CN109692715A - A kind of method that ground-dipping uranium extraction solves resin poison and blocking - Google Patents
A kind of method that ground-dipping uranium extraction solves resin poison and blocking Download PDFInfo
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- CN109692715A CN109692715A CN201910079377.3A CN201910079377A CN109692715A CN 109692715 A CN109692715 A CN 109692715A CN 201910079377 A CN201910079377 A CN 201910079377A CN 109692715 A CN109692715 A CN 109692715A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J49/00—Regeneration or reactivation of ion-exchangers; Apparatus therefor
- B01J49/60—Cleaning or rinsing ion-exchange beds
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- 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
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Abstract
The invention belongs to neutral or alkaline Leaching ground-dipping uranium extraction technical fields, and in particular to a kind of method that ground-dipping uranium extraction solves resin poison and blocking.For resin organic matter intoxicating phenomenon, there are reagent consumptions for prior art processes greatly, preparation labor intensity is high, immersion effect resin property and resin inside introduce OH to high concentration soda acid repeatedly‑, in absorption, may cause the resin further drawbacks such as hardened.The present invention includes: step 1: analysis sediment ingredient and resin poison reason；Step 2: processing scheme is determined；Step 3: clear water recoil；Step 4: preparation of reagents and immersion；Step 5: adsorption tail liquid combines compressed air recoil；Step 6: observation processing.The present invention can effectively improve working efficiency, and cost is relatively low compared with domestic and international used method, have great advantages and utility value.
Description
Technical field
The invention belongs to neutral or alkaline Leaching ground-dipping uranium extraction technical fields, and in particular to a kind of ground-dipping uranium extraction solution resin
The method of poisoning and blocking.
Background technique
In neutral and alkaline Leaching In-situ Leaching Uranium Mine production process, ion exchange resin poisoning and clogging deposits are existing
As occurring often, resin poison not only reduces the saturated capacity of resin, but also increases the consumption of post-treatment reagents, and raising is produced into
This；Resin blocking is even more the great difficult problem that In-situ Leaching Uranium Mine enterprise faces, the work that each mine processing resin blockage problem uses
Process also has difference, but not can effectively solve resin poison, blockage problem.
It is higher to receive carbonate in the ditch Uranium deposit ore of ridge, pyrite, feldspar ore and the content of organic matter, and when exploitation uses CO2+
O2In-situ leaching process, the technique while Leaching Uranium, can react with the gangue mineral in ore causes largely non-utilities
It is leached and as leachate enters ion exchange system, according to resin saturated capacity and appearance color situation of change and in tower
Sediment ingredient sampling analysis determines that causing the main matter of resin poison is organic matter, predominantly there is resin tamper in tower
Machine matter, carbonate, iron hydroxide, aluminium hydroxide and precipitation of silica object.
Due to receiving ridge ditch uranium hydrometallurgy adsorption process ion exchange resin, there are serious poisonings, chemical precipitates and machinery
Suspended particle clogging phenomenon, the influence to hydrometallurgy absorbing process can not be ignored.Field operational data analysis is found, the tree of tower is newly entered
Rouge was run in about 180 days or so time, and adsorption tower single column average flow rate is 40.2m3/ h, tower body pressure < 0.13MPa, at it
Adsorption tower single column processing capacity is dropped rapidly to less than 15m in the time less than 15 days afterwards3/h；Resin is adsorbed at continuous four times
After circulation, saturated capacity is by initial 130.2mgU/ml (RIt is wet) drop to 92.3mgU/ml (RIt is wet), rate of descent reaches 29.1%,
And resin appearance color is gradually deepened, and faint yellow is changed into light brown, dark-brown, sepia and dark brown by initial.
For resin hardened phenomenon, domestic outer portion CO2+O2In-situ Leaching Uranium Mine takes measures are as follows:
(1) giant is used to destroy resin hardening layer to ensure the normal operation of absorbing process, but established hardened
Object remains between resin, and after running a period of time, hardened object reassembles and influence the normal operation of absorbing process；
(2) remove partly precipitated object object using a large amount of water modes such as poor resin that recoil, but the program be not thorough in the presence of cleaning,
The problems such as resin cycle-index that treated is few and the outer discharge capacity of waste water is larger.
(3) the 13 groups of popularization tests of ridge ditch are received using resin transfer techniques solution resin blockage problem, but the technology is not
Sediment between energy Scavenger resin, meanwhile, there are certain abrasions in transfer process for resin, the waste of resin is not only caused, and
And the separation of the resin and completed resin after wearing is extremely difficult, the accumulative liquid energy excessively for further affecting resin of toner
Power.
