CN103111354A - Pretreatment method for cathode deposition of molten salt electrorefining - Google Patents
Pretreatment method for cathode deposition of molten salt electrorefining Download PDFInfo
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- CN103111354A CN103111354A CN2013100371774A CN201310037177A CN103111354A CN 103111354 A CN103111354 A CN 103111354A CN 2013100371774 A CN2013100371774 A CN 2013100371774A CN 201310037177 A CN201310037177 A CN 201310037177A CN 103111354 A CN103111354 A CN 103111354A
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Abstract
The invention discloses a pretreatment method for cathode deposition of molten salt electrorefining. The method comprises the following steps of: breaking and ball-milling the cathode deposition in an inert gas shielding environment to obtain a mixture of metal powder and electrolyte powder, wherein the granularity of the mixture is 44-150 microns; and pneumatically separating the mixture powder through airflow so as to separate the metal powder and the electrolyte powder. The pretreatment method disclosed by the invention has the advantages that the separation of the electrolyte and the metal powder is achieved so as to effectively reduce the electrolyte content of the cathode deposition; and the dosage of diluted acid and the frequency of clean water washing in a wet treatment process can be reduced so as to improve process economical efficiency and reduce environment pressure.
Description
Technical field
The present invention relates to the separating treatment technical field of fused-salt electrolytic refining product, more particularly, relate to a kind of to fused-salt electrolytic refining extract vanadium, the resulting cathode deposition of titanium technique carries out preprocess method.
Background technology
Usually, vanadium/titanium is extracted in fused-salt electrolytic refining, thick vanadium/the titanium of general employing is as anode, metal material is negative electrode, electrolyte is alkali metal or alkaline-earth halide and adds wherein a certain amount of low price ion, forms electrolytic cell and carries out electrolysis, and thick vanadium/titanium enters fused salt at Anodic Stripping and with ionic species, migrate to negative electrode and separate out the formation cathode deposition under electric field force and concentration gradient effect, cooled cathode deposition is blocks of solid.
Except the metal dust of crystallization, also contain a large amount of electrolyte in cathode deposition, electrolytical content is according to the variation of electrolytic condition, and fluctuation range is 30%~90%.
In order to obtain qualified metal powder product, must separate metal powder and electrolyte in cathode deposition, therefore, need the target precipitate to carry out hydrometallurgical process, described hydrometallurgical process generally includes: broken, leach, grind, the operations such as washing, wet classification, dehydration, oven dry.Owing to containing a large amount of electrolyte in cathode deposition, need to use a large amount of diluted acids during leaching, solid-to-liquid ratio is generally 1: 5~and 1: 10, and 6~7 diluted acids of needs and clear water washing, this process can produce a large amount of addition products and spent acid, and this will have a strong impact on process economy and cause larger pressure to environment.
Summary of the invention
For the prior art above shortcomings, one of purpose of the present invention is to provide a kind of and simple and directly effective and free from environmental pollution the method that vanadium, the resulting cathode deposition of titanium technique separate is extracted in fused-salt electrolytic refining.
The invention provides a kind of preprocess method of cathode deposition of fused-salt electrolytic refining.Said method comprising the steps of: under the environment of inert gas shielding, described cathode deposition is carried out fragmentation, ball milling, to obtain the mixture of metal dust and electrolyte powder, wherein, the particle diameter of described mixture is 44~150 μ m; Use air-flow to carry out wind-force to mix powder and separate, to realize separating of metal dust and electrolyte powder.
In one exemplary embodiment of the present invention, described air-flow can be formed by inert gas.
In one exemplary embodiment of the present invention, described wind-force separating step can adopt described mixture is vertically fallen, and the mode that adopts the air-flow of along continuous straight runs motion to blow to the mixture that is in falling state is carried out.
In one exemplary embodiment of the present invention, the falling speed of described mixture can be 0.5~10kg/min.
In one exemplary embodiment of the present invention, the flowing velocity of described air-flow can be 5~25L/min.
In one exemplary embodiment of the present invention, described inert gas and air-flow can be argon gas.
Compared with prior art, the beneficial effect of preprocess method of the present invention comprises: can realize separating of electrolyte and metal dust, effectively reduce the electrolyte content in cathode deposition; And can reduce wet-treating process diluted acid use amount and clear water washing times, can improve process economy, reduce environmental pressure.
Description of drawings
Fig. 1 shows the wind-force separator schematic diagram be used to the preprocess method of the cathode deposition of realizing fused-salt electrolytic refining of the present invention.
Description of reference numerals:
1-feed bin, 2-baiting valve, 3-air current spray nozzle, 4-metal bunker for collecting and 5-electrolyte bunker for collecting.
