CN103846081A - Acidic resolution process for D382 type resin - Google Patents
Acidic resolution process for D382 type resin Download PDFInfo
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- CN103846081A CN103846081A CN201210518105.7A CN201210518105A CN103846081A CN 103846081 A CN103846081 A CN 103846081A CN 201210518105 A CN201210518105 A CN 201210518105A CN 103846081 A CN103846081 A CN 103846081A
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Abstract
The invention provides a resolution and transformation process for D382 type resin under a high-mineralization and high-chloride alkaline-process leaching condition, wherein the resolution and transformation process is simple and convenient to operate and environment-friendly as well. The resolution process is advantageous in that the resolution process is simplified, the resolution flow ratio is reduced, the uranium concentration of qualified liquid is increased, and the consumption of technical salt and ammonium bicarbonate is prevented; compared with an alkaline resolution process, the acidic resolution process has the advantages of lowering the production cost, reducing the working strength of staff, preventing emission of ammonia gas and being simpler and more environment-friendly in operating procedures.
Description
Technical field
The invention belongs to ground-dipping uranium extraction hydrometallurgy processing technology field, be specifically related to parsing, the transformation process of D382 type resin under " high mineralization, high chlorine root " alkaline Leaching condition.
Background technology
The technology of soaking obtains successfully and in the whole nation and develops rapidly at Yi Li uranium mine acid system, but can only be with the neutral extract technology of weak reagent in more complicated certain mine of geological conditions, this mine grade of ore is low simultaneously, leachate uranium concentration is low, " the high salinity of leachate, high chloride ion " make most of resin adsorption uranium not substantially, under the cooperation of Hua Ye institute, develop D382 type resin, take this model resin leachate aftertreatment technology flow process can be adapted to this mineral deposit " high salinity, high chloride ion " the leachate processing of content, and can be satisfied with " low concentration, large flow " leachate process conditions.But industrial experiment initial stage resin treatment need be carried out in two steps, sodium chloride adds carbonic acid oronain to carry out alkalescence and resolves, and then makes the transition with technical hydrochloric acid, this technological process is too much, troublesome poeration, and workload is large, raw-material consumption is large, the unfavorable workman's physical and mental health of operating process ammonia emission.Therefore, the utmost point need be developed a kind of toxic emission minimizing, the acid technique of resolving of operation D382 type easy to operate and more environmental protection resin.
Summary of the invention
The object of the invention is to overcome the defect of prior art, parsing, the transformation process of the easy and simple to handle and environmental protection of a kind of D382 type resin under " high mineralization, high chlorine root " alkaline Leaching condition is provided.
To achieve these goals, technical scheme of the present invention is that the acid technique of resolving of a kind of D382 type resin, comprises following steps:
Step 1, after D382 type resin adsorption is saturated, will be adsorbed in the impurity cleanings such as silt in resin particle gap through backwash operation, rear with the compressed air of 0.2MPa pressure by for subsequent use the drain in resin particle gap;
Step 2, is mixed with acidifying solution by qualifying liquid, technical hydrochloric acid according to the ratio of volume ratio 14～16:3, after the volume of configuration acidifying solution must satisfied be full of the adsorption tower that comprises D382 type resin completely, also has 1m
3surplus; Then 60% acidifying solution is wherein delivered in adsorption tower, to soaking through step 1 D382 type after treatment resin, soak time is 6～8 hours;
Step 3, by adsorption tower and outside adsorption tower acidifying solution circulate, endless form adopts lower feed liquor, the mode of upper fluid; Circulate and monitor circulation fluid pH after 6～8 hours, when feed liquor and fluid pH value reach consistent and≤stop circulation 1.5 time; If pH value is below standard, add 0.5m
3technical hydrochloric acid, continues circulation, until feed liquor and fluid pH value reach consistent and≤1.5 o'clock;
Step 4, enters parsing operation after completing steps 3, resolve operation and select the hydrochloric acid solution that parsing agent is 3～4g/L, adopts three tower cascade connected parsing, and analysis mode adopts upper feed liquor, lower fluid, and in adsorption tower, the linear velocity of desorbed solution is 0.8～1.0m/h; Stop into parsing agent when parsing when liquid flowing ratio reaches 2 left and right, obtain and resolve qualifying liquid; Then enter the compressed air of 0.2MP to the first tower in three towers, continue to resolve, fluid is to acidifying solution storage tank, and processing industry hydrochloric acid is mixed with the parsing for other adsorption towers after acidifying solution; Enter compressed air first tower is pressed dry to rear end parsing operation, proceed to step 5;
Step 5, Xiang Shouta injects clear water washing, and linear velocity is 2m/h, is greater than 4.0 and can stops until fluid uranium concentration is less than 1mg/L and pH value;
Step 6, the parsing qualifying liquid that step 4 is obtained carries out neutrality precipitation: add NaOH limit to stir toward resolving limit in qualifying liquid, pH value determination after stirring, until pH value is, stops adding NaOH and stirring at 7.0～8.0 o'clock, precipitates; Precipitate after 12 hours, discharge supernatant, then add the parsing qualifying liquid of same volume, repeat the neutral settling step in this step, until precipitation number of times reaches after 70 times, carry out plate compression operation and obtain product.
