CN110714121B - Method for reducing consumption of organic phase in uranium molybdenum extraction process - Google Patents
Method for reducing consumption of organic phase in uranium molybdenum extraction process Download PDFInfo
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
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- C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
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Abstract
The invention belongs to the technical field of chemical metallurgy, and particularly relates to a method for reducing consumption of an organic phase in a uranium molybdenum extraction process. The invention comprises the following steps: step 1, researching the volatile property of an organic phase, and strictly controlling the extraction temperature of each link; step 2, selecting an organic phase with stable quality according to the property of the unit material; step 3, adding various standing oil separation facilities to prevent water phase entrainment; step 4, reducing the generation of triphase substances and recycling organic phases in the triphase substances; step 5, reasonably adjusting the air draft of equipment, and reducing the air draft of the organic phase; and 6, strictly operating, and reducing loss caused by organic phase overload. The invention can reduce the consumption of organic phase, improve the air quality of an extraction workshop, improve the quality of subsequent back extraction qualified liquid, and reduce the oil removal cost of raffinate water and other associated lock effects.
Description
Technical Field
The invention belongs to the technical field of chemical metallurgy, and particularly relates to a method for reducing consumption of an organic phase in a uranium molybdenum extraction process.
Background
In the ore hydrometallurgy process, metals in leaching filtrate are recovered by extraction and back extraction methods, wherein the more commonly used extraction organic phase (light phase) comprises sulfonated kerosene (light phase flowing carrier), TFA (extracting agent) and TBP (co-extracting agent), which are uniformly mixed in a certain proportion to form an organic phase; the organic phase plays an important role as a carrier and a transportation tool in the extraction and back extraction processes of uranium and molybdenum, but in the extraction process, the loss of the organic phase is large due to factors such as volatilization of the organic phase, quality problems, outflow of entrained aqueous phase, generation of three-phase substances, air draft of equipment, overload operation and the like, and the purchase cost of the organic phase is high, namely 1m3The prepared organic phase is 1 ten thousand yuan, so that a better extraction process control method is not provided, and the organic phase consumption is larger. The annual average unit consumption of 3.46Kg/T ore of a certain uranium molybdenum ore (the annual average unit consumption of 1.45Kg/T ore of the uranium molybdenum ore) in the prior organic phase has high production cost, and the volatile factors of the organic phase also have certain influence on the workshop environment, so that the development of a method for reducing the consumption of the organic phase in the extraction process is urgently needed.
Disclosure of Invention
The technical problems solved by the invention are as follows: the invention provides a method for reducing consumption of an organic phase in a uranium-molybdenum extraction process, which can reduce consumption of the organic phase, improve air quality of an extraction workshop, improve quality of subsequent back-extraction qualified liquid, reduce oil removal cost of raffinate water and other associated lock effects.
The technical scheme adopted by the invention is as follows:
a method for reducing consumption of an organic phase in a uranium molybdenum extraction process, comprising the steps of: step 1, researching the volatile property of an organic phase, and strictly controlling the extraction temperature of each link; step 2, selecting an organic phase with stable quality according to the property of the unit material; step 3, adding various standing oil separation facilities to prevent water phase entrainment; step 4, reducing the generation of triphase substances and recycling organic phases in the triphase substances; step 5, reasonably adjusting the air draft of equipment, and reducing the air draft of the organic phase; and 6, strictly operating, and reducing loss caused by organic phase overload.
In the step 1, the temperature of each extraction process is controlled within 25 +/-2 ℃.
The specific steps of the step 1 are as follows: the temperature of the extraction stock solution filtered by the rotary drum is 35-40 ℃, the temperature of the extraction stock solution is controlled to 25 +/-2 ℃ by 3 filtrate cooling towers, and then extraction is carried out; the uranium molybdenum water washing is heated to 20-25 ℃ by a heating device of an automatic interlocking temperature controller; the pickling solution is alternately used by two acidizing water configuration tanks, the configuration of each tank needs 1 hour, each tank can be cooled for 3 hours by a jacket water cooling mode, and the temperature of the acidizing water is reduced to about 25 ℃; the temperature of the molybdenum anti-reagent is not controlled, and the temperature of the uranium anti-reagent is controlled to be about 25 ℃ when the uranium anti-reagent is heated in the preparation process.
