CN114672648B - Treatment method of N263 alkaline extraction raffinate - Google Patents
Treatment method of N263 alkaline extraction raffinate Download PDFInfo
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- CN114672648B CN114672648B CN202210221134.0A CN202210221134A CN114672648B CN 114672648 B CN114672648 B CN 114672648B CN 202210221134 A CN202210221134 A CN 202210221134A CN 114672648 B CN114672648 B CN 114672648B
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- 238000000605 extraction Methods 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 56
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- 238000000746 purification Methods 0.000 claims abstract description 31
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 16
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 15
- 239000010937 tungsten Substances 0.000 claims abstract description 15
- 238000003723 Smelting Methods 0.000 claims abstract description 9
- 239000007787 solid Substances 0.000 claims abstract description 7
- 239000012074 organic phase Substances 0.000 claims abstract description 5
- 239000002699 waste material Substances 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 12
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- 238000005352 clarification Methods 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000003350 kerosene Substances 0.000 claims description 4
- 238000004064 recycling Methods 0.000 claims description 4
- 239000002002 slurry Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- MGRWKWACZDFZJT-UHFFFAOYSA-N molybdenum tungsten Chemical compound [Mo].[W] MGRWKWACZDFZJT-UHFFFAOYSA-N 0.000 abstract description 8
- 239000000395 magnesium oxide Substances 0.000 abstract description 7
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 239000003513 alkali Substances 0.000 abstract 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 abstract 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 abstract 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 18
- 229910052750 molybdenum Inorganic materials 0.000 description 11
- 239000011733 molybdenum Substances 0.000 description 11
- 229910000029 sodium carbonate Inorganic materials 0.000 description 9
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 8
- 238000005070 sampling Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 239000010802 sludge Substances 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 230000004075 alteration Effects 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- QCJQWJKKTGJDCM-UHFFFAOYSA-N [P].[S] Chemical compound [P].[S] QCJQWJKKTGJDCM-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Abstract
The invention relates to the field of tungsten-molybdenum smelting, in particular to a treatment method of N263 alkaline extraction raffinate, which comprises the steps of pH value adjustment, extraction, purification conversion, reuse decomposition and the like. The method comprises the steps of firstly adjusting the pH value, adding solid NaOH into the N263 alkaline extraction raffinate, controlling the concentration of free alkali in the raffinate to be more than or equal to 5g/L, then carrying out 2-level countercurrent extraction by utilizing an N263 extractant, further reducing the concentration of WO 3 and Mo in the raffinate, reducing the metal quantity of circulating WO 3 and Mo, enabling an unsaturated loaded organic phase to enter the main process of N263 extraction, purifying and converting the raffinate by using magnesium oxide/sodium hydroxide, removing P in the raffinate, simultaneously converting HCO 3 in the raffinate into CO 3 2‑, and finally completing the efficient treatment of the N263 alkaline extraction raffinate by using the purified and converted raffinate to decompose tungsten smelting waste, thereby reducing the loss of WO 3 and Mo.
Description
[ Field of technology ]
The invention relates to the field of tungsten-molybdenum smelting, and relates to a treatment method of N263 alkaline extraction raffinate.
[ Background Art ]
Tungsten and molybdenum are rare metals and have wide application. At present, the tungsten-molybdenum productivity of China accounts for about 90% of the world. With the increase of high-quality tungsten-molybdenum ore resource consumption, the utilization of tungsten-molybdenum waste materials difficult to smelt is gradually paid attention to, wherein the tungsten-molybdenum waste materials are mainly represented by low-grade high-molybdenum high-phosphorus scheelite. In order to improve the utilization technology of low-grade high-molybdenum high-phosphorus scheelite, the professor of China and south university Zhao Zhongwei, the professor of Zhang Gui and the professor of Jiangxi university Mo Linsheng are subjected to deep technical development, the technology of sulfur-phosphorus mixed acid technology/sodium carbonate high-pressure decomposition-N263 alkaline extraction technology/phosphate decomposition technology and the like is invented, the extraction rate of tungsten and molybdenum is obviously improved, and the production cost is reduced. The sodium carbonate high-pressure decomposition-N263 alkaline extraction technology is used for treating the N263 extraction link of the low-grade high-molybdenum high-phosphorus scheelite, a large amount of raffinate is generated, the part of raffinate can gradually accumulate P and other impurity elements, meanwhile, the P and other impurity elements are directly removed, coprecipitation of tungsten and molybdenum can be caused, the recovery rate of tungsten and molybdenum is reduced, and the production operation is not facilitated.
Aiming at the problem of difficult treatment of the N263 alkaline extraction raffinate, the invention develops a treatment method of the N263 alkaline extraction raffinate, realizes recovery of WO 3 and Mo in the N263 alkaline extraction raffinate through the steps of pH value adjustment, extraction, purification conversion, reuse decomposition and the like, reduces the loss of tungsten and molybdenum in the purification conversion process, realizes closed cycle utilization of sodium carbonate in the raffinate, reduces the consumption of auxiliary materials, and obviously improves economic and environmental benefits.