In described step 3, when feed liquor and fluid pH value reach consistent and≤stop circulation 1.3 time.
In described step 4, resolve operation and select the hydrochloric acid solution that parsing agent is 3.5g/L.
In described step 6, after qualifying liquid precipitation is complete, add 1.5 times of slurry volume clear water to carry out clear water precipitation, after drained supernatant, then enter plate compression operation acquisition product.
Progressive part of the present invention is to have simplified parsing technique, has reduced resolution flow ratio, has improved qualifying liquid uranium concentration, has removed the consumption of technique salt and carbonic hydroammonium; Resolve compared with technique with alkalescence, reduced production cost, alleviated employee's working strength, removed the discharge of ammonia, the more simple and environmental protection of operating process.
The specific embodiment
Below in conjunction with embodiment, the present invention is described further.
Device for carrying out said
The acid technique of resolving of a kind of D382 type resin, implement by means of following existing device:
A. adsorption tower: adsorption tower is diameter 2.5m iron flask, and height overall is 7.5m, and effective depth is 6m, liner PO, parts comprise: interface at the bottom of tower, DN200 flange, is liquid liquid outlet; Tower top interface, DN25, setting pressure table is used; Tower top interface, DN500 flange, is stoste inlet; Tower top interface, DN40, is connected with compressed air piping; Compressed air piping is DN50 iron pipe, and all the other connecting pipes are PPR tubing, size and flange size correspondence.
B. resolve agent storage tank: diameter 2.5m iron flask is highly 2m, liner PO, parts bag: tower top interface, DN40 flange, is connected with fresh water pipeline by DN40 iron pipe; Tower top exhaust outlet, 40cm*40cm; Interface at the bottom of tower, DN40 flange, resolves agent liquid outlet, is connected with parsing agent delivery pump by the PPR pipe of DN40.
C. acidifying solution storage tank: diameter 2.5m iron flask, high 4m, liner PO, parts comprise: tower top interface, DN40 flange, is connected with fresh water pipeline by DN40 iron pipe; Tower top interface, DN40 flange, connects hydrochloric acid pipeline by DN40PPR pipeline; Tower top exhaust outlet, DN50; Tower top interface, DN80 flange, acidifying circulating backwater, is connected by DN80PPR pipeline; Interface at the bottom of tower, DN80 flange, acidifying solution fluid use, connects DN80PPR pipeline.
D. former liquid pool: former liquid pool is long 25m, wide 20m, high 3.5m cement tub, parts comprise: stoste inlet, long 40cm, wide 40cm; Exhaust outlet, long 40cm, wide 40cm; Exhaust outlet, long 40cm, wide 40cm; Stoste liquid outlet, DN200 flange, by DN200 iron pipe with enter tower pump and dock.
E. mother liquor pond: the long 6m in mother liquor pond, wide 6m, high 2m metal trough, parts comprise: DN40 iron pipe, clap clear liquid in mother liquor pond and use.
F. stillpot: diameter 1.5m, high 3.3m iron flask, liner PO, parts comprise: tank deck interface, DN40 flange, is connected with qualifying liquid pipeline by DN40PPR pipeline; Tank deck interface, DN40 flange, is connected with fresh water pipeline by DN40PPR pipeline; Tank deck interface, DN40 flange, is connected with plate water return pipeline by DN40PPR pipeline; Tank deck mouth, long 40cm, wide 40cm, precipitation adds sheet alkali and uses; Interface at the bottom of tank, DN40 flange, the frame grout outlet that re-packs, is connected by DN40PPR pipeline.