The specific embodiment
Hereinafter, describe the preprocess method of the cathode deposition of fused-salt electrolytic refining of the present invention in detail in connection with exemplary embodiment.
Can comprise the following steps according to the preprocess method of the cathode deposition of fused-salt electrolytic refining of the present invention: under the environment of inert gas (being preferably argon gas) protection, described cathode deposition is carried out fragmentation, ball milling, to obtain the mixture of metal dust and electrolyte powder, wherein, the particle diameter of described mixture is 44~150 μ m; Use air-flow to carry out wind-force to mix powder and separate, to realize separating of metal dust and electrolyte powder.
Specifically, the cathode deposition that fused-salt electrolytic refining extraction vanadium/titanium obtains is by metal dust and electrolyte ingredient, and the electrolyte after wherein metal dust is solidified wraps up.Can destroy simple reunion between metal powder granulates and most of electrolyte to the parcel of metal by fragmentation and ball milling, obtain the physical mixture of metal dust and electrolyte powder.The density of vanadium and titanium is respectively 6.11g/cm
3, 4.51g/cm
3, electrolyte density is generally 1.6~2.4g/cm
3, when metal dust and electrolyte free-falling, do the used time when being subject to onesize wind-force, the electrolyte powder that density is less can produce larger skew track, thereby falls in different containers from metal dust, realizes separating.
In an exemplary embodiment of the preprocess method of cathode deposition of the present invention, air-flow is formed by inert gas (being preferably argon gas).
In another exemplary embodiment of the preprocess method of cathode deposition of the present invention, the wind-force separating step vertically falls mixture, and adopts the air-flow of along continuous straight runs motion to blow to the mixture that is in falling state.Wherein, the too fast meeting of mixture falling speed reduces metal and electrolytical separation rate, and the slow operating efficiency that fell is lower, and therefore best falling speed is 0.5~10kg/min; For metal dust is fully separated with electrolysis mass-energy, the speed of air-flow should be not less than 5L/min in addition, and air-flow velocity is excessive, can make a large amount of metal dusts enter the electrolyte feeder, and the flowing velocity that therefore should control air-flow is 5~25L/min; The particle size after cracking of cathode deposition is also the important indicator that affects separation process, the too small electrolyte that can not fully destroy of particle size after cracking is to the parcel of metal dust and the reunion between metal dust, therefore only have and cathode deposition is crushed to suitable scope could obtains higher separation rate, through experimental verification, best particle size after cracking scope is 44~150 μ m.
The advantage of the preprocess method of cathode deposition of the present invention comprises: this preprocess method is physical method, do not produce addition product, environmentally friendly, equipment is simple, energy consumption is low, and is significant to improving the economy that fused-salt electrolytic refining extracts vanadium, titanium technique.
Fig. 1 shows the wind-force separator schematic diagram be used to the preprocess method of the cathode deposition of realizing fused-salt electrolytic refining of the present invention.
As shown in Figure 1, in one exemplary embodiment of the present invention, the preprocess method of the cathode deposition of fused-salt electrolytic refining can be realized in the following manner:
At first, block cathode deposition is carried out fragmentation, and ball milling is 44~150 μ m to the particle size range of mixture, this process is carried out under the inert gas shielding of drying;
Then, the mixture after ball milling being used as shown in Figure 1, device carries out the wind-force separation.Specifically, mixture is positioned in feed bin 1, control blanking velocity by baiting valve 2, mixture falls naturally through the gas flow of air current spray nozzle 3 ejections under Action of Gravity Field, metal dust density is larger, and the skew track is less under airflow function, falls into metal bunker for collecting 4, the electrolyte powder that density is less produces larger skew track and falls into electrolyte bunker for collecting 5 under airflow function, thereby has realized metal dust and most of electrolytical separation.
Example 1
Get titanium cathode deposition 1500g, wherein electrolyte content 85%, after fragmentation, be milled to particle diameter 150 μ m in ball mill, mix powder is positioned in separator, and controlling blanking velocity by baiting valve is 0.5kg/min, and the control throughput is 5L/min, after separating end, in titanium valve, electrolyte content is 9.8% after testing.
Example 2
Get titanium cathode deposition 1500g, wherein electrolyte content 85%, after fragmentation, be milled to particle diameter 44 μ m in ball mill, mix powder is positioned in separator, and controlling blanking velocity by baiting valve is 10kg/min, and the control throughput is 25L/min, after separating end, in titanium valve, electrolyte content is 5.0% after testing.