(4) separate sediment with resin by the way of screening for hardened resin, but this technique is to fine particle shape
The separation of sediment is more applicable in, and receive sediment in the ditch uranium deposit adsorption tower of ridge is in bulky grain floccule more, due to its adherency
Property it is larger compared with strong and floc sedimentation, separate resin with floccule extremely difficult, by field test, only with
The program, which cannot reach, thoroughly to be solved the problems, such as to receive ridge ditch resin and blocks.
For resin organic matter intoxicating phenomenon, measure is generally used both at home and abroad are as follows:
Resin is impregnated using the hydrochloric acid solution and sodium hydroxide solution of high concentration, i.e., is first impregnated the hydrochloric acid solution of high concentration
Resin, the sodium hydroxide solution for then reusing high concentration impregnate resin.There are reagent consumptions for the technique greatly, it is strong to prepare labour
Degree is high, immersion effect resin property and resin inside introduce OH to high concentration soda acid repeatedly-, absorption when, may cause resin into
The drawbacks such as one step is hardened.
Summary of the invention
One, purpose
The solution resin poison that uranium mine uses, choked technique method are adopted not for domestic and international neutral or alkaline in situ leach
Foot is not additionally introducing other impurities ion and as few as possible broken according to resin poison reason and each sediment physico-chemical property
In the case where bad resin properties, the present invention provides a kind of resin removing toxic substances de-plugging integral process (hydrochloric acid and hydrogen peroxide solution leachings
Bubble, compressed air agitate the process integration with adsorption tail liquid recoil) toxiresin in blocking and organic matter is handled, reach and disappears
Except the purpose of sediment, recovery resin exchange capacity between resin.
Two, technical solution
Neutral or alkaline in situ leach adopts the technical solution of uranium mine resin removing toxic substances de-plugging integral process are as follows:
1. analyzing sediment ingredient and resin poison reason
(1) by analysis sediment ingredient, determine that sediment is mainly organic matter, carbonate, iron hydroxide, aluminium hydroxide
And precipitation of silica object；
(2) it by comparative analysis resin appearance color and resin saturated capacity situation of change, and combines and receives ridge ditch ore group
Divide, impurity composition and content in neutral ground-dipping uranium extraction characteristic and leachate, determines that the reason of causing resin saturated capacity to decline is
Organic matter poisoning.
2. determining processing scheme
Not additionally introduce except Cl-And HCO3 -Before outer other impurities ion and destruction resin properties as few as possible are
Mention, according to organic matter, carbonate, iron hydroxide, alumino-silicate physico-chemical property, determine hydrochloric acid and 2% hydrogen peroxide solution leaching
Bubble, compressed air agitate the process integration with adsorption tail liquid recoil.
3. clear water recoils
Eluent remaining in tower is emptied using compressed air, tower is then filled by tower bottom using reverse osmosis clear water, to tower
After interior solution is filled, continue the resin that recoils using reverse osmosis clear water, this stage control flow velocity is 3~4m/h, when recoil water outlet reaches
To 0.5V/VRWhen, stop recoil, and solution remaining in tower is emptied using compressed air.
4. preparation of reagents and immersion
The H for being 2% in concentration2O2Hydrochloric acid is added in solution, the mixed solution of preparation is poured into adsorption tower by tower bottom and is impregnated
Resin 12h is passed through compressed air 15min by tower bottom every 2h in soaking process, the bubble generated in discharge tower and make reagent with
Resin and sediment come into full contact with reaction.
5. adsorption tail liquid combines compressed air recoil
It uses flow velocity to backwash resin for the adsorption tail liquid of 5~8m/h, after flow velocity adjusts and stablizes, compression is passed through by tower bottom
During which air agitation resin bed controls adsorption column pressure in 0.45MPa hereinafter, adjusting backwash when the water outlet that recoils is more clear
Flow velocity carries out ion exchange resin conversion to 1.5m/h, and transition haline water is discharged into evaporation tank, and low-solids water, which enters reverse osmosis unit, to carry out at desalination
Reason, gained clear water enters clear water storage tank after processing, uses in case preparing removing toxic substances de-plugging agent.
6. observation is handled
By taking resin-like observation to judge that sediment removes situation, and is run according to resin adsorption and determine resin saturated capacity
And cross liquid measure and restored, achieve the purpose that resin removing toxic substances de-plugging.
CO is added before using tower in resin absorption technique2Mode adjust into tower solution ph to 6.5~6.8, make molten into tower
Subacidity is presented in liquid, inhibits the generation of carbonate sediment, slows down resin blocking speed, it is ensured that resin crosses fluidity energy.