Implementation step
Step 1, after D382 type resin adsorption is saturated, will be adsorbed in the impurity cleanings such as silt in resin particle gap through backwash operation, rear with the compressed air of 0.2MPa pressure by for subsequent use the drain in resin particle gap;
Step 2, certain uranium mine adopts 15m
3uranium concentration is less than in the qualifying liquid of 5g/L and adds 3m
3the ratio of technical hydrochloric acid is mixed with the consistent acidifying solution of adsorption tower volume, by acidifying solution delivery pump, 60% acidifying solution is delivered in adsorption tower resin is soaked; Qualifying liquid soaks the uranium-bearing liquid of saturated resin after resolving agent parsing in technology with referring to, and technical hydrochloric acid is that mass percent is the 31% HCl solution having, soak time 8 hours; ;
Step 3, circulates the acidifying solution in adsorption tower and outside adsorption tower, and endless form adopts lower feed liquor, the mode of upper fluid; Circulate and monitor circulation fluid pH after 6～8 hours, when feed liquor and fluid pH value reach consistent and≤preferably stop circulation 1.3 time; If pH value is below standard, add 0.5m
3technical hydrochloric acid, continues circulation, until feed liquor and fluid pH value reach consistent and≤1.3 o'clock;
Step 4, enters parsing operation after completing steps 3, resolve operation and select the hydrochloric acid solution that parsing agent is 3.5g/L, adopts three tower cascade connected parsing, and analysis mode adopts upper feed liquor, lower fluid, and in adsorption tower, the linear velocity of desorbed solution is 0.8～1.0m/h; When parsing when liquid flowing ratio reaches 2 left and right of recording of electronic flowmeter stops into parsing agent, obtain and resolve qualifying liquid; Then open air compressor machine, the first tower in Xiang Santa enters the compressed air of 0.2MP, continues to resolve, fluid is to acidifying solution storage tank, processing industry hydrochloric acid is mixed with the parsing for other adsorption towers after acidifying solution, enters compressed air and first tower is pressed dry to rear end resolves operation, proceeds to the rinsing process of step 5; In the present embodiment, when first tower press dry, first tower desorbed solution uranium concentration is less than 800mg/L, and the D382 type resin before parsing is saturated resin, after step 4 is resolved, becomes poor resin, and the remaining uranium capacity of the poor resin of first tower is less than 1g/L;
Step 5, Xiang Shouta injects clear water washing, and control flow is 10m
3/ h, is greater than 4.0 and can stops until fluid uranium concentration is less than 1mg/L and pH value, to reach the object that reclaims remaining uranium on resin and improve system pH in adsorption tower;
Step 6, the parsing qualifying liquid that step 4 is obtained carries out neutrality precipitation: parsing qualifying liquid pump is squeezed in stillpot, add while stirring sheet alkali, qualifying liquid stops feed liquor apart from 10cm left and right, stillpot top, stir and regulate pH value to 7.0～8.0 after 5 minutes, if pH is inadequate, adds appropriate sheet alkali and continue to stir, until pH is up to standard, stops stirring and precipitate; After 12 hours, arrange supernatant and go to mother liquor pond, and then add qualifying liquid and continue to repeat step above.In the time that reaching more than 70 times, precipitation number of times can carry out plate compression operation, reduce product impurity content, improve product grade, after qualifying liquid precipitation is complete, in stillpot, add approximately 1.5 times of slurry volume clear water to carry out clear water precipitation, the frame operation that can re-pack after drained supernatant obtains product.
Result of implementation: the present invention contrasts in table 1 and table 2 with parameter comparison and economic indicator that alkalescence is resolved qualifying liquid precipitation products obtained therefrom:
Table 1: two kinds of product parameters contrasts
Two kinds of process economics indexs of table 2
As can be seen from Table 1, have some superiority compared with alkalescence parsing qualifying liquid precipitation products obtained therefrom, product uranium grade can improve approximately 7%,, chloride ion content reduces approximately 1%.
As can be seen from Table 2, be reduced to a step and complete by this technique alkalescence is resolved-acid two step process that make the transition, resolution flow ratio is by being down to 2.0 left and right in 3 left and right, qualifying liquid uranium concentration is brought up to 12g/L left and right by 8g/L left and right, remove the consumption of technique salt and carbonic hydroammonium, produced uranium per ton and can reduce production costs approximately 1.4 ten thousand yuan compared with alkalescence parsing technique, alleviated employee's working strength simultaneously, remove the discharge of ammonia, the more simple and environmental protection of operating process.
Above embodiments of the invention are explained in detail, above-mentioned embodiment is only optimum embodiment of the present invention, but the present invention is not limited to above-described embodiment, in the ken possessing those of ordinary skills, can also under the prerequisite that does not depart from aim of the present invention, make various variations.
