CN115092999B - Flocculation treatment method of uranium purification waste liquid - Google Patents
Flocculation treatment method of uranium purification waste liquid Download PDFInfo
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- CN115092999B CN115092999B CN202210704914.0A CN202210704914A CN115092999B CN 115092999 B CN115092999 B CN 115092999B CN 202210704914 A CN202210704914 A CN 202210704914A CN 115092999 B CN115092999 B CN 115092999B
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- 239000007788 liquid Substances 0.000 title claims abstract description 99
- 239000002699 waste material Substances 0.000 title claims abstract description 91
- 229910052770 Uranium Inorganic materials 0.000 title claims abstract description 75
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 238000000746 purification Methods 0.000 title claims abstract description 48
- 238000005189 flocculation Methods 0.000 title claims abstract description 41
- 230000016615 flocculation Effects 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 239000007787 solid Substances 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims description 11
- 239000006228 supernatant Substances 0.000 claims description 11
- 229920002401 polyacrylamide Polymers 0.000 claims description 10
- 229920000642 polymer Polymers 0.000 claims description 8
- 125000002091 cationic group Chemical group 0.000 claims description 7
- 238000003860 storage Methods 0.000 claims description 7
- 230000002378 acidificating effect Effects 0.000 claims description 6
- 239000008394 flocculating agent Substances 0.000 claims description 6
- 238000012546 transfer Methods 0.000 claims description 5
- 238000005352 clarification Methods 0.000 claims description 4
- 239000002689 soil Substances 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 230000005587 bubbling Effects 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000005191 phase separation Methods 0.000 claims description 3
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 150000001768 cations Chemical class 0.000 claims description 2
- 230000014759 maintenance of location Effects 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract description 4
- 230000000903 blocking effect Effects 0.000 abstract description 4
- 229910017604 nitric acid Inorganic materials 0.000 abstract description 4
- 239000012074 organic phase Substances 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000004880 explosion Methods 0.000 abstract description 2
- 238000012423 maintenance Methods 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 description 11
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- 238000000605 extraction Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000036961 partial effect Effects 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 2
- 229910002007 uranyl nitrate Inorganic materials 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000011038 discontinuous diafiltration by volume reduction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- -1 suspended matters Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Abstract
The invention relates to the technical field of waste liquid treatment, and particularly discloses a flocculation treatment method of uranium purification waste liquid, which comprises the following steps: step 1: preparing a flocculant; step 2: mixing the waste liquid and the flocculant for the first time; step 3: mixing the waste liquid and the flocculant again; step 4: and (5) flocculation separation. According to the invention, the waste liquid is treated by the flocculant, so that on one hand, solid particles and suspended matters in the uranium purification waste liquid are effectively removed, scaling and even blocking of a reboiler in a rear nitric acid recovery process are avoided, the maintenance cost is reduced, and the continuous stability of the operation of a production line is improved; on the other hand, part of organic phase entrained in uranium purification waste liquid is removed, the risk of explosion of red oil of a reboiler is reduced, and beneficial guarantee is provided for safe operation of a production line.
Description
Technical Field
The invention belongs to the technical field of waste liquid treatment, and particularly relates to a flocculation treatment method of uranium purification waste liquid.
Background
The raffinate produced by the uranium purification process is acidic uranium-containing waste liquid, the concentration of H + is about 1.5mol/L, the concentration of uranium is less than 100mg/L, and the uranium-containing waste liquid contains Fe, cr, ni, mo, ca and other various metal impurities, and also comprises ore particles or impurities which are insoluble in nitric acid and suspended matters formed by mud carried in slag in the waste liquid. Wherein the main components of the mud component which is symbiotic with the ore are SiO 2 and silicate, and the waste liquid forms colloid after being dispersed.
