CN114350945B - Separation and recovery method for three-phase matters of wet smelting molybdenum back extraction of uranium molybdenum ore - Google Patents
Separation and recovery method for three-phase matters of wet smelting molybdenum back extraction of uranium molybdenum ore Download PDFInfo
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- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 148
- 239000011733 molybdenum Substances 0.000 title claims abstract description 148
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 140
- 238000000605 extraction Methods 0.000 title claims abstract description 74
- 238000000034 method Methods 0.000 title claims abstract description 57
- KTEXACXVPZFITO-UHFFFAOYSA-N molybdenum uranium Chemical compound [Mo].[U] KTEXACXVPZFITO-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000000926 separation method Methods 0.000 title claims abstract description 32
- 238000003723 Smelting Methods 0.000 title claims abstract description 21
- 238000011084 recovery Methods 0.000 title claims abstract description 11
- 239000012071 phase Substances 0.000 claims abstract description 136
- 239000007788 liquid Substances 0.000 claims abstract description 102
- 239000012074 organic phase Substances 0.000 claims abstract description 65
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000002386 leaching Methods 0.000 claims abstract description 34
- 239000012065 filter cake Substances 0.000 claims abstract description 31
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000005406 washing Methods 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 230000032798 delamination Effects 0.000 claims abstract description 16
- 239000000047 product Substances 0.000 claims abstract description 16
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 11
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 11
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 11
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 11
- 238000000746 purification Methods 0.000 claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 25
- 229910052770 Uranium Inorganic materials 0.000 claims description 20
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 claims description 20
- 239000012535 impurity Substances 0.000 claims description 15
- 239000002244 precipitate Substances 0.000 claims description 15
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 11
- 239000002893 slag Substances 0.000 claims description 11
- -1 molybdenum metals Chemical class 0.000 claims description 10
- 238000003916 acid precipitation Methods 0.000 claims description 5
- 159000000003 magnesium salts Chemical class 0.000 claims description 4
- 238000010907 mechanical stirring Methods 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 3
- 238000003828 vacuum filtration Methods 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 21
- 239000013049 sediment Substances 0.000 abstract description 3
- 239000007790 solid phase Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 description 14
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 10
- 239000002253 acid Substances 0.000 description 10
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 9
- 229910052785 arsenic Inorganic materials 0.000 description 9
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 229910052698 phosphorus Inorganic materials 0.000 description 9
- 239000011574 phosphorus Substances 0.000 description 9
- 229910052710 silicon Inorganic materials 0.000 description 9
- 239000010703 silicon Substances 0.000 description 9
- 238000000967 suction filtration Methods 0.000 description 9
- 239000008346 aqueous phase Substances 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 5
- 235000019341 magnesium sulphate Nutrition 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000009825 accumulation Methods 0.000 description 4
- 239000000084 colloidal system Substances 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 235000010755 mineral Nutrition 0.000 description 4
- 239000011707 mineral Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- MXZRMHIULZDAKC-UHFFFAOYSA-L ammonium magnesium phosphate Chemical compound [NH4+].[Mg+2].[O-]P([O-])([O-])=O MXZRMHIULZDAKC-UHFFFAOYSA-L 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- MIIQUCFATSFCBP-UHFFFAOYSA-L azanium;magnesium;trioxido(oxo)-$l^{5}-arsane Chemical compound [NH4+].[Mg+2].[O-][As]([O-])([O-])=O MIIQUCFATSFCBP-UHFFFAOYSA-L 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000391 magnesium silicate Substances 0.000 description 3
- 229910052919 magnesium silicate Inorganic materials 0.000 description 3