Three, effect
Hydrochloric acid and hydrogen peroxide solution are impregnated can achieve the effect that resin de-plugging and removing toxic substances with adsorption tail liquid bounce home test simultaneously,
Using the technical solution, to receive ridge ditch uranium deposit expanding test elution after poor resin handle and has been applied, it is logical
Overwriting, analysis adsorption tower single cycle operation data, and sampling analysis saturated resin capacity, obtain, resin is saturated after processing
Capacity restoration to initial capacity 95% or more (table 1), adsorption tower cross liquid measure restore to it is initial cross liquid measure 96% or more (table
2)。
The 10 tower resin saturated capacity recovery situations of table 1 after treatment
Be averaged liquid measure situation of change after the processing of 2 adsorption tower of table
It uses and is agitated with adsorption tail liquid recoil process integration using hydrochloric acid and hydrogen peroxide solution immersion, compressed air as core
Resin removing toxic substances and de-plugging integral process, significantly receive ridge ditch uranium deposit hydrometallurgy adsorption conditions, successfully alleviate and receive ridge 30
Group scale ditch expanding test hydrometallurgy runs existing outstanding problem, compared with domestic and international used method, can effectively improve work
Efficiency, and cost is relatively low, has great advantages and utility value, the industrial project that may be directly applied to Na Linggou uranium deposit are built
And if running, and can be to there are the mines of similar problems to provide reference frame.
Specific embodiment
Between existed liquid ability is greatly lowered, tower body pressure is substantially increased, sample in discovery tower body exist resin it is big
Amount sediment, the variation of resin appearance color is obvious and saturated capacity declines the ion exchange tower for being abnormal situation such as larger, really
It is fixed to be poisoned and blocked.
Firstly, according to type (Cl type and the HCO of the poor resins exchange group of ridge ditch is received3Type), not additionally introduce except Cl-And
HCO3 -Premised on outer other impurities ion and destruction resin properties as few as possible, according to organic matter, carbonate, hydroxide
Iron, the suitable separation of physico-chemical property selection of alumino-silicate and dissolving method.It is normal by the organic matter in resin adsorption and sediment
Removing method is oxidation, macromolecular organic matter decomposition can be made at gas or the small molecule of solubility using suitable oxidant
Organic matter selects H during test2O2With two kinds of oxidants of NaClO.For carbonate, iron hydroxide and aluminum hydroxide precipitation
Object, since it is soluble in acid, and Fe (OH)3It can be completely dissolved when pH value is less than 2.5, Al (OH)3It can when pH value is less than 4.0
It is completely dissolved, Ca (Mg) CO3It can be completely dissolved when pH value is less than 5.5.It therefore, can be by three of the above sediment using acid solution
It is completely dissolved, and forms soluble ion, solution ph, can perfect solution iron, aluminium 2.0~2.5 after control reaction when use
And calcium, magnesium precipitate object, 35% technical hydrochloric acid are the common raw material in scene, price is lower, and do not additionally introduce other impurities from
Therefore son selects lytic agent of the technical hydrochloric acid as carbonate, iron hydroxide and aluminum hydroxide precipitate, according to field test,
Show that clear water amount needed for impregnating every cube of resin is 0.6m3, hydrochloric acid dosage 24L.With this condition, various concentration has been prepared
H2O2Carry out the immersion treatment repeatedly of 10 circulations to resin respectively with NaClO solution, and between contents of precipitate resin after immersion
And the properties of resin are analyzed, are detected, and obtain H2O2When concentration >=2%, NaClO concentration >=0.25%, resins exchange is held
It is preferable to measure sediment removal situation between recovery situation and resin, but NaClO of the concentration higher than 0.25% destroys the performance of resin
It is larger, and unstable chemcial property easily decomposes and generates chlorine NaClO in acid condition, when preparation, smell is larger, has to human body
It seriously endangers, therefore selects the remover of 2% hydrogen peroxide as organic matter.Such as dioxy undissolvable for chemical dissolution method
SiClx sediment installs suitable filter in tower top according to resin size situation, using big flow adsorption tail liquid recoil with
The method that compressed air agitates process integration recoil disturbance resin bed, flushes out retained sediments object between resin.
Secondly, eluent remaining in tower is emptied using compressed air, tower is then filled by tower bottom using reverse osmosis clear water,
After solution is filled in tower, continue the resin that recoils using reverse osmosis clear water, to replace remaining eluent in tower, reduces at resin
Reagent dosage when reason.