In the existing uranium purification process, the volume reduction treatment of acidic uranium-containing waste liquid and the recycling and multiplexing of nitric acid are realized by adopting a decompression rectification technology. However, because the composition of the uranium purification waste liquid is complex, the scale formation and even the blockage of a reboiler tube array are easy to cause, and the waste liquid treatment capacity of the uranium purification production line is seriously affected. Aiming at a heterogeneous system of uranium purification waste liquid, an effective and feasible treatment method is not available.
It is therefore desirable to devise a flocculation treatment method for uranium purification waste liquid to solve the above problems.
Disclosure of Invention
The invention aims to provide a flocculation treatment method of uranium purification waste liquid, which is used for realizing pretreatment of acidic uranium-containing waste liquid at the front end of a vacuum rectification process.
The technical scheme of the invention is as follows:
A flocculation treatment method of uranium purification waste liquid comprises the following steps:
Step 1: preparing flocculant
Adding deionized water into a flocculant preparation tank, weighing polymer flocculant solids, and adding the polymer flocculant solids into the flocculant preparation tank to prepare a flocculant;
Step 2: primary mixing waste liquid and flocculant
Temporary storage is carried out on acid uranium-containing waste liquid generated by a uranium purification production line in a waste liquid receiving tank, the waste liquid is conveyed to a mixer by a shielding pump A, a flocculating agent is conveyed to the mixer by a metering pump, and primary mixing is realized in the mixer;
step 3: mixing the waste liquid and the flocculant again
The waste liquid after primary mixing and the flocculating agent enter a three-stage pipeline mixer for further mixing, so that uniform mixing is ensured, and flocculate is prevented from being crushed again;
step 4: flocculation separation
The flocculate and the clear liquid are clarified and split in a clarifier, so that a clear interface is formed between the flocculate and the clear liquid.
The polymer flocculant solid in the step 1 is cationic polyacrylamide, polyvinyl alcohol, sodium polyacrylate or polyaluminium chloride.
The mass concentration of the flocculant prepared in the step 1 is 0.3-0.8%.
In the step 1, 10m 3/h of compressed air is introduced into the flocculant preparation tank to realize bubbling stirring so as to be fully and uniformly mixed.
In step 2, the ratio of the flocculant to the waste liquid stream mixed at one time is 1 (1-60).
In the step 3, the time of the liquid passing through the three-stage pipeline mixer is controlled within 0.5-6 s.
In the step 4, the retention time of the liquid in the clarifier is 50-300 s when the phase separation is clarified.
In step 4, the volume content of polyacrylamide (cation type) in the supernatant after clarification is less than 0.01%, the content of suspended matters is less than 20mg/L, and the COD content is less than 300mg/L.
In the step 4, the supernatant flows to the waste liquid middle tank from the overflow port, and is subsequently sent to the rectification system through the shielding pump B for the rectification process.
In step 4, the flocs are discharged from the bottom of the clarifier to a soil storage tank and then pumped to temporary storage by a soil transfer pump.
The invention has the remarkable effects that:
according to the invention, the waste liquid is treated by the flocculant, so that on one hand, solid particles and suspended matters in the uranium purification waste liquid are effectively removed, scaling and even blocking of a reboiler in a rear nitric acid recovery process are avoided, the maintenance cost is reduced, and the continuous stability of the operation of a production line is improved; on the other hand, part of organic phase entrained in uranium purification waste liquid is removed, the risk of explosion of red oil of a reboiler is reduced, and beneficial guarantee is provided for safe operation of a production line. Specifically:
(1) The invention flocculates the raffinate (acid waste liquid) generated in the extraction process, avoids the flocculant from contacting tributyl phosphate caused by adding the flocculant into uranyl nitrate extract stock solution, has adverse effects on the extraction mass transfer process and clarification phase separation, and avoids the competitive extraction of uranyl nitrate by high molecular amide flocculant and tributyl phosphate;
(2) According to the invention, before the rectification treatment of the uranium purification waste liquid, the separation of solid particles, suspended matters, organic phases and metal impurities is realized, and the rectification treatment difficulty of the uranium purification waste liquid is reduced from a source item;
(3) According to the invention, the cationic polyacrylamide is used for replacing hydrogenated kerosene to realize oil removal of uranium purification waste liquid, so that the waste organic phase production amount in the uranium purification process is reduced.