- 235000019792 magnesium silicate Nutrition 0.000 description 3
- ZADYMNAVLSWLEQ-UHFFFAOYSA-N magnesium;oxygen(2-);silicon(4+) Chemical compound [O-2].[O-2].[O-2].[Mg+2].[Si+4] ZADYMNAVLSWLEQ-UHFFFAOYSA-N 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 229910052567 struvite Inorganic materials 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- 108010057081 Merozoite Surface Protein 1 Proteins 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000012080 ambient air Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- XMYHHSMIUHHPEW-UHFFFAOYSA-N azane;molybdenum Chemical compound N.[Mo] XMYHHSMIUHHPEW-UHFFFAOYSA-N 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 239000012629 purifying agent Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention belongs to the technical field of uranium molybdenum ore wet smelting, and relates to a separation and recovery method of a three-phase object of molybdenum back extraction in uranium molybdenum ore wet smelting, which comprises the following steps: placing the molybdenum back-extraction qualified liquid discharged from the water phase outlet of the molybdenum back-extraction mixing clarifier into a buffer tank to obtain molybdenum qualified liquid containing three-phase matters; performing preliminary solid-liquid separation, and washing the filtered three-phase filter cake with clear water; uniformly mixing the washed three-phase filter cake with uranium-molybdenum ore leaching pulp, leaching by a sulfuric acid method, and carrying out subsequent extraction back extraction and other processes on the leaching liquid; the solution containing organic phase and water phase, which is subjected to solid-liquid separation and washing and is removed of sediment, is conveyed into a clarifier for standing and layering; mixing the organic phase subjected to standing delamination with the lean organic phase subjected to molybdenum back extraction, and carrying out a subsequent extraction process; and (3) conveying the water-phase molybdenum qualified liquid subjected to standing and layering to a purification process to prepare an ammonium molybdate product. The invention effectively damages the structure of the three-phase matters, so that the organic phase, the water phase and the solid phase are fully separated and recovered.
Description
Technical Field
The invention belongs to the technical field of uranium molybdenum ore wet smelting, and particularly relates to a method for separating and recycling three-phase matters generated by ammonia water molybdenum back extraction in a primary uranium molybdenum ore acid leaching and amine extraction process flow.
Background
Molybdenum is a traditional dominant mineral resource in China, along with the development of economy in China, the application field of molybdenum is continuously expanded, the molybdenum industry is rapidly developed, the requirements of various industries on molybdenum and molybdenum products are continuously increased, and molybdenum is used as a strategic mineral resource, and the irreproducibility of the molybdenum is determined by incapability of purely relying on unconditional exploitation of natural ore to extract molybdenum, so that the smelting technology is required to be improved, and the comprehensive recycling of the molybdenum resource is increased. The molybdenum resources in China are mostly common and associated molybdenum ores, the beneficiation pressure is high, according to statistics, molybdenum is used as a single mineral deposit, the reserves of the molybdenum only account for 14% of the total reserves of molybdenum in China, so that the molybdenum resources of high grade which are gradually reduced are made up, the molybdenum resources lean and hybridization trend is adapted, and the research on the molybdenum extraction technology of low grade complex molybdenum ores and molybdenum secondary resources is more and more. Uranium molybdenum co-associated ore belongs to one of complex molybdenum ores, and the traditional physical or chemical ore dressing technology is difficult to realize the enrichment of useful minerals, concentrate cannot be prepared, and the direct wet smelting of raw ore tends to leach various impurity elements into a system, so that the difficulty of impurity removal, concentration and enrichment is increased in the process of preparing products. The invention provides a three-phase object separation and recovery method aiming at the three-phase object generated in a molybdenum back extraction link in the wet smelting comprehensive recovery process of uranium molybdenum co-associated crude ore.
