CN101700898B - Recovery method of inorganic salt in technology of molybdenum oxide or molybdenum waste alkali leaching-extraction preparing ammonium molybdate - Google Patents
Recovery method of inorganic salt in technology of molybdenum oxide or molybdenum waste alkali leaching-extraction preparing ammonium molybdate Download PDFInfo
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Abstract
The invention discloses a recovery method of inorganic salt in a technology of molybdenum oxide or molybdenum waste alkali leaching-extraction preparing ammonium molybdate. An extraction liquid obtained after extraction is evaporated and crystallized in the low temperature and negative pressure, and parameters thereof are as follows: temperature is 28-70 DEG C, the pressure is minus 0.02- minuse 0.05Mpa, and the stirring speed is 20-60rpm; by mass, the evaporation is continuously carried out till the solid content in the extraction liquid is 20-60%, and then solid-liquid separation is carried out on the extraction liquid, thus obtaining the inorganic salt by separating. The method is suitable for various molybdenum ores or molybdenum waste processing procedures containing alkali leaching and extraction-back exaction operations. The method can realize the 100% recovery of the inorganic salt; and the purity of the obtained salt is larger than 99%; and the separated liquid phase can recycled, thus realizing the zero discharge of sewage.
Description
Technical field
The invention belongs to molybdenum oxide or molybdenum waste alkali leaching-extraction preparing ammonium molybdate Technology field, particularly the recovery method of inorganic salt in a kind of molybdenum oxide or the molybdenum waste alkali leaching-extraction preparing ammonium molybdate technology.
Background technology
Existing molybdenum oxide or molybdenum waste alkali leaching-extraction preparing ammonium molybdate technology is as shown in Figure 1: at first molybdenum oxide or molybdenum waste material are carried out ore grinding, breeze behind the ore grinding back of sizing mixing adds yellow soda ash and sodium hydroxide and carries out alkali and soak the molybdenum that makes wherein and enter in the solution with the form of molybdate, solid-liquid separation obtains alkali immersion liquid (sodium molybdate solution) and tailings afterwards, then alkali immersion liquid (sodium molybdate solution) is added mineral acid and adjust the pH value, use again through extracting with the organic phase after a kind of mineral acid acidifying (the secondary octanol+kerosene of phase N235+ is arranged), make molybdate in the sodium molybdate solution enter organic phase and become load organic phases, strip with ammoniacal liquor again and obtain the ammonium molybdate solution of molybdenum concentration greater than 100g/l, ammonium molybdate solution is through the heavy ammonium molybdate product that obtains of peracid, inorganic acid radical after the extraction then enters in the raffinate, the ion that contain in the raffinate this moment mainly is inorganic acid radical and sodium ion, so the salt in the raffinate has only a kind of--inorganic salt, but in the prior art, with being discharged after the lime treatment, this has just caused the inorganic salt that contain in the raffinate to be wasted to raffinate often.
Summary of the invention
For overcoming the inorganic salt waste problem that exists in the prior art, the object of the present invention is to provide the recovery method of inorganic salt in a kind of molybdenum oxide or the molybdenum waste alkali leaching-extraction preparing ammonium molybdate technology.
For achieving the above object, the present invention has taked following technical scheme:
The recovery method of inorganic salt in a kind of molybdenum oxide or the molybdenum waste alkali leaching-extraction preparing ammonium molybdate technology: the extraction liquid that will extract the back acquisition carries out the low-temperature negative-pressure evaporative crystallization, its parameter is: 28～70 ℃ of temperature, pressure-0.02～-0.05Mpa, stir speed (S.S.) 20～60rpm, in mass, to be evaporated to the extraction liquid solid content be 20～60% o'clock, be the recyclable inorganic salt that obtain again with the extraction liquid solid-liquid separation.Described stirring is that the anchor formula stirs.
Described inorganic salt are SODIUMNITRATE, sodium-chlor or sodium sulfate.
Described solid-liquid separation is centrifugation, and centrifugal rotational speed is 500～4000rpm, and centrifugation time is 1～30min.
Resulting liquid phase after the solid-liquid separation returned and the extraction liquid low-temperature negative-pressure evaporative crystallization that circulates together.