The flocculation treatment method has certain capability of removing oil and partial metal impurities, and effectively avoids the risk of blocking a reboiler in the uranium purification waste liquid rectification process.
In addition, the flocculation treatment method has simple process and low medicament cost, and the method has feasibility and reliability through the flocculation treatment verification of uranium purification waste liquid.
Drawings
FIG. 1 is a schematic flow chart of a processing method.
In the figure: 1a waste liquid receiving tank; 2 shielding the pump A;3, a flocculating agent preparation groove; 4, a metering pump; 5 a mixer; 6 three-stage pipeline mixer; 7 a clarifier; 8 a waste liquid middle tank; 9 shielding the pump B;10 a dirt storage tank; 11 dirt transfer pump.
Detailed Description
The invention will be described in further detail with reference to the accompanying drawings and specific examples.
As shown in fig. 1, a flocculation treatment method of uranium purification waste liquid includes the following steps:
Step 1: preparing flocculant
Adding deionized water into a flocculant preparation tank 3, weighing polymer flocculant solids such as cationic polyacrylamide, polyvinyl alcohol, sodium polyacrylate, polyaluminium chloride and the like, adding the polymer flocculant solids into the flocculant preparation tank 3, and preparing flocculant with the mass concentration of 0.3-0.8%; introducing 10m 3/h compressed air into the flocculant preparation tank 3 to realize bubbling stirring so as to fully and uniformly mix;
No mechanical stirring is used in the flocculant preparation tank 3, so that flocculant degradation caused by shearing can be effectively avoided; the flocculant should be used within 24 hours after being prepared;
Step 2: primary mixing waste liquid and flocculant
The acidic uranium-containing waste liquid generated by the uranium purification production line is temporarily stored in a waste liquid receiving tank 1, is conveyed to a mixer 5 by a shielding pump A2, and is conveyed to the mixer 5 by a metering pump 4, and the two are mixed in the mixer 5 at one time according to a constant flow ratio, wherein the flow ratio is controlled to be 1:1-60 of the waste liquid;
the flocculant is not conveyed by a centrifugal pump, so that the degradation of the flocculant caused by centrifugal shearing of an impeller can be effectively avoided;
step 3: mixing the waste liquid and the flocculant again
The waste liquid after primary mixing and the flocculating agent enter a three-stage pipeline mixer 6 for further mixing, the time of the liquid passing through the three-stage pipeline mixer 6 is controlled within 0.5-6 s, so that uniform mixing is ensured, and flocculate is prevented from being crushed again;
step 4: flocculation separation
Clarifying and phase-separating the flocculate and the clear liquid in a clarifier 7, wherein the residence time of the liquid in the clarifier 7 is 50-300 s so as to ensure that a clear interface is formed between the flocculate and the clear liquid; the positive ion content of polyacrylamide in the supernatant after clarification is less than 0.01 percent by volume, the content of suspended matters is less than 20mg/L, and the COD content is less than 300mg/L;
The supernatant flows to the waste liquid middle tank 8 from the overflow port, and is subsequently sent to a rectification system through the shielding pump B9 for a rectification process; the flocs are discharged from the bottom of clarifier 7 to a dirt storage tank 10 and then sent to temporary storage by a dirt transfer pump 11.
Example 1
The uranium purification waste liquid is treated by the flocculation method, and the acidity, uranium concentration, impurity content, turbidity, suspended matter content and COD content of the uranium purification waste liquid and the flocculated supernatant are analyzed, and the comparison results are shown in Table 1.