Again, the H for being 2% in concentration2O2Hydrochloric acid is added in solution, the mixed solution of preparation is inversely poured into tower by tower bottom
It is interior, and resin is impregnated, timing is passed through compressed air by tower bottom in soaking process, and the bubble that reaction generates in discharge tower simultaneously makes reagent
It comes into full contact with and reacts with resin and sediment.
Then, resin is backwashed using the adsorption tail liquid of certain flow rate, after flow velocity adjusts and stablizes, compression is passed through by tower bottom
Air agitation resin bed, on the one hand loosens resin bed, safety caused by avoiding recoil initial stage tower bottom pressure excessively high
Hidden danger, the compressed air disturbance resin bed being on the other hand passed through, makes the partly precipitated object for being adhered to resin surface and resin point
From, and the floccule mass that can destroy bulky grain sediment is allowed to form short grained sediment, consequently facilitating the development of recoil technique,
And it can reach the purpose for reducing recoil water consumption.During recoil, control adsorption column pressure within the specified scope, wait recoil water outlet compared with
When clear, adjust backwash flow velocity and carry out ion exchange resin conversion, transition haline water is discharged into evaporation tank, and low-solids water enters reverse osmosis unit progress
Desalting processing, gained clear water enters clear water storage tank after processing, uses in case preparing removing toxic substances de-plugging agent.
Finally, CO is added before using tower in resin absorption technique2Mode adjust into tower solution ph, make into tower solution present
Subacidity inhibits the generation of carbonate sediment, slows down resin blocking speed, it is ensured that resin crosses fluidity energy.
Claims (7)
1. a kind of method that ground-dipping uranium extraction solves resin poison and blocking, it is characterised in that: step 1: analysis sediment ingredient and
Resin poison reason；Step 2: processing scheme is determined；Step 3: clear water recoil；Step 4: preparation of reagents and immersion；Step
Five: adsorption tail liquid combines compressed air recoil；Step 6: observation processing；The step 4 includes: the H for being 2% in concentration2O2It is molten
Hydrochloric acid is added in liquid, the mixed solution of preparation is poured into adsorption tower immersion resin 12h by tower bottom, in soaking process every 2h by
Tower bottom is passed through compressed air 15min, and the bubble generated in tower is discharged and comes into full contact with reagent with resin and sediment and reacts.
2. the method that a kind of ground-dipping uranium extraction as described in claim 1 solves resin poison and blocking, it is characterised in that: described
Step 1 includes: (1) by analysis sediment ingredient, determines that sediment is mainly organic matter, carbonate, iron hydroxide, hydrogen-oxygen
Change aluminium and precipitation of silica object；(2) it by comparative analysis resin appearance color and resin saturated capacity situation of change, and combines
Receive ridge ditch ore composition, impurity composition and content in neutral ground-dipping uranium extraction characteristic and leachate, determination causes resin saturated capacity
The reason of decline is organic matter poisoning.
3. the method that a kind of ground-dipping uranium extraction as described in claim 1 solves resin poison and blocking, it is characterised in that: described
Step 2 includes: not additionally introduce except Cl-And HCO3 -Outer other impurities ion and destruction resin properties as few as possible are
Premise, according to organic matter, carbonate, iron hydroxide, alumino-silicate physico-chemical property, determine the hydrogen peroxide solution of hydrochloric acid and 2%
It impregnates, compressed air agitates the process integration to recoil with adsorption tail liquid.
4. the method that a kind of ground-dipping uranium extraction as described in claim 1 solves resin poison and blocking, it is characterised in that: described
Step 3 includes: to be emptied eluent remaining in tower using compressed air, then fills tower by tower bottom using reverse osmosis clear water, to
After solution is filled in tower, continue the resin that recoils using reverse osmosis clear water, this stage control flow velocity is 3~4m/h, when recoil is discharged
Reach 0.5V/VRWhen, stop recoil, and solution remaining in tower is emptied using compressed air.
5. the method that a kind of ground-dipping uranium extraction as described in claim 1 solves resin poison and blocking, it is characterised in that: described
Step 6 includes: to run determining resin saturation by taking resin-like observation to judge sediment removal situation, and according to resin adsorption
Capacity and liquid measure excessively have been restored, and achieve the purpose that resin removing toxic substances de-plugging.
6. the method that a kind of ground-dipping uranium extraction as claimed in claim 5 solves resin poison and blocking, it is characterised in that: described
Step 6 further include: CO is added before using tower in resin absorption technique2Mode adjust into tower solution ph to 6.5~6.8, make into
Subacidity is presented in tower solution, inhibits the generation of carbonate sediment, slows down resin blocking speed, it is ensured that resin crosses fluidity energy.