Molybdenum oxide or molybdenum waste alkali leaching-extraction preparing ammonium molybdate technology can be operated by prior art, can specifically press following process operation among the present invention: as shown in Figure 1, at first molybdenum oxide or molybdenum waste material are carried out ore grinding, be milled to particle diameter at-200 purpose breeze weight contents more than 90%, breeze behind the ore grinding is sized mixing, making powdered ore quality concentration is 20～45%, add yellow soda ash and sodium hydroxide and soak 30～120min at 75～100 ℃ of following alkali, molybdenum is wherein entered in the solution with the form of molybdate, wherein the weight consumption of yellow soda ash and sodium hydroxide is respectively 5～20% and 1～5% of a breeze weight, solid-liquid separation obtains alkali immersion liquid (sodium molybdate solution) and tailings (emitting) afterwards, then alkali immersion liquid (sodium molybdate solution) is added mineral acid (hydrochloric acid, nitric acid or sulfuric acid) to adjust the pH value be 2.0～3.0, use again through (the secondary octanol+kerosene of phase N235+ being arranged with the organic phase after a kind of mineral acid acidifying, three's volumn concentration is in the organic phase: phase N235 20% is arranged, secondary octanol 10%, kerosene 70%) extract 3～10min down at 20～30 ℃, extraction phase is than organic phase: water=2: 3～4: 3, make molybdate in the sodium molybdate solution enter organic phase and become load organic phases, the ammoniacal liquor of using mass concentration 10～20% again is at 15～30 ℃ of 1～10min that strip down, organic phase is compared in back extraction: water=3: 1～5: 1, obtain water and unloading organic phase, water is the ammonium molybdate solution of molybdenum concentration greater than 100g/l, ammonium molybdate solution is through heavy (the heavy pH value 2～3 of acid of mineral acid acid, 45～55 ℃ of the heavy temperature of acid) obtain the ammonium molybdate product, the unloading organic phase is then returned the organic phase recycle after acidifying before the extraction.
The invention has the advantages that: the inventive method is suitable for containing alkali and leaches and extract--the various molybdenum ores or the molybdenum waste disposal operation of reextraction operation, adopt the inventive method can realize that 100% of inorganic salt reclaim, the purity of the inorganic salt that obtain is greater than 99%, and the liquid phase after separating can recycle, thereby " zero " of having realized sewage discharges.
Description of drawings
Fig. 1: existing molybdenum oxide or molybdenum waste alkali leaching-extraction preparing ammonium molybdate process flow diagram;
Fig. 2: the recovery method schematic flow sheet of inorganic salt in molybdenum oxide of the present invention or the molybdenum waste alkali leaching-extraction preparing ammonium molybdate technology.
Embodiment
Below in conjunction with accompanying drawing technical scheme of the present invention is described in further detail, but protection scope of the present invention is not limited thereto:
Embodiment 1
As shown in Figure 1, at first molybdenum oxide or molybdenum waste material are carried out ore grinding, be milled to particle diameter at-200 purpose breeze weight contents more than 90%, to the breeze behind the ore grinding size mixing to the ore pulp mass concentration be 30%, add yellow soda ash and sodium hydroxide and soak 90min at 90 ℃ of following alkali, molybdenum is wherein entered in the solution with the form of molybdate, wherein the weight consumption of yellow soda ash and sodium hydroxide is respectively 15% and 3% of a breeze weight, solid-liquid separation obtains alkali immersion liquid (sodium molybdate solution) and tailings (emitting) afterwards, then alkali immersion liquid (sodium molybdate solution) being added nitric acid adjustment pH value is 2.5, use the organic phase after the acidifying of 2mol/L nitric acid (the secondary octanol+kerosene of phase N235+ to be arranged again, three's volumn concentration is in the organic phase: phase N235 20% is arranged, secondary octanol 10%, kerosene 70%) extract 6min down at 25 ℃, extraction phase is than organic phase: water=1: 1, make molybdate in the sodium molybdate solution enter organic phase and become load organic phases, the ammoniacal liquor of using mass concentration 15% again is at 25 ℃ of reextraction 5min, back extraction is in a ratio of organic phase: water=4: 1, obtain water and unloading organic phase, water is the ammonium molybdate solution of molybdenum concentration greater than 100g/l, ammonium molybdate solution is through heavy (the heavy pH value 2.5 of acid of peroxy-nitric acid acid, 50 ℃ of the heavy temperature of acid) obtain the ammonium molybdate product, the unloading organic phase is then returned the organic phase recycle before the extraction.