In step 2, the organic phase was detected for TFA and TBP.
The method comprises the following specific steps: and carrying out five-stage countercurrent extraction test with the extraction stock solution after configuration, and comparing the appearance, saturation capacity, flash point, compatibility, phase separation condition and water phase clarity after extraction with the original specimen, wherein the product is qualified if no larger difference exists.
The specific steps of the step 3 are as follows: the extracted water phase comprises uranium extraction residual water, pickling solution, washing solution and uranium molybdenum qualified solution, multi-stage oil separation is carried out on a large oil separation tank for a large water phase amount, then the water phase is discharged, and single-stage oil separation is carried out on other water phases with small amounts; the separated organic phase is periodically recovered and reused after being treated.
The specific steps of the step 4 comprise: adding an organic phase acidification regeneration process; the transformation of the organic phase can greatly reduce impurities and degradation products in the poor organic phase; increasing the standing time of the leaching filtrate; adding 1% hydrogen peroxide into the back extraction acid; optimizing and adjusting the operation methods of uranium molybdenum extraction, pickling and water washing and back extraction; and adding a plate-and-frame filter press to filter the formed three-phase substances.
The specific steps of the step 5 comprise: the extraction tank exhaust fans are installed to be variable-frequency, the proper opening degree of the air valve is adjusted, the air draft speed on the extraction tank body is reduced, and organic phase is prevented from being taken away due to air draft.
The specific steps of the step 6 are as follows: the reason and the phenomenon of overload are understood, and the loss caused by the overload of the organic phase is noticed.
The invention has the beneficial effects that:
the method for reducing the consumption of the organic phase in the uranium-molybdenum extraction process greatly reduces the consumption of organic phase and reduces the production cost; lays a foundation for optimizing the process operation; the problem of recovering the organic phase in the three-phase substance is solved; the ventilation technology is improved, so that the organic phase loss is reduced, and the air quality of a workshop is improved; the quality of the qualified uranium molybdenum liquid is improved, and the oil removal cost of raffinate water is reduced.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
The invention provides a method for reducing consumption of an organic phase in a uranium molybdenum extraction process, which comprises the following steps:
step 1, researching the volatile property of an organic phase and strictly controlling the extraction temperature of each link
The volatilization experiment of the organic phase is carried out at different temperatures, when the temperature is increased from 25 to 40 ℃, the volatilization amount of the organic phase is gradually increased (even multiplied), the organic phase volatilized into the air can not be recovered, and certain influence is also generated on the air quality. The organic phase was volatilized at different temperatures as shown in Table 1:
table 1: volatilization of organic phase at different temperatures
The method comprises the following specific steps of controlling the temperature of a certain uranium molybdenum ore to be 25 +/-2 ℃ in the extraction process: the temperature of the extraction stock solution filtered by the rotary drum is higher, usually at 35-40 ℃, the temperature of the extraction stock solution is controlled to 25 +/-2 ℃ by 3 filtrate cooling towers for extraction; the uranium molybdenum water washing is heated to 20-25 ℃ by a heating device of an automatic interlocking temperature controller; the pickling solution is alternately used by two acidizing water configuration tanks, the configuration of each tank needs 1 hour, each tank can be cooled for 3 hours by a jacket water cooling mode, and the temperature of the acidizing water is reduced to about 25 ℃; the temperature of the molybdenum anti-agent (ammonia water) is not controlled, and the temperature of the uranium anti-agent is controlled to be about 25 ℃ when the uranium anti-agent is heated in the preparation process.
Step 2, use of organic phase of stable quality
And (3) detecting the quality of TFA and TBP entering a certain uranium molybdenum ore organic phase mainly. Before unloading, a sample needs to be taken and sent to an analysis center to be used as a raw material inspection experiment, and the main process is as follows: after the preparation, the prepared sample and the extraction stock solution are subjected to a five-stage countercurrent extraction test, compared with the original specimen, the sample has the advantages of appearance, saturation capacity, flash point, compatibility, phase separation condition, clarity of the extracted water phase and the like, and if the sample does not have a large difference, the sample can be unloaded after being qualified, so that the sample is suitable for production and application.