Leaching uranium and molybdenum from uranium-molybdenum raw ore by sulfuric acid method, leaching uranium, molybdenum and some impurity elements into solution, carrying out uranium and molybdenum step-by-step extraction by using organic phase prepared from sulfonated kerosene, tri-aliphatic amine and tributyl phosphate, carrying out acid washing on molybdenum-loaded organic phase by using acidified water to remove uranium, carrying out back extraction on the molybdenum-loaded organic phase after acid washing by using ammonia water to obtain molybdenum qualified liquid, adding magnesium sulfate into the molybdenum qualified liquid under certain technological conditions to remove arsenic, phosphorus and silicon impurities in a precipitation form, removing organic matters and decolorization in the molybdenum qualified liquid by using active carbon adsorption, and finally adding concentrated sulfuric acid for precipitation to obtain ammonium molybdate product. The process leaching solution contains impurity ions such as arsenic, phosphorus, silicon, iron and the like, the impurity ions enter a molybdenum-loaded organic phase in the extraction process, part of uranium can be extracted at the same time, although 99% of uranium is removed in the pickling process, a small amount of uranium enters the back extraction process along with the molybdenum-loaded organic phase, precipitates of uranium, arsenic, phosphorus, silicon and iron are generated under the alkaline condition in the ammonia molybdenum back extraction operation process, the solid precipitates adsorb and entrain the organic phase and the water phase, finally, sticky three-phase matters are formed and mixed with molybdenum qualified liquid to enter a purifying and impurity removing process, the three-phase matters occupy larger volume, have more stable structure and sticky properties, have the density close to that of the molybdenum qualified liquid, and increase the difficulty of separation and recovery. Leading to a series of process problems: 1. absorbing and entraining the organic phase by the three-phase matters, so as to cause the loss of the organic phase; 2. the impurities of the three-phase matters enter a magnesium salt impurity removal and activated carbon adsorption process along with the qualified molybdenum liquid, and the impurity removal efficiency is reduced due to the existence of the three-phase matters, so that the consumption of the activated carbon is increased; 3. if a part of three-phase matters or organic phase after purification enters an acid precipitation process along with qualified liquid, the risk of influencing the quality of ammonium molybdate products exists.
The prior art for separating and recycling the three-phase matters of the molybdenum back extraction in uranium molybdenum ore wet smelting has the defects of poor performance and common treatmentThe method comprises the following steps: chemical method, standing for clarifying, and ultrasonic wave. Breaking three-phase material by chemical method, adding NaF and Na into the three-phase material 2 CO 3 Salts such as NaCl and the like can introduce other ions into a production system to influence the product quality and the operation of a main process; the ultrasonic wave has high energy consumption for breaking three-phase matters, the three-phase matters contain colloid substances, and the demulsification effect is poor; by adopting a standing clarification method, the qualified liquid density of the three-phase material is close to that of molybdenum, the layering effect of the sticky three-phase material is poor, and the three-phase material cannot be effectively separated and recovered.
Disclosure of Invention
Aiming at the problems that organic phase loss, uranium and molybdenum metal loss and high consumption of a purifying agent are caused by three-phase matters generated by acid wet-process molybdenum back extraction of the native uranium-molybdenum ore, and the product quality risk is potentially influenced, the invention provides a separation and recovery method for the three-phase matters in the wet-process molybdenum back extraction of the uranium-molybdenum ore, which belongs to a physical separation method, effectively damages the structure of the three-phase matters, fully separates and recovers the organic phase, the water phase and the solid phase, reasonably and effectively controls the addition of powdery active carbon when molybdenum qualified liquid is purified and decontaminated, increases the purification efficiency, remarkably improves the quality of ammonium molybdate products produced by an acid precipitation process, reduces the loss of organic phases of a system, really solves the problems of resource waste, high impurity ion introduction, energy efficiency consumption and poor effect in the prior wet-process uranium-molybdenum ore wet-process smelting industry development, and realizes the development concept of production operation quality improvement, synergy and cost reduction.