Claims (4)
1. the acid technique of resolving of D382 type resin, is characterized in that comprising following steps:
Step 1, after D382 type resin adsorption is saturated, will be adsorbed in the impurity cleanings such as silt in resin particle gap through backwash operation, rear with the compressed air of 0.2MPa pressure by for subsequent use the drain in resin particle gap;
Step 2, is mixed with acidifying solution by qualifying liquid, technical hydrochloric acid according to the ratio of volume ratio 14～16:3, after the volume of configuration acidifying solution must satisfied be full of the adsorption tower that comprises D382 type resin completely, also has the surplus of 1m3; Then 60% acidifying solution is wherein delivered in adsorption tower, to soaking through step 1 D382 type after treatment resin, soak time is 6～8 hours;
Step 3, by adsorption tower and outside adsorption tower acidifying solution circulate, endless form adopts lower feed liquor, the mode of upper fluid; Circulate and after 6～8 hours, monitor circulation fluid pH value, when feed liquor and fluid pH value reach consistent and≤stop circulation 1.5 time; If pH value is below standard, add 0.5m3 technical hydrochloric acid, continue circulation, until feed liquor and fluid pH value reach consistent and≤1.5 o'clock;
Step 4, enters parsing operation after completing steps 3, resolve operation and select the hydrochloric acid solution that parsing agent is 3～4g/L, adopts three tower cascade connected parsing, and analysis mode adopts upper feed liquor, lower fluid, and in adsorption tower, the linear velocity of desorbed solution is 0.8～1.0m/h; Stop into parsing agent when parsing when liquid flowing ratio reaches 2 left and right, obtain and resolve qualifying liquid; Then enter the compressed air of 0.2MP to the first tower in three towers, continue to resolve, fluid is to acidifying solution storage tank, and processing industry hydrochloric acid is mixed with the parsing for other adsorption towers after acidifying solution; Enter compressed air first tower is pressed dry to rear end parsing operation, proceed to step 5;
Step 5, Xiang Shouta injects clear water washing, and linear velocity is 2m/h, is greater than 4.0 and can stops until fluid uranium concentration is less than 1mg/L and pH value;
Step 6, the parsing qualifying liquid that step 4 is obtained carries out neutrality precipitation: add NaOH limit to stir toward resolving limit in qualifying liquid, pH value determination after stirring, until pH value is, stops adding NaOH and stirring at 7.0～8.0 o'clock, precipitates; Precipitate after 12 hours, discharge supernatant, then add the parsing qualifying liquid of same volume, repeat the neutral settling step in this step, until precipitation number of times reaches after 70 times, carry out plate compression operation and obtain product.
2. the acid technique of resolving of a kind of D382 type resin as claimed in claim 1, is characterized in that in step 3, when feed liquor and fluid pH value reach consistent and≤stop circulating 1.3 time.
3. the acid technique of resolving of a kind of D382 type resin as claimed in claim 1, is characterized in that in step 4, resolves operation and selects the hydrochloric acid solution that parsing agent is 3.5g/L.
4. a kind of D382 type resin acidity as claimed in claim 1 is resolved technique, it is characterized in that in step 6, after qualifying liquid precipitation is complete, first adds 1.5 times of slurry volume clear water to carry out clear water precipitation, after drained supernatant, then enters plate compression operation acquisition product.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210518105.7A CN103846081B (en) | 2012-12-06 | 2012-12-06 | A kind of D382 type resin acidic resolves technique |
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|---|---|---|---|
| CN201210518105.7A CN103846081B (en) | 2012-12-06 | 2012-12-06 | A kind of D382 type resin acidic resolves technique |
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| CN103846081A true CN103846081A (en) | 2014-06-11 |
| CN103846081B CN103846081B (en) | 2016-06-29 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106702184A (en) * | 2016-12-30 | 2017-05-24 | 新疆中核天山铀业有限公司 | Clear water desorption process of alkalescence anion resin |
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| US4242097A (en) * | 1979-03-05 | 1980-12-30 | Dionex Corporation | Method and apparatus for quantitative analysis of weakly ionized anions or cations |
| CN101195862A (en) * | 2007-12-20 | 2008-06-11 | 金川集团有限公司 | Method for purifying and cadmium removing from nickel and cobalt solution |
| CN101224436A (en) * | 2007-09-25 | 2008-07-23 | 张剑秋 | Ion exchange resin regeneration method |
| CN102219258A (en) * | 2010-04-14 | 2011-10-19 | 湖南荣宏钼业材料股份有限公司 | Method for extracting molybdenum from waste materials in ammonium molybdate production field |
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2012
- 2012-12-06 CN CN201210518105.7A patent/CN103846081B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4242097A (en) * | 1979-03-05 | 1980-12-30 | Dionex Corporation | Method and apparatus for quantitative analysis of weakly ionized anions or cations |
| CN101224436A (en) * | 2007-09-25 | 2008-07-23 | 张剑秋 | Ion exchange resin regeneration method |
| CN101195862A (en) * | 2007-12-20 | 2008-06-11 | 金川集团有限公司 | Method for purifying and cadmium removing from nickel and cobalt solution |
| CN102219258A (en) * | 2010-04-14 | 2011-10-19 | 湖南荣宏钼业材料股份有限公司 | Method for extracting molybdenum from waste materials in ammonium molybdate production field |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106702184A (en) * | 2016-12-30 | 2017-05-24 | 新疆中核天山铀业有限公司 | Clear water desorption process of alkalescence anion resin |
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