Step 3, adding various standing oil separation facilities to prevent water phase entrainment
Two 10-grade old extraction tanks (each 70 m) are utilized by a certain uranium molybdenum ore extraction plant for uranium extraction raffinate water (with large flow)3And in each 2 stages, small openings are opened at the bottoms of the inter-stage plates and are combined into 1 large stage for overflow oil separation), oil separation is carried out in parallel, oil separation is carried out on other water phases with smaller flow by utilizing a certain single stage of the waste extraction tank, and when the main collecting process is abnormal in operation, the abnormal water phases carry oil. The effect is obvious, and the organic phase recovered by various oil separation facilities in each month is about 10m3Left and right.
Step 4, reducing the generation of triphase substances and recovering organic phases in the triphase substances
A certain uranium molybdenum ore is respectively used as depleted uranium molybdenum for acidizing regeneration by utilizing waste original molybdenum-saturated pickling tanks (two pickling tanks), and impurities in the depleted organic phase are greatly reduced by carrying out organic phase transformation, so that the organic phase is clear and transparent, and the generation of three-phase substances is reduced; by standing the leaching filtrate for more than 15 hours, partial impurities such as Ca, si and the like can be effectively separated out along with the clarification of the filtrate and the reduction of the temperature; the turbidity of the molybdenum extraction stock solution is reduced to be less than 50ppm through the standing process of the clarification tank and the vacuum drum filtration, and 480-550mv of stable potential can be applied to the hydrogen peroxide automatic replenishing system; 1% hydrogen peroxide is added in the back extraction acid saturation, so that the generation of three-phase substances in the back extraction process can be effectively reduced; the stable comparison of the operation methods (the first choice is to adjust the split phase clarity) of uranium and molybdenum extraction, pickling and water washing and back extraction is optimized and adjusted, and the discovery is that: the uranium and molybdenum washing and uranium back extraction are continuous and better in water phase, and are more stable than the uranium and molybdenum washing and uranium back extraction which are stable in an O/A (O represents an organic phase) of 0.5-0.8:1 (A represents an aqueous phase), and the uranium and molybdenum extraction and molybdic acid washing and back extraction are continuous better in organic phase, and are more stable than the uranium and molybdenum washing and uranium back extraction which are stable in an O/A (O/A) of 1-1.5: 1;
in order to process three-phase substances in the qualified molybdenum liquid and improve the quality of the qualified molybdenum liquid, 1 small plate-and-frame filter press is additionally arranged for filtering, and compared with a centrifuge for filtering, the effect is remarkable. After the technology is used, the quality of the qualified molybdenum liquid is greatly improved, and the organic phase in the three-phase substance can be recycled.
Step 5, reasonably adjusting the air draft of the equipment, and reducing the organic phase caused by air draft
Certain uranium molybdenum ore extraction workshop increases the replacement of outside air to factory building inside through reforming workshop exhaust system, simultaneously with each extraction tank air exhauster installation frequency conversion, adjusts the suitable aperture of blast gate, reduces the convulsions wind speed on the extraction cell body, prevents promptly that the organic phase is taken away by wind-force, improves workshop air quality again greatly.
Step 6, strict operation is carried out, and loss caused by organic phase overload is reduced
The best extraction capacity (saturation capacity) of an organic phase in a molybdenum system of a uranium molybdenum ore extraction plant is 9-12g/l of molybdenum, and the best extraction capacity of the organic phase in uranium extraction is 3-4g/l of uranium. Controlling the extract stock solution to the organic phase flow according to the requirement can greatly reduce the generation of viscous oil droplets (mainly TFA), the loss of the organic phase is small, and the extraction efficiency is stable.
After a certain uranium molybdenum ore is modified by the technical method: firstly, the unit consumption of organic phase is obviously reduced,the average unit consumption in 17 years is 1.45Kg/T ore, which is reduced by 2.3 times compared with the previous unit consumption of 3.46Kg/T ore. The organic phase is reduced to 502.5 tons (about 605.4 m) in 17 years by the conversion of annual ore handling capacity of 25 ten thousand tons3) And the production cost is saved by 605.4 ten thousand yuan. Secondly, the problem of three-phase substance treatment is solved. The interlocking effect is good: the quality of qualified liquid supplied to downstream workshops is improved, and the first-grade yield of molybdenum products is increased to over 95 percent from 70 percent in the past; the oil removing cost of the raffinate water is reduced, and the like.
