloric acid, hydrofluoric acid and hydrogen peroxide are fully stirred until the solution is uniform, and the preparation of the detoxification reagent is completed.
(2) Preparation of detoxification resin
The toxic resin uranium adsorption tower is sent to a leaching transformation tower through a saturated resin escort tank, a leaching process is carried out in a mode of feeding liquid into three towers in series, after the leaching process is finished, lean liquid in the tower is compressed by using compressed air, lean resin is cleaned in the same feeding liquid mode by using adsorption tail liquid, the cleaning volume is 2 times of the bed volume, after the cleaning is finished, a compressed air inlet valve at the top of a blow-down valve at the bottom of the leaching tower is opened, liquid in the tower is emptied, and the preparation of the resin detoxification process is finished.
(3) Detoxification of resin
Opening a liquid inlet valve of a transfer agent pipeline of the leaching transfer tower (a transfer agent pipeline is used for detoxification), opening a liquid outlet valve at the bottom of the tower (directly connected to the evaporation tank), adjusting liquid inlet flow by using a frequency converter, controlling the contact time to be 24 hours, controlling the liquid-solid ratio to be 2:1, and feeding liquid in an upper liquid inlet mode and feeding tail liquid into the evaporation tank.
(4) Preparation of detoxified resin adsorption
After the detoxification is completed, the liquid in the tower is compressed in the same way, a liquid inlet valve of the tail liquid at the top of the tower is opened, the resin is cleaned, the liquid-solid ratio is 5:1, and the cleaning liquid enters the evaporation pool. After the cleaning is finished, the tail liquid inlet valve is closed, the tower bottom liquid outlet valve is opened, the tower top compressed air inlet valve and the tower bottom resin transfer valve are opened, resin is transferred to the resin escort tank, and the resin is further transferred to the compaction layer at the top of the adsorption tower through the resin transfer process, so that the detoxification process is completely finished.
As can be seen from fig. 1 and 2: the resin surface is clearly seen to be wrapped from the electron microscope image, and flocculate is attached, so that the flocculate and the wrapping on the resin surface are basically eliminated after detoxification. The elemental analysis result of the detoxification resin shows that substances such as calcium, aluminum, iron, silicon and the like are basically eliminated, the content of concentrated main toxicants is detected in the detoxification liquid, and the resin performance is recovered to 95.5mg/mlR after the resin is detoxified, and the rise and fall reach 79.4%.
Claims (10)
1. A D231-YT anion exchange resin detoxification process is characterized by comprising the following steps:
step 1: preparing detoxification reagent;
step 2: preparing detoxification resin;
step 3: detoxification of the resin;
step 4: and (5) preparing the detoxication resin by adsorption.
2. A process for detoxification of D231-YT anion exchange resin as defined in claim 1, wherein: step 1 include, prepare the groove with the transformation agent and regard as antidote to prepare the instrument, add at first to the inslot and adsorb the tail liquid to open the stirring rake, open and prepare the tank bottom blowoff valve, carry out tank cleaning, close the blowoff valve after accomplishing the cleaning, open and prepare tank top clear water feed liquor valve, open the stirring rake, add detoxification reagent according to certain ratio in proper order: hydrochloric acid, hydrofluoric acid and hydrogen peroxide are fully stirred until the solution is uniform, and the preparation of the detoxification reagent is completed.
3. A process for detoxification of D231-YT anion exchange resin as defined in claim 2, wherein: in the step 1, in the step of adding the adsorption tail liquid into the tank, the liquid level of the adsorption tail liquid is 1 meter, and the stirring time is 1 hour.
4. A process for detoxification of D231-YT anion exchange resin as defined in claim 3, wherein: in the step 1, in the step of opening the clear water inlet valve at the top of the preparation tank, the clear water inlet is stopped when the liquid level reaches 0.5 m of the notch, and the stirring paddle is opened.
5. A process for detoxification of D231-YT anion exchange resin as defined in claim 1, wherein: step 2 comprises that the toxic resin uranium adsorption tower is sent to a leaching transformation tower through a saturated resin escort tank, leaching technology is carried out in a mode of feeding liquid into three towers in series, after the leaching technology is finished, lean liquid in the tower is leached by compressed air, lean resin is cleaned in the same feeding liquid mode by using adsorption tail liquid, after cleaning is finished, a compressed air inlet valve at the top of a blow-down valve at the bottom of the leaching tower is opened, liquid in the tower is emptied, and resin detoxification technology preparation is finished.
6. The process for detoxification of D231-YT anion exchange resin as defined in claim 5, wherein: in the step 2, the cleaning volume is 2 times of the bed volume in the step of cleaning the lean resin by using the adsorption tail liquid.
7. A process for detoxification of D231-YT anion exchange resin as defined in claim 1, wherein: and step 3, opening a liquid inlet valve of a transfer agent pipeline of the leaching transfer tower, using the transfer agent pipeline for detoxification, opening a liquid outlet valve at the bottom of the tower, directly connecting to an evaporation pond, and using a frequency converter to regulate liquid inlet flow.
8. A process for detoxification of D231-YT anion exchange resin as defined in claim 7, wherein: in the step 3, the contact time is controlled to be 24 hours, the liquid-solid ratio is 2:1, the liquid feeding mode is upper liquid feeding, and tail liquid enters an evaporation tank.
9. A process for detoxification of D231-YT anion exchange resin as defined in claim 1, wherein: step 4 includes that after detoxification is completed, liquid in the tower is compressed in the same mode, a tower top tail liquid inlet valve is opened, resin starts to be cleaned, cleaning liquid enters an evaporation pond, after cleaning is completed, the tail liquid inlet valve is closed, a tower bottom liquid outlet valve is opened, a tower top compressed air inlet valve is opened, a tower bottom resin transfer valve is used for transferring resin to a resin escort tank, and the resin is further transferred to a tower top compaction layer of an adsorption tower through a resin transfer process, so that the detoxification process is completed completely.
10. A process for detoxification of D231-YT anion exchange resin as defined in claim 9, wherein: in the step 4, a step of cleaning the resin is started, and the liquid-solid ratio is 5:1.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111618432.5A CN116351480A (en) | 2021-12-27 | 2021-12-27 | D231-YT anion exchange resin detoxification process |
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| CN202111618432.5A CN116351480A (en) | 2021-12-27 | 2021-12-27 | D231-YT anion exchange resin detoxification process |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117467862A (en) * | 2023-12-22 | 2024-01-30 | 核工业北京化工冶金研究院 | Method for preventing resin organic matter poisoning in neutral leaching uranium mining hydrometallurgy process |
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Cited By (2)
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| CN117467862A (en) * | 2023-12-22 | 2024-01-30 | 核工业北京化工冶金研究院 | Method for preventing resin organic matter poisoning in neutral leaching uranium mining hydrometallurgy process |
| CN117467862B (en) * | 2023-12-22 | 2024-03-29 | 核工业北京化工冶金研究院 | Method for preventing resin organic matter poisoning in neutral leaching uranium mining hydrometallurgy process |
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