As shown in Figure 2, the extraction liquid that obtains after the above-mentioned extraction is carried out the low-temperature negative-pressure evaporative crystallization, its parameter is: 50 ℃ of temperature, pressure-0.03Mpa, anchor formula stir speed (S.S.) 40rpm, in mass, to be evaporated to the extraction liquid solid content be 40% o'clock, (centrifugal rotational speed is 2000rpm by the whizzer separation with extraction liquid again, centrifugation time is 15min) be the recyclable SODIUMNITRATE (purity 99.3%) that obtains, resulting liquid phase after the centrifugation returned and the extraction liquid low-temperature negative-pressure evaporative crystallization that circulates together.
Embodiment 2
As shown in Figure 1, at first molybdenum oxide or molybdenum waste material are carried out ore grinding, be milled to particle diameter at-200 purpose breeze weight contents more than 90%, to the breeze behind the ore grinding size mixing to the ore pulp mass concentration be 20%, add yellow soda ash and sodium hydroxide and soak 30min at 75 ℃ of following alkali, molybdenum is wherein entered in the solution with the form of molybdate, wherein the weight consumption of yellow soda ash and sodium hydroxide is respectively 5% and 1% of a breeze weight, solid-liquid separation obtains alkali immersion liquid (sodium molybdate solution) and tailings (emitting) afterwards, then alkali immersion liquid (sodium molybdate solution) being added hydrochloric acid adjustment pH value is 2.0, (the secondary octanol+kerosene of phase N235+ is arranged with the organic phase behind the hcl acidifying again, three's volumn concentration is in the organic phase: phase N235 20% is arranged, secondary octanol 10%, kerosene 70%) extract 3min down at 20 ℃, extraction phase is than organic phase: water=2: 3, make molybdate in the sodium molybdate solution enter organic phase and become load organic phases, the ammoniacal liquor of using mass concentration 10% again is at 15 ℃ of reextraction 1min, organic phase is compared in back extraction: water=3: 1, obtain water and unloading organic phase, water is the ammonium molybdate solution of molybdenum concentration greater than 100g/l, ammonium molybdate solution is through heavy (the heavy pH value 2 of acid of persalt acid, 45 ℃ of the heavy temperature of acid) obtain the ammonium molybdate product, the unloading organic phase is then returned the organic phase recycle before the extraction.
As shown in Figure 2, the extraction liquid that obtains after the above-mentioned extraction is carried out the low-temperature negative-pressure evaporative crystallization, its parameter is: 28 ℃ of temperature, pressure-0.05Mpa, anchor formula stir speed (S.S.) 20rpm, in mass, to be evaporated to the extraction liquid solid content be 20% o'clock, (centrifugal rotational speed is 4000rpm by the whizzer separation with extraction liquid again, centrifugation time is 1min) be the recyclable sodium-chlor (purity 99.5%) that obtains, resulting liquid phase after the centrifugation returned and the extraction liquid low-temperature negative-pressure evaporative crystallization that circulates together.