Claims (5)
1. A method for reducing consumption of an organic phase in a uranium molybdenum extraction process is characterized in that: the method comprises the following steps: step (1), researching the volatile property of an organic phase, and strictly controlling the extraction temperature of each link: controlling the temperature of each extraction procedure within 25 +/-2 ℃; and (2) selecting an organic phase with stable quality according to the unit material property: detecting TFA and TBP of an organic phase, and specifically comprising the following steps: after the preparation, carrying out a five-stage countercurrent extraction test with the extraction stock solution, comparing the appearance, saturation capacity, flash point, compatibility, phase-splitting condition and clarity of the extracted water phase with the original specimen, and if the difference is not large, determining that the specimen is qualified; adding various standing oil separation facilities to prevent water phase entrainment; and (4) reducing the generation of triphase substances and recovering organic phases in the triphase substances: adding an organic phase acidification regeneration process; the transformation of the organic phase can greatly reduce impurities and degradation products in the poor organic phase; increasing the standing time of the leaching filtrate; adding 1% hydrogen peroxide into the back extraction acid; optimizing and adjusting the operation methods of uranium molybdenum extraction, pickling and water washing and back extraction; adding a plate-and-frame filter press to filter the formed three-phase substances; step (5), reasonably adjusting the air draft of equipment, and reducing the organic phase from being taken away by the air draft; and (6) strictly operating, and reducing loss caused by organic phase overload.
2. A method of reducing the consumption of the organic phase in a uranium molybdenum extraction process according to claim 1, characterised in that: the specific steps of the step (1) are as follows: the temperature of the extraction stock solution filtered by the rotary drum is 35-40 ℃, the temperature of the extraction stock solution is controlled to 25 +/-2 ℃ by 3 filtrate cooling towers, and then extraction is carried out; the uranium molybdenum water washing is heated to 20-25 ℃ by a heating device of an automatic interlocking temperature controller; the pickling solution is alternately used by two acidizing water configuration tanks, the configuration of each tank needs 1 hour, each tank can be cooled for 3 hours by a jacket water cooling mode, and the temperature of the acidizing water is reduced to about 25 ℃; the temperature of the molybdenum anti-reagent is not controlled, and the temperature of the uranium anti-reagent is controlled to be about 25 ℃ when the uranium anti-reagent is heated in the preparation process.
3. A method of reducing the consumption of the organic phase in a uranium molybdenum extraction process according to claim 1, characterised in that: the specific steps of the step (3) are as follows: the extracted water phase comprises uranium extraction residual water, pickling solution, washing solution and uranium molybdenum qualified solution, multi-stage oil separation is carried out on a large oil separation tank for a large water phase amount, then the water phase is discharged, and single-stage oil separation is carried out on other water phases with small amounts; the separated organic phase is periodically recovered and reused after being treated.
4. A method of reducing the consumption of the organic phase in a uranium molybdenum extraction process according to claim 1, characterised in that: the specific steps of the step (5) comprise: the extraction tank exhaust fans are installed to be variable-frequency, the proper opening degree of the air valve is adjusted, the air draft speed on the extraction tank body is reduced, and organic phase is prevented from being taken away due to air draft.
5. A method of reducing the consumption of the organic phase in a uranium molybdenum extraction process according to claim 1, characterised in that: the specific steps of the step (6) are as follows: the reason and the phenomenon of overload are understood, and the loss caused by the overload of the organic phase is noticed.
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| CN114369731B (en) * | 2021-12-17 | 2023-10-20 | 中核沽源铀业有限责任公司 | Method for reducing molybdenum back extraction three-phase matters |
| CN114350945B (en) * | 2021-12-31 | 2024-02-09 | 中核沽源铀业有限责任公司 | Separation and recovery method for three-phase matters of wet smelting molybdenum back extraction of uranium molybdenum ore |
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