7. the method that a kind of ground-dipping uranium extraction as described in claim 1 solves resin poison and blocking, it is characterised in that: described
Step 5 includes: that flow velocity is used to backwash resin for the adsorption tail liquid of 5~8m/h, after flow velocity adjusts and stablizes, is passed through by tower bottom
Compressed air disturbs resin bed, during which controls adsorption column pressure in 0.45MPa hereinafter, adjusting anti-when the water outlet that recoils is more clear
Irrigation flow rate carries out ion exchange resin conversion to 1.5m/h, and transition haline water is discharged into evaporation tank, and low-solids water enters reverse osmosis unit and taken off
Salt treatment, gained clear water enters clear water storage tank after processing, uses in case preparing removing toxic substances de-plugging agent.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111905842A (en) * | 2020-08-21 | 2020-11-10 | 四川省宜宾惠美线业有限责任公司 | Method for treating poisoned anion resin |
| CN112680606A (en) * | 2020-12-16 | 2021-04-20 | 核工业北京化工冶金研究院 | Ion exchange method for gas generation in uranium extraction process |
| CN113058663A (en) * | 2021-04-09 | 2021-07-02 | 中核四0四有限公司 | Detoxification regeneration method of ion exchange resin for uranium adsorption |
| CN114369732A (en) * | 2021-12-09 | 2022-04-19 | 中核内蒙古矿业有限公司 | CO (carbon monoxide)2+O2Multi-reagent combined well flushing method for in-situ leaching uranium mining mine |
| CN114369729A (en) * | 2021-12-28 | 2022-04-19 | 江苏容汇通用锂业股份有限公司 | Process for removing potassium from leaching solution by using lithium slag |
| CN114534800A (en) * | 2022-03-23 | 2022-05-27 | 中陕核工业集团综合分析测试有限公司 | Regeneration method of uranium-containing poisoning saturated resin |
| CN115945229A (en) * | 2022-12-02 | 2023-04-11 | 中核内蒙古矿业有限公司 | Ion exchange resin regeneration method |
| CN116351479A (en) * | 2021-12-27 | 2023-06-30 | 新疆中核天山铀业有限公司 | Anion exchange resin detoxification process |
| CN116351480A (en) * | 2021-12-27 | 2023-06-30 | 新疆中核天山铀业有限公司 | D231-YT anion exchange resin detoxification process |
| 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 (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111905842A (en) * | 2020-08-21 | 2020-11-10 | 四川省宜宾惠美线业有限责任公司 | Method for treating poisoned anion resin |
| 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 |
| CN112680606A (en) * | 2020-12-16 | 2021-04-20 | 核工业北京化工冶金研究院 | Ion exchange method for gas generation in uranium extraction process |
| CN113058663A (en) * | 2021-04-09 | 2021-07-02 | 中核四0四有限公司 | Detoxification regeneration method of ion exchange resin for uranium adsorption |
| CN114369732A (en) * | 2021-12-09 | 2022-04-19 | 中核内蒙古矿业有限公司 | CO (carbon monoxide)2+O2Multi-reagent combined well flushing method for in-situ leaching uranium mining mine |
| CN114369732B (en) * | 2021-12-09 | 2023-10-20 | 中核内蒙古矿业有限公司 | CO (carbon monoxide) 2 +O 2 Multi-reagent combined well flushing method for in-situ leaching uranium mining mine |
| CN116351479A (en) * | 2021-12-27 | 2023-06-30 | 新疆中核天山铀业有限公司 | Anion exchange resin detoxification process |
| CN116351480A (en) * | 2021-12-27 | 2023-06-30 | 新疆中核天山铀业有限公司 | D231-YT anion exchange resin detoxification process |
| CN114369729A (en) * | 2021-12-28 | 2022-04-19 | 江苏容汇通用锂业股份有限公司 | Process for removing potassium from leaching solution by using lithium slag |
| CN114369729B (en) * | 2021-12-28 | 2023-11-03 | 江苏容汇通用锂业股份有限公司 | Process for removing potassium from leaching solution by utilizing lithium slag |
| CN114534800A (en) * | 2022-03-23 | 2022-05-27 | 中陕核工业集团综合分析测试有限公司 | Regeneration method of uranium-containing poisoning saturated resin |
| CN115945229A (en) * | 2022-12-02 | 2023-04-11 | 中核内蒙古矿业有限公司 | Ion exchange resin regeneration method |
| 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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