[ Invention ]
The invention aims to overcome the defects of the prior art and provide a treatment method of N263 alkaline extraction raffinate, and the method can efficiently treat the N263 alkaline extraction raffinate, improve the recovery rate of tungsten and molybdenum, reduce the coprecipitation loss of tungsten and molybdenum in a purification conversion process, realize closed cycle utilization of sodium carbonate in the raffinate, reduce the consumption of auxiliary materials and improve economic and environmental benefits.
The invention discloses a treatment method of N263 alkaline extraction raffinate, which comprises the following steps:
(1) Adjusting the pH value: adding solid NaOH into the N263 alkaline extraction raffinate, stirring and dissolving, controlling the concentration of free NaOH to be more than 5g/L, and completing pH value adjustment, thus entering the next link.
(2) Extraction: the feed liquid obtained in the step (1) is subjected to 2-stage countercurrent extraction, an extraction system comprises about N26340%, about 30% of sulfonated kerosene, about 30% of octanol, the extraction ratio is V O/VA =1/2-1/3 compared with O/A=1/1, the extraction time is 10min, the clarification time is 5-10min, the extraction is completed, the unsaturated loaded organic phase enters the main process of N263 alkaline extraction, and the raffinate enters the next link.
(3) Purification conversion: adding MgO/NaOH into the raffinate to carry out purification conversion, wherein the adding amount of MgO is 20-80g/L, the adding amount of NaOH is 5-10g/L, the purification conversion time is 60-120min, the stirring speed is 60-120r/min, the purification conversion temperature is 80-95 ℃, the purification conversion is completed, and the next step is carried out.
(4) Recycling and decomposing: the raffinate after purification and conversion is used for decomposing tungsten smelting waste, the solid-liquid ratio of the prepared slurry is controlled to be 3/1-4/1, the concentration of Na 2CO3 is controlled to be 100-160g/L, the decomposition temperature is 180-200 ℃, the decomposition time is 120-180min, the stirring speed is 60-100r/min, the decomposition is completed, the filtering and washing are carried out, the filter residue is collected and treated, and the filtrate is returned to the main flow of extracting WO 3 and Mo.
Compared with the prior art, the invention has the following advantages:
The extraction of tungsten and molybdenum in the N263 alkaline extraction raffinate and the removal of impurity elements such as P are completed through pH value adjustment, extraction, purification conversion and reuse decomposition, and the conversion of HCO 3 - into CO 3 2- not only improves the recovery rate of valuable metals WO 3 and Mo, but also realizes the closed cycle utilization of sodium carbonate and reduces the consumption of auxiliary materials, thereby being a method for efficiently extracting the N263 alkaline extraction raffinate.
[ Description of the drawings ]
The invention is described in further detail below with reference to the attached drawing figures, wherein:
FIG. 1 is a process flow diagram of the present invention;
[ detailed description ] of the invention
The invention is further illustrated by means of fig. 1 and an example.
Example 1
In this example, the N263 alkaline extraction raffinate was obtained from a tungsten molybdenum smelter, and the sampling test results were WO 3 12.21.21 g/L, mo1.43g/L, P0.65g/L, and total C (sodium carbonate or sodium bicarbonate) 116.54g/L.
(1) Adjusting the pH value: adding solid NaOH into the N263 alkaline extraction raffinate, stirring and dissolving, wherein the concentration of free NaOH is 6.8g/L, and adjusting the pH value to finish the next link.
(2) Extraction: the feed liquid obtained in the step (1) is subjected to 2-stage countercurrent extraction, wherein an extraction system comprises N26340%, sulfonated kerosene volume 30%, octanol volume 30%, extraction ratio O/A=1/1, extraction flow ratio V O/VA =1/2, extraction time is 10min, clarification time is 10min, the concentration of WO 3 and Mo in the raffinate is 0.79g/L and 0.13g/L respectively, the unsaturated loaded organic phase enters an N263 alkaline extraction main process, and the raffinate enters the next link.
(3) Purification conversion: adding MgO/NaOH into the raffinate for purification and conversion, wherein the MgO addition amount is 20g/L, the NaOH addition amount is 8g/L, the purification and conversion time is 60min, the stirring speed is 60r/min, the purification and conversion temperature is 90 ℃, the purification and conversion is completed, sampling and detection are carried out, the concentrations of WO 3、Mo、Na2CO3, naOH and P are respectively 0.62g/L,0.11g/L,108.22g/L, 5.5g/L,0.02g/L, the P removal rate is 96.92%, and the purification and conversion is completed, thereby entering the next link.
(4) Recycling and decomposing: the raffinate after purification and conversion is used for decomposing tungsten smelting environment-friendly sludge (WO 3 6.51.51 percent and Mo2.36 percent), 500g of tungsten smelting environment-friendly sludge is weighed and placed in a 5000L volume autoclave, the liquid-solid ratio of the prepared slurry is controlled to be 3/1, the concentration of Na 2CO3 is controlled to be 108.22g/L, the decomposition temperature is 200 ℃, the decomposition time is 120min, the stirring speed is 60r/min, the decomposition is completed, filtering and washing are carried out, the filter residues are dried and collected, the weighing is 454.22g, the content of WO 3 and Mo in the sampling measurement is respectively 0.21 percent and 0.11 percent, the leaching rates of WO 3 and Mo are respectively 97.07 percent and 95.77 percent, and the filtrate returns to the main flow of extracting WO 3 and Mo.