Embodiment 3
As shown in Figure 1, at first molybdenum oxide or molybdenum waste material are carried out ore grinding, be milled to particle diameter at-200 purpose breeze weight contents more than 90%, to the breeze behind the ore grinding size mixing to the ore pulp mass concentration be 45%, add yellow soda ash and sodium hydroxide and soak 120min at 100 ℃ of following alkali, molybdenum is wherein entered in the solution with the form of molybdate, wherein the weight consumption of yellow soda ash and sodium hydroxide is respectively 20% and 5% of a breeze weight, solid-liquid separation obtains alkali immersion liquid (sodium molybdate solution) and tailings (emitting) afterwards, then alkali immersion liquid (sodium molybdate solution) being added sulfuric acid adjustment pH value is 3.0, use again through (the secondary octanol+kerosene of phase N235+ being arranged with the organic phase behind a kind of sulfuric acid acidation, three's volumn concentration is in the organic phase: phase N235 20% is arranged, secondary octanol 10%, kerosene 70%) extract 10min down at 30 ℃, extraction phase is than organic phase: water=4: 3, make molybdate in the sodium molybdate solution enter organic phase and become load organic phases, the ammoniacal liquor of using mass concentration 20% again is at 30 ℃ of reextraction 10min, organic phase is compared in back extraction: water=5: 1, obtain water and unloading organic phase, water is the ammonium molybdate solution of molybdenum concentration greater than 100g/l, ammonium molybdate solution is through heavy (the heavy pH value 3 of acid of persulfuric acid acid, 55 ℃ of the heavy temperature of acid) obtain the ammonium molybdate product, the unloading organic phase is then returned the organic phase recycle before the extraction.
As shown in Figure 2, the extraction liquid that obtains after the above-mentioned extraction is carried out the low-temperature negative-pressure evaporative crystallization, its parameter is: 70 ℃ of temperature, pressure-0.02Mpa, anchor formula stir speed (S.S.) 60rpm, in mass, to be evaporated to the extraction liquid solid content be 60% o'clock, (centrifugal rotational speed is 500rpm by the whizzer separation with extraction liquid again, centrifugation time is 30min) be the recyclable sodium sulfate (purity 99.2%) that obtains, resulting liquid phase after the centrifugation returned and the extraction liquid low-temperature negative-pressure evaporative crystallization that circulates together.
Claims (4)
1. the recovery method of inorganic salt in molybdenum oxide or the molybdenum waste alkali leaching-extraction preparing ammonium molybdate technology, it is characterized in that: the raffinate that will extract the back acquisition carries out the low-temperature negative-pressure evaporative crystallization, its parameter is: 28～70 ℃ of temperature, pressure-0.02～-0.05Mpa, stir speed (S.S.) 20～60rpm, in mass, to be evaporated to the raffinate solid content be 20～60% o'clock, be the recyclable inorganic salt that obtain with the raffinate solid-liquid separation again, described inorganic salt are SODIUMNITRATE, sodium-chlor or sodium sulfate.
2. the recovery method of inorganic salt in molybdenum oxide as claimed in claim 1 or the molybdenum waste alkali leaching-extraction preparing ammonium molybdate technology is characterized in that: described stirring is that the anchor formula stirs.
3. the recovery method of inorganic salt in molybdenum oxide as claimed in claim 1 or 2 or the molybdenum waste alkali leaching-extraction preparing ammonium molybdate technology, it is characterized in that: described solid-liquid separation is centrifugation, and centrifugal rotational speed is 500～4000rpm, and centrifugation time is 1～30min.
4. the recovery method of inorganic salt in molybdenum oxide as claimed in claim 3 or the molybdenum waste alkali leaching-extraction preparing ammonium molybdate technology is characterized in that: resulting liquid phase is returned and the raffinate low-temperature negative-pressure evaporative crystallization that circulates together after the solid-liquid separation.
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| CN110438349B (en) * | 2019-09-12 | 2021-12-24 | 河北欣芮再生资源利用有限公司 | Method for preparing high-purity ammonium molybdate from low-grade molybdenum material |
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Inventor after: Wang Anli Inventor after: Li Jianzheng Inventor after: Wang Qingli Inventor after: Fan Shangli Inventor after: Ku Jiangang Inventor after: Xue Wei Inventor after: Li Sanli Inventor after: Qiao Cuijie Inventor before: Ku Jiangang Inventor before: Wang Anli Inventor before: Xue Wei Inventor before: Li Sanli Inventor before: Wang Qingli Inventor before: Fan Shangli |
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Address after: 472500, Jincheng Road, Lingbao City, Henan, Sanmenxia 20 Patentee after: Lingbao Jinyuan Mining Co.,Ltd. Address before: 472500, Jincheng Road, Lingbao City, Henan Province, No. 20 Patentee before: Lingbao City Jinyuan Mining Co., Ltd. |