The technical scheme for realizing the purpose of the invention comprises the following steps:
the separation and recovery method of the three-phase matters of the wet smelting molybdenum back extraction of the native uranium molybdenum ore comprises the following steps:
step 1, putting molybdenum back-extraction qualified liquid discharged from a water phase outlet of a molybdenum back-extraction mixer-settler into a buffer tank to obtain molybdenum qualified liquid containing three-phase matters;
step 2, conveying the qualified molybdenum liquid containing the three-phase matters to perform primary solid-liquid separation, washing a filtered three-phase matter filter cake by a certain amount of clear water, and further replacing an organic phase and the qualified molybdenum liquid in the three-phase matter filter cake;
step 3, uniformly mixing the washed three-phase filter cake with uranium-molybdenum ore leaching pulp, leaching by a sulfuric acid method, dissolving uranium and molybdenum metals adsorbed and precipitated in the three-phase slag into leaching liquid, further recovering uranium and molybdenum metals adsorbed and precipitated in the three-phase slag, and carrying out subsequent extraction back extraction and other processes on the leaching liquid;
step 4, conveying a solution containing an organic phase and a water phase, which are subjected to solid-liquid separation and washing to remove precipitates, into a clarifier for standing and layering, wherein the upper layer is the organic phase, and the lower layer is a water phase molybdenum qualified liquid, so that oil-water separation is realized;
step 5, mixing the organic phase subjected to standing delamination with the lean organic phase subjected to molybdenum back extraction, and carrying out a subsequent extraction process to further reasonably utilize the recovered organic phase;
and 6, conveying the water-phase molybdenum qualified liquid subjected to standing delamination to a purification process for removing impurities of magnesium salts and adsorbing by activated carbon, and then carrying out acid precipitation to prepare an ammonium molybdate product.
In the step 1, the content of three-phase matters in the obtained molybdenum back-extraction qualified liquid, namely the dry weight of three-phase matters and the volume ratio of the molybdenum qualified liquid are 1.5-20g/L, and the temperature is 20-40 ℃.
In the step 2, the solid-liquid separation mode adopts negative pressure vacuum filtration or positive pressure diaphragm filter pressing.
The volume mass ratio of the washing clear water amount to the dry weight of the three-phase slag in the step 2 is 0.5-5:1, and the temperature of the washing water is 20-40 ℃.
And in the step 3, the mass ratio of the dry weight of the three-phase slag to the dry weight of uranium-molybdenum ore leaching ore pulp is 0.02-0.25%.
The mixing mode in the step 3 is mechanical stirring, and the mixing time is 0.5-2h.
In the step 4, the standing delamination time is 0.5-5 h.
In the step 5, the mixing ratio of the organic phase subjected to standing delamination and the lean organic phase subjected to molybdenum back extraction is 0-1:1.
in the step 6, the oil content in the water phase molybdenum qualified liquid subjected to standing layering is below 30 mg/L.
The beneficial technical effects of the invention are as follows:
1. the method adopts a physical technology, does not add any chemical reagent, does not introduce other ions into a production system, and avoids the influence of other ions on the quality of ammonium molybdate products and the production process.
2. The method adopts a solid-liquid separation mode of negative pressure suction filtration or positive pressure diaphragm filter pressing, a filter cake is formed on the surface of filter media such as filter paper or filter cloth in the filtration process of the three-phase substances, most of organic phases adsorbed and entrained in the three-phase substances are separated from solid precipitates and colloid substances under the action of the vacuum negative pressure or the positive pressure, and molybdenum qualified liquid in the filtration liquid can also replace part of organic phases adsorbed and entrained in the three-phase substances, so that the organic phases are separated from the solid precipitates.
3. The method adopts clear water to wash a three-phase filter cake formed after solid-liquid separation, the clear water disc washing can replace organic phases and molybdenum qualified liquid remained in the three-phase filter cake formed on the surfaces of filter media such as filter paper or filter cloth, the organic phases and molybdenum metal in the three-phase filter cake are further separated, and more than 80% of the organic phases adsorbed and entrained in the three-phase filter cake can be separated from solid precipitates through solid-liquid separation and water cleaning.
4. According to the method, colloid substances, precipitates and the like in the three-phase substances can be trapped in a filter cake through solid-liquid separation, the quality of an organic phase recovered through standing layering can meet the process requirement, the organic phase is mixed with a lean organic phase of molybdenum back extraction and then returned to a molybdenum extraction process for use, and the volume of the recovered organic phase can reach 2% -15% of the volume of the molybdenum qualified liquid according to the difference of the three-phase substances in the molybdenum back extraction qualified liquid; the oil content in the water phase molybdenum qualified liquid recovered by standing and layering can reach below 30mg/L, thereby avoiding the adverse effect of three-phase matters on magnesium salt impurity removal and active carbon adsorption procedures, improving impurity removal, deoiling and decoloring efficiency, reducing the consumption of magnesium sulfate and active carbon, and the consumption of the used powdered active carbon is 20kg/m 3 The product quality of the acid precipitation ammonium molybdate is improved, and the product chemical grade MSA-1 accounts for more than 95 percent.