Example 2
In this example, the N263 alkaline extraction raffinate was obtained from a tungsten molybdenum smelter, and the results of the sampling and detection were WO 3 6.33.33 g/L, mo1.08g/L, P0.35 and total C (sodium carbonate or sodium bicarbonate) 125.79g/L.
(1) Adjusting the pH value: adding solid NaOH into the N263 alkaline extraction raffinate, stirring and dissolving, wherein the concentration of free NaOH is 5.8g/L, and adjusting the pH value to finish the next link.
(2) Extraction: the feed liquid obtained in the step (1) is subjected to 2-stage countercurrent extraction, wherein an extraction system comprises N26340%, sulfonated kerosene volume 30%, octanol volume 30%, extraction ratio O/A=1/1, extraction flow ratio V O/VA =1/3, extraction time is 10min, clarification time is 10min, the concentration of WO 3 and Mo in the raffinate is 0.35g/L and 0.10g/L respectively, the unsaturated loaded organic phase enters an N263 alkaline extraction main process, and the raffinate enters the next link.
(3) Purification conversion: adding MgO/NaOH into the raffinate for purification and conversion, wherein the MgO addition amount is 20g/L, the NaOH addition amount is 6g/L, the purification and conversion time is 60min, the stirring speed is 60r/min, the purification and conversion temperature is 95 ℃, the purification and conversion is completed, sampling and detection are carried out, the concentrations of WO 3、Mo、Na2CO3, naOH and P are respectively 0.30g/L,0.08g/L, 116.54g/L, 5.0g/L and 0.011, the P removal rate is 96.86%, and the purification and conversion is completed, thereby entering the next link.
(4) Recycling and decomposing: the raffinate after purification and conversion is used for decomposing tungsten smelting environment-friendly sludge (WO 3 7.89.89 percent and Mo2.75 percent), namely 500g of tungsten smelting environment-friendly sludge is placed in a 5000L volume autoclave, the solid ratio of the prepared slurry liquid is controlled to be 4/1, the concentration of Na 2CO3 is controlled to be 116.54g/L, the decomposition temperature is 195 ℃, the decomposition time is 180min, the stirring speed is 60r/min, the decomposition is completed, the filtering and washing are carried out, the filter residues are dried and collected, the weighing is 441.32g, the content of WO 3 and Mo measured by sampling is 0.15 percent and 0.10 percent, the leaching rates of WO 3 and Mo are 98.32 percent and 96.79 percent respectively, and the filtrate is returned to the main flow of extracting WO 3 and Mo.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that various changes, modifications, substitutions and alterations can be made herein by those skilled in the art without departing from the technical principles of the present invention, and such changes, modifications, substitutions and alterations are also to be regarded as the scope of the invention.
Claims (1)
1. A method for processing N263 alkaline extraction raffinate is characterized in that: comprises the following steps:
(1) Adjusting the pH value: adding solid NaOH into the N263 alkaline extraction raffinate, stirring and dissolving, controlling the concentration of free NaOH to be more than 5g/L, and completing pH value adjustment, so as to enter the next link;
(2) Extraction: the feed liquid obtained in the step (1) is subjected to 2-stage countercurrent extraction, an extraction system comprises N263, sulfonated kerosene volume 30%, octanol volume 30%, an extraction ratio of O/A=1/1, an extraction flow ratio of V O/VA =1/2-1/3, an extraction time of 10min and a clarification time of 5-10min, the extraction is completed, an unsaturated loaded organic phase enters an N263 alkaline extraction main process, and raffinate enters the next link;
(3) Purification conversion: adding MgO/NaOH into the raffinate to carry out purification conversion, wherein the adding amount of MgO is 20-80g/L, the adding amount of NaOH is 5-10g/L, the purification conversion time is 60-120min, the stirring speed is 60-120r/min, the purification conversion temperature is 80-95 ℃, the purification conversion is completed, and the next step is carried out;
(4) Recycling and decomposing: the raffinate after purification and conversion is used for decomposing tungsten smelting waste, the solid-liquid ratio of the prepared slurry is controlled to be 3/1-4/1, the concentration of Na 2CO3 is controlled to be 100-160g/L, the decomposition temperature is 180-200 ℃, the decomposition time is 120-180min, the stirring speed is 60-100r/min, the decomposition is completed, the filtering and washing are carried out, the filter residue is collected and treated, and the filtrate is returned to the main flow of extracting WO 3 and Mo.
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| CN202210221134.0A CN114672648B (en) | 2022-03-07 | Treatment method of N263 alkaline extraction raffinate |
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| CN202210221134.0A CN114672648B (en) | 2022-03-07 | Treatment method of N263 alkaline extraction raffinate |
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| CN114672648B true CN114672648B (en) | 2024-06-11 |
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|---|---|---|---|---|
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