Table 1 comparison of flocculation treatment data for uranium purified waste
| Project | Unit (B) | Uranium purification waste liquid | Supernatant after flocculation |
| Acidity of | mol/L | 1.43 | 1.43 |
| Uranium concentration | mg/L | 86 | 85 |
| [Fe] | μg/L | 432 | 411 |
| [Cr] | μg/L | 136 | 128 |
| [Ni] | μg/L | 34 | 29 |
| [Mo] | μg/L | 7.3 | 6.6 |
| [Ca] | μg/L | 6.2 | 3.5 |
| [Si] | μg/L | 2130 | 138 |
| Turbidity degree | NTU | 216 | 12 |
| Suspension of | mg/L | 260 | 8 |
| COD | mg/L | 631 | 255 |
As can be seen from the data in table 1, after the uranium purification waste liquid is subjected to flocculation treatment by cationic polyacrylamide, the acidity and uranium concentration of the uranium purification waste liquid are basically unchanged, and the content of metal impurities Fe, cr, ni, mo, ca is slightly reduced but not obvious; the nonmetallic Si content, turbidity, suspended matter content and COD content are obviously reduced, a good flocculation separation effect is obtained, and the subsequent rectification treatment requirement of uranium purification waste liquid is met.
Example 2
The uranium purification waste liquid was treated by the flocculation method, and the acidity, uranium concentration, impurity content, turbidity, suspended matter content and COD content of the uranium purification waste liquid and the flocculated supernatant were analyzed, and the comparison results are shown in Table 2.
Table 2 comparison of flocculation treatment data for uranium purified waste
As can be seen from the data in table 2, after the uranium purification waste liquid is subjected to flocculation treatment by the cationic polyacrylamide, the acidity and the uranium concentration of the uranium purification waste liquid are basically unchanged, and the content of metal impurities Fe, cr, ni, mo, ca is slightly reduced but not obvious; the nonmetallic Si content, turbidity, suspended matter content and COD content are obviously reduced, a good flocculation separation effect is obtained, and the subsequent rectification treatment requirement of uranium purification waste liquid is met.
Example 3
The uranium purification waste liquid was treated by the flocculation method, and the acidity, uranium concentration, impurity content, turbidity, suspended matter content and COD content of the uranium purification waste liquid and the flocculated supernatant were analyzed, and the comparison results are shown in Table 3.
Table 3 comparison of flocculation treatment data for uranium purified waste
| Project | Unit (B) | Uranium purification waste liquid | Supernatant after flocculation |
| Acidity of | mol/L | 1.56 | 1.56 |
| Uranium concentration | mg/L | 135 | 135 |
| [Fe] | μg/L | 564 | 498 |
| [Cr] | μg/L | 165 | 146 |
| [Ni] | μg/L | 56 | 49 |
| [Mo] | μg/L | 11.2 | 10.6 |
| [Ca] | μg/L | 9.8 | 6.3 |
| [Si] | μg/L | 2698 | 321 |
| Turbidity degree | NTU | 301 | 21 |
| Suspension of | mg/L | 465 | 15 |
| COD | mg/L | 769 | 234 |
As can be seen from the data in table 3, the acidity and uranium concentration of the uranium purification waste liquid are basically unchanged after the uranium purification waste liquid is subjected to cationic polyacrylamide flocculation treatment, and the content of metal impurities Fe, cr, ni, mo, ca is slightly reduced but not obvious; the nonmetallic Si content, turbidity, suspended matter content and COD content are obviously reduced, a good flocculation separation effect is obtained, and the subsequent rectification treatment requirement of uranium purification waste liquid is met.
By implementing the method, flocculation treatment of the uranium purification waste liquid is completed, and separation of suspended matters in the uranium purification waste liquid is realized. The flocculation treatment method has certain oil removal and partial metal impurity removal capacity, and effectively avoids the risk of blocking a reboiler in the uranium purification waste liquid rectification process. The flocculation treatment method is simple in process and low in medicament cost, and the flocculation treatment method of the verified uranium purification waste liquid is feasible and reliable.