5. According to the method, the three-phase filter cake after solid-liquid separation and clear water washing is returned to the front end of the main process flow to be mixed and stirred with raw ore pulp, the uranium and molybdenum useful metals adsorbed and precipitated in the three-phase filter cake are reacted into solution through an acid leaching process, and the uranium and molybdenum metals in the recovered three-phase filter cake can reach more than 90%.
Drawings
Fig. 1 is a flow chart of a separation and recovery method for a three-phase object of uranium molybdenum ore wet smelting molybdenum back extraction.
Detailed Description
The invention is described in further detail below with reference to the drawings and examples.
Example 1
And step 1, placing the molybdenum back-extraction qualified liquid discharged from the water phase outlet of the molybdenum back-extraction mixer-settler into a buffer tank to obtain molybdenum qualified liquid containing three-phase matters, wherein the content of the three-phase matters (the dry weight of three-phase matters and the volume ratio of the molybdenum qualified liquid) in the molybdenum back-extraction qualified liquid is 5g/L, and the temperature is 25 ℃.
Step 2, connecting and preparing a Buchner funnel, a suction bottle and a vacuum suction filter of an experimental device, paving qualitative filter paper on the Buchner funnel, wetting with clear water, starting the suction filter, taking 2L of molybdenum qualified liquid with three-phase matters obtained by back extraction, adding the molybdenum qualified liquid into the Buchner funnel, carrying out negative pressure suction filtration of-650 mmHg, wherein the suction filtration time is about 40min, the surface of a three-phase matter filter cake has no obvious liquid accumulation, adding 50ml of clear water at 25 ℃ after the suction filtration of the filtrate is finished, continuing to carry out suction filtration until the surface of the three-phase matter filter cake has no obvious liquid accumulation, and at the moment, 89% of organic phase adsorbed and entrained in the three-phase matters can enter the suction bottle at the lower part of the Buchner funnel along with the molybdenum qualified liquid and washing water.
And 3, mixing the washed three-phase filter cake with uranium-molybdenum ore leaching ore pulp for 1h through mechanical stirring, wherein the ratio of the dry weight of the three-phase material slag to the dry ore of the uranium-molybdenum ore pulp is 0.05%, adding concentrated sulfuric acid for acid leaching, enabling 95% of uranium and molybdenum metals adsorbed and precipitated in the three-phase material slag to react with the sulfuric acid and dissolve into leaching liquid, and carrying out subsequent extraction back extraction and other processes on the leaching liquid.
And 4, transferring the solution containing the organic phase and the aqueous phase, which is subjected to solid-liquid separation and washing and is subjected to sediment removal, into a clarifier for standing and layering, wherein a separating funnel can be used for replacing the clarifier, the upper layer is the organic phase, the lower layer is the aqueous phase molybdenum qualified liquid, and the layering time is 30min, so that the molybdenum qualified liquid and the organic phase can be well layered.
And 5, mixing the organic phase subjected to standing delamination and the lean organic phase subjected to molybdenum back extraction at a ratio of 0.2:1, and performing a molybdenum extraction process, wherein all extraction indexes and operation conditions are normal, and the quality of the organic phase recovered by standing delamination can meet the process requirements.
Step 6, analyzing and detecting oil content in the water-phase molybdenum qualified liquid subjected to standing and layering to be 10mg/L, performing a purification process, adding 1.2 times of excessive magnesium sulfate by theoretical calculation according to analysis and detection data of arsenic, phosphorus and silicon in the molybdenum qualified liquid, removing the arsenic, the phosphorus and the silicon from the solution in the form of precipitates such as magnesium ammonium arsenate, magnesium ammonium phosphate and magnesium silicate, and then adding 15kg/m of the precipitate 3 Adding powdered activated carbon (weight of powdered activated carbon/volume of molybdenum qualified liquid), deoiling, decolorizing, and adsorbing, and adding concentrated sulfuric acid to reach solution temperature of 55-65deg.C and pH of 2.0 to obtain ammonium molybdate product.