Example 3
Get vanadium cathode deposition 1500g, after fragmentation, wherein electrolyte content 85%, be milled to particle diameter 74 μ m in ball mill, mix powder is positioned in separator, and controlling blanking velocity by baiting valve is 5kg/min, and the control throughput is 10L/min, after separating end, in titanium valve, electrolyte content is 8.2% after testing.
Can find out, in the cathode deposition after employing the inventive method is processed, electrolyte content can be down to 5~10%.
In sum, preprocess method of the present invention is applicable to the cathode deposition of fused-salt electrolytic refining is processed; Can realize separating of electrolyte and metal dust, effectively reduce the electrolyte content in cathode deposition; And can reduce wet-treating process diluted acid use amount and clear water washing times, can improve process economy, reduce environmental pressure.
Although the above has described the present invention with exemplary embodiment by reference to the accompanying drawings, those of ordinary skills should be clear, in the situation that do not break away from the spirit and scope of claim, can carry out various modifications to above-described embodiment.
Claims (6)
1. the preprocess method of the cathode deposition of a fused-salt electrolytic refining, is characterized in that, said method comprising the steps of:
Under the environment of inert gas shielding, described cathode deposition is carried out fragmentation, ball milling, to obtain the mixture of metal dust and electrolyte powder, wherein, the particle diameter of described mixture is 44~150 μ m;
Use air-flow to carry out wind-force to mix powder and separate, to realize separating of metal dust and electrolyte powder.
2. the preprocess method of the cathode deposition of fused-salt electrolytic refining according to claim 1, is characterized in that, described air-flow is formed by inert gas.
3. the preprocess method of the cathode deposition of fused-salt electrolytic refining according to claim 1, is characterized in that, described wind-force separating step vertically falls described mixture, and adopt the air-flow of along continuous straight runs motion to blow to the mixture that is in falling state.
4. the preprocess method of the cathode deposition of fused-salt electrolytic refining according to claim 3, is characterized in that, the falling speed of described mixture is 0.5~10kg/min.
5. the preprocess method of the cathode deposition of fused-salt electrolytic refining according to claim 3, is characterized in that, the flowing velocity of described air-flow is 5~25L/min.
6. the preprocess method of the cathode deposition of fused-salt electrolytic refining according to claim 1, is characterized in that, described inert gas and air-flow are argon gas.
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104480498A (en) * | 2015-01-05 | 2015-04-01 | 攀钢集团攀枝花钢铁研究院有限公司 | Molten salt electrolysis cathode educt separating method and device |
CN106191929A (en) * | 2016-09-07 | 2016-12-07 | 攀钢集团攀枝花钢铁研究院有限公司 | The method separating Titanium from titanium electrolysis cathode product |
CN107282598A (en) * | 2017-07-03 | 2017-10-24 | 李立安 | A kind of aluminium cell discards the recoverying and utilizing method of cathode carbon pieces |
CN107537769A (en) * | 2017-08-24 | 2018-01-05 | 江苏米莫金属股份有限公司 | A kind of metal powder recycling device |
CN108339746A (en) * | 2017-01-25 | 2018-07-31 | 宁波创润新材料有限公司 | Screening plant for detaching powder |
CN109499729A (en) * | 2019-01-04 | 2019-03-22 | 亚太环保股份有限公司 | A kind of breaking method of waste cathode of aluminum electrolytic cell |
CN114405827A (en) * | 2022-01-27 | 2022-04-29 | 武汉大学 | Wind power separation method for separating carbon materials in molten salt |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104480498A (en) * | 2015-01-05 | 2015-04-01 | 攀钢集团攀枝花钢铁研究院有限公司 | Molten salt electrolysis cathode educt separating method and device |
CN106191929A (en) * | 2016-09-07 | 2016-12-07 | 攀钢集团攀枝花钢铁研究院有限公司 | The method separating Titanium from titanium electrolysis cathode product |
CN108339746A (en) * | 2017-01-25 | 2018-07-31 | 宁波创润新材料有限公司 | Screening plant for detaching powder |
CN107282598A (en) * | 2017-07-03 | 2017-10-24 | 李立安 | A kind of aluminium cell discards the recoverying and utilizing method of cathode carbon pieces |
CN107537769A (en) * | 2017-08-24 | 2018-01-05 | 江苏米莫金属股份有限公司 | A kind of metal powder recycling device |
CN109499729A (en) * | 2019-01-04 | 2019-03-22 | 亚太环保股份有限公司 | A kind of breaking method of waste cathode of aluminum electrolytic cell |
CN114405827A (en) * | 2022-01-27 | 2022-04-29 | 武汉大学 | Wind power separation method for separating carbon materials in molten salt |
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