Claims (8)
1. A flocculation treatment method of uranium purification waste liquid is characterized by comprising the following steps: the method comprises the following steps:
Step 1: preparing flocculant
Adding deionized water into the flocculant preparation tank (3), weighing polymer flocculant solids, and adding the polymer flocculant solids into the flocculant preparation tank (3) to prepare a flocculant;
Step 2: primary mixing waste liquid and flocculant
The acidic uranium-containing waste liquid generated by the uranium purification production line is temporarily stored in a waste liquid receiving tank (1), is conveyed to a mixer (5) by a shielding pump A (2), and is conveyed to the mixer (5) by a metering pump (4), and the acidic uranium-containing waste liquid and the flocculating agent are mixed in the mixer (5) for one time;
step 3: mixing the waste liquid and the flocculant again
The waste liquid after primary mixing and the flocculating agent enter a three-stage pipeline mixer (6) for further mixing, so that uniform mixing is ensured, and flocculate is prevented from being crushed again;
step 4: flocculation separation
Clarifying and phase-separating the flocculate and the clear liquid in a clarifier (7) to form a clear interface between the flocculate and the clear liquid;
The polymer flocculant solid in the step 1 is cationic polyacrylamide, polyvinyl alcohol, sodium polyacrylate or polyaluminium chloride;
the mass concentration of the flocculant prepared in the step 1 is 0.3-0.8%.
2. A flocculation treatment method of uranium purified waste liquid as claimed in claim 1, wherein: in the step 1, 10m 3/h of compressed air is introduced into the flocculant preparation tank (3) to realize bubbling stirring so as to be fully and uniformly mixed.
3. A flocculation treatment method of uranium purified waste liquid as claimed in claim 1, wherein: in step 2, the ratio of the flocculant to the waste liquid stream mixed at one time is 1 (1-60).
4. A flocculation treatment method of uranium purified waste liquid as claimed in claim 1, wherein: in the step 3, the time of the liquid passing through the three-stage pipeline mixer (6) is controlled within 0.5-6 s.
5. A flocculation treatment method of uranium purified waste liquid as claimed in claim 1, wherein: in the step 4, the retention time of the liquid in the clarifier (7) is 50-300 s during clarifying phase separation.
6. A flocculation treatment method of uranium purified waste liquid as claimed in claim 1, wherein: in step 4, the volume content of polyacrylamide (cation type) in the supernatant after clarification is less than 0.01%, the content of suspended matters is less than 20mg/L, and the COD content is less than 300mg/L.
7. A flocculation treatment method of uranium purified waste liquid as claimed in claim 1, wherein: in the step 4, the supernatant flows to a waste liquid middle tank (8) from an overflow port, and is subsequently sent to a rectification system through a shielding pump B (9) for a rectification process.
8. A flocculation treatment method of uranium purified waste liquid as claimed in claim 1, wherein: in step 4, the flocs are discharged from the bottom of the clarifier (7) to a soil reservoir (10) and then sent to temporary storage by a soil transfer pump (11).
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| CN202210704914.0A CN115092999B (en) | 2022-06-21 | Flocculation treatment method of uranium purification waste liquid |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210704914.0A CN115092999B (en) | 2022-06-21 | Flocculation treatment method of uranium purification waste liquid |
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| CN115092999A CN115092999A (en) | 2022-09-23 |
| CN115092999B true CN115092999B (en) | 2024-06-11 |
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|---|---|---|---|---|
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| US4569768A (en) * | 1983-10-07 | 1986-02-11 | The Dow Chemical Company | Flocculation of suspended solids from aqueous media |
| CN107098496A (en) * | 2017-04-05 | 2017-08-29 | 浙江工业大学 | Preprocess method and its device that PU chemical leather DMF waste liquor rectifications are reclaimed |
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