Example 2
Step 1, placing molybdenum back-extraction qualified liquid discharged from an aqueous phase outlet of a molybdenum back-extraction mixer-settler into a container such as a beaker to obtain molybdenum qualified liquid containing three-phase matters, wherein the content of the three-phase matters (the dry weight of three-phase matters and the volume ratio of the molybdenum qualified liquid) in the molybdenum back-extraction qualified liquid is 8g/L, and the temperature is 30 ℃;
step 2, connecting and preparing a Buchner funnel, a suction bottle and a vacuum suction filter of an experimental device, paving qualitative filter paper on the Buchner funnel, wetting with clear water, starting the suction filter, taking 4L of molybdenum qualified liquid with three-phase matters obtained by back extraction, adding the molybdenum qualified liquid into the Buchner funnel, carrying out negative pressure suction filtration of-650 mmHg, wherein the suction filtration time is about 2 hours, the surface of a three-phase matter filter cake has no obvious liquid accumulation, adding 50ml of clear water at 35 ℃ after the suction filtration of the filtrate is finished, continuing to carry out suction filtration until the surface of the three-phase matter filter cake has no obvious liquid accumulation, and at the moment, 86% of organic phase adsorbed and entrained in the three-phase matters can enter the suction bottle at the lower part of the Buchner funnel along with the molybdenum qualified liquid and washing water.
And 3, mixing the washed three-phase filter cake with uranium-molybdenum ore leaching ore pulp for 1.5 hours through mechanical stirring, wherein the ratio of the dry weight of the three-phase material slag to the dry ore of the uranium-molybdenum ore pulp is 0.1%, adding concentrated sulfuric acid to perform acid leaching, enabling 93% of uranium and molybdenum metals adsorbed and precipitated in the three-phase material slag to react with the sulfuric acid and dissolve into leaching liquid, and performing subsequent extraction and back extraction on the leaching liquid.
And 4, transferring the solution containing the organic phase and the aqueous phase, which is subjected to solid-liquid separation and washing and is subjected to sediment removal, into a clarifier for standing and layering, wherein a separating funnel can be used for replacing the clarifier, the upper layer is the organic phase, the lower layer is the aqueous phase molybdenum qualified liquid, and the layering time is 40min, so that the molybdenum qualified liquid and the organic phase can be well layered.
And 5, mixing the organic phase subjected to standing delamination and the lean organic phase subjected to molybdenum back extraction at a ratio of 0.5:1, and performing a molybdenum extraction process, wherein all extraction indexes and operation conditions are normal, and the quality of the organic phase recovered by standing delamination can meet the process requirements.
Step 6, analyzing and detecting oil content in the water-phase molybdenum qualified liquid subjected to standing and layering to be 12mg/L, performing a purification process, adding 1.2 times of excessive magnesium sulfate by theoretical calculation according to analysis and detection data of arsenic, phosphorus and silicon in the molybdenum qualified liquid, removing the arsenic, the phosphorus and the silicon from the solution in the form of precipitates such as magnesium ammonium arsenate, magnesium ammonium phosphate and magnesium silicate, and then adding 15kg/m of the precipitate 3 Adding powdered activated carbon (weight of powdered activated carbon/volume of molybdenum qualified liquid), deoiling, decolorizing, and adsorbing, and adding concentrated sulfuric acid to reach solution temperature of 55-65deg.C and pH of 2.0 to obtain ammonium molybdate product.
Example 3
Step 1, placing molybdenum back-extraction qualified liquid discharged from an aqueous phase outlet of a molybdenum back-extraction mixer-settler into a buffer tank to obtain molybdenum qualified liquid containing three-phase matters, wherein the content of the three-phase matters (the dry weight of three-phase matters and the volume ratio of the molybdenum qualified liquid) in the molybdenum back-extraction qualified liquid is 15g/L, and the temperature is 35 ℃; the method is beneficial to the solid-liquid separation filtration speed along with the increase of the temperature, but the ammonia in the molybdenum qualified liquid with overhigh temperature volatilizes more strongly, which affects the quality of the ambient air, is unfavorable for occupational health, increases the ventilation difficulty, and the molybdenum back-extraction qualified liquid containing three-phase matters in the buffer tank can be directly subjected to solid-liquid separation without temperature regulation.
And 2, conveying the qualified molybdenum solution containing the three-phase matters into a Jing Jin XAYG20/809-U type box-type membrane filter press through a pump to perform solid-liquid separation, wherein the filtering pressure is 0.5-0.55MPa, stopping feeding after the three-phase matters are saturated in a cavity of the filter press, feeding clean water from a central hole of the filter press through the pump to wash a three-phase matters filter cake, wherein the volume mass ratio of the washing water quantity to the dry weight of the three-phase matters is 2:1, and the washing water temperature is 35 ℃, at the moment, 82% of adsorbed and entrained organic phases in the three-phase matters can enter a buffer tank along with the qualified molybdenum solution and washing water, and the box-type membrane filter press has a squeezing function and further separates the residual organic phases and solution in the three-phase matters from the filter cake through mutual extrusion of membrane plates and matching plates in the cavity of the filter press.
And 3, unloading the washed three-phase filter cake, mechanically stirring and mixing the three-phase filter cake with uranium-molybdenum ore leaching ore pulp for 2 hours, wherein the ratio of the dry weight of the three-phase filter cake to the dry ore of the uranium-molybdenum ore pulp is 0.2%, adding concentrated sulfuric acid for acid leaching, wherein the sulfuric acid leaching is a conventional hydrogen peroxide oxidation acid leaching or acid oxygen pressure leaching process, and reacting uranium and molybdenum metals adsorbed and precipitated in the three-phase filter cake into a solution through the leaching process to further recover uranium and molybdenum metals. 91% of uranium and molybdenum metals adsorbed and precipitated in the three-phase slag can react with sulfuric acid to be dissolved into leaching solution, and the leaching solution is subjected to subsequent extraction back extraction and other processes.
And 4, continuously conveying a solution containing an organic phase and a water phase, which are subjected to solid-liquid separation and washing to remove precipitates, into a clarifier for standing, wherein the clarifier is provided with a light phase overflow weir at the upper part and a heavy phase weir at the lower part, the organic phase is gradually separated from the water phase along with the time extension, the upper layer is an organic phase, the lower layer is a water phase molybdenum qualified solution, the clarifier is provided with a light phase overflow weir at the upper part and a heavy phase weir at the lower part, the standing layering time is 2h, and the analysis and detection oil content of the water phase molybdenum qualified solution is 15mg/L.
And 5, mixing the organic phase subjected to standing delamination with the lean organic phase subjected to molybdenum back extraction at a ratio of 1:1, intercepting colloid substances, precipitates and the like in the three-phase substances in a filter cake through solid-liquid separation, conveying the filter cake to a molybdenum extraction process, ensuring that all extraction indexes and operation conditions are normal, and returning the quality of the organic phase subjected to standing delamination recovery after mixing with the lean organic phase subjected to molybdenum back extraction to the molybdenum extraction for use.
Step 6, the molybdenum qualified liquid discharged from the heavy phase weir pipeline is conveyed to a purification process through standing layering of a clarifier, and is led inAnalysis and detection data of arsenic, phosphorus and silicon in molybdenum-passing qualified liquid, adding 1.4 times of excessive magnesium sulfate by theoretical calculation, removing arsenic, phosphorus and silicon from the solution in the form of precipitate of magnesium ammonium arsenate, magnesium ammonium phosphate, magnesium silicate and the like, and then adding 20kg/m of solution 3 Adding powdered activated carbon (weight of powdered activated carbon/volume of molybdenum qualified liquid), deoiling, decolorizing, adsorbing, removing organic matters and decolorizing, and adding concentrated sulfuric acid to reach 55-65deg.C and pH of 2.0 to obtain ammonium molybdate product.
The present invention has been described in detail with reference to the drawings and the embodiments, but the present invention is not limited to the embodiments described above, and various changes can be made within the knowledge of those skilled in the art without departing from the spirit of the present invention. The invention may be practiced otherwise than as specifically described.
Claims (9)
1. The separation and recovery method for the three-phase matters of the wet smelting molybdenum back extraction of the native uranium molybdenum ore is characterized by comprising the following steps:
step 1, putting molybdenum back-extraction qualified liquid discharged from a water phase outlet of a molybdenum back-extraction mixer-settler into a buffer tank to obtain molybdenum qualified liquid containing three-phase matters;
step 2, conveying the qualified molybdenum liquid containing the three-phase matters to perform primary solid-liquid separation, washing a filtered three-phase matter filter cake by a certain amount of clear water, and further replacing an organic phase and the qualified molybdenum liquid in the three-phase matter filter cake;
step 3, uniformly mixing the washed three-phase filter cake with uranium-molybdenum ore leaching pulp, leaching by a sulfuric acid method, dissolving uranium and molybdenum metals adsorbed and precipitated in the three-phase slag into leaching liquid, further recovering uranium and molybdenum metals adsorbed and precipitated in the three-phase slag, and carrying out a subsequent extraction back extraction process on the leaching liquid;
step 4, conveying a solution containing an organic phase and a water phase, which are subjected to solid-liquid separation and washing to remove precipitates, into a clarifier for standing and layering, wherein the upper layer is the organic phase, and the lower layer is a water phase molybdenum qualified liquid, so that oil-water separation is realized;
step 5, mixing the organic phase subjected to standing delamination with the lean organic phase subjected to molybdenum back extraction, and carrying out a subsequent extraction process to further reasonably utilize the recovered organic phase;
and 6, conveying the water-phase molybdenum qualified liquid subjected to standing delamination to a purification process for removing impurities of magnesium salts and adsorbing by activated carbon, and then carrying out acid precipitation to prepare an ammonium molybdate product.
2. The method for separating and recovering three-phase matters from the molybdenum strip by wet smelting of the native uranium molybdenum ore according to claim 1, wherein in the step 1, the content of the three-phase matters in the qualified molybdenum strip liquid, namely the dry weight of three-phase matters and the volume ratio of the qualified molybdenum liquid, is 1.5-20g/L, and the temperature is 20-40 ℃.
3. The method for separating and recovering the three-phase matters of the wet smelting molybdenum back extraction of the native uranium molybdenum ore according to claim 1, wherein in the step 2, a solid-liquid separation mode adopts negative pressure vacuum filtration or positive pressure diaphragm filter pressing.
4. The method for separating and recovering the three-phase matters from the wet smelting molybdenum of the native uranium molybdenum ore according to claim 1, wherein the volume mass ratio of the washing water amount to the dry weight of the three-phase matters in the step 2 is 0.5-5ml to 1g, and the temperature of the washing water is 20-40 ℃.
5. The method for separating and recovering the three-phase matters of the wet smelting molybdenum back extraction of the native uranium molybdenum ore according to claim 1, wherein the mass ratio of the dry weight of the three-phase matters to the dry weight of the uranium molybdenum ore leaching pulp obtained in the step 3 is 0.02-0.25%.
6. The method for separating and recovering the three-phase matters of the wet smelting molybdenum from the native uranium molybdenum ore according to claim 1, wherein the mixing mode in the step 3 is mechanical stirring, and the mixing time is 0.5-2h.
7. The method for separating and recovering the three-phase matters of the wet smelting molybdenum back extraction of the native uranium molybdenum ore according to claim 1, wherein in the step 4, the standing delamination time is 0.5-5 h.
8. The method for separating and recovering three phases of molybdenum stripping in wet smelting of uranium molybdenum ore as defined in claim 1, wherein in the step 5, the mixing ratio of the organic phase separated by standing and delamination to the lean organic phase of molybdenum stripping is 0-1:1.
9. the method for separating and recovering the three-phase matters of the wet smelting molybdenum back extraction of the native uranium molybdenum ore according to claim 1, wherein in the step 6, oil content in the qualified aqueous molybdenum liquid subjected to standing delamination is below 30 mg/L.
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