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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- cathode deposition
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- electrolytic refining
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- 230000008021 deposition Effects 0.000 title claims description 38
- 150000003839 salts Chemical class 0.000 title abstract description 3
- 238000002203 pretreatment Methods 0.000 title 1
- 238000000034 method Methods 0.000 claims abstract description 38
- 239000003792 electrolyte Substances 0.000 claims abstract description 37
- 229910052751 metal Inorganic materials 0.000 claims abstract description 30
- 239000002184 metal Substances 0.000 claims abstract description 30
- 239000000203 mixture Substances 0.000 claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 24
- 238000007670 refining Methods 0.000 claims abstract description 21
- 239000002245 particle Substances 0.000 claims abstract description 11
- 239000011261 inert gas Substances 0.000 claims abstract description 10
- 238000000498 ball milling Methods 0.000 claims abstract description 7
- 239000000428 dust Substances 0.000 claims description 19
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 238000013467 fragmentation Methods 0.000 claims description 8
- 238000006062 fragmentation reaction Methods 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 238000000926 separation method Methods 0.000 abstract description 7
- 239000002253 acid Substances 0.000 abstract description 6
- 238000005406 washing Methods 0.000 abstract description 5
- 239000002244 precipitate Substances 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 13
- 239000010936 titanium Substances 0.000 description 13
- 229910052719 titanium Inorganic materials 0.000 description 13
- 229910052720 vanadium Inorganic materials 0.000 description 9
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 9
- 239000000047 product Substances 0.000 description 4
- 238000005336 cracking Methods 0.000 description 3
- 150000007513 acids Chemical class 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 238000009854 hydrometallurgy Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000006069 physical mixture Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 238000010333 wet classification Methods 0.000 description 1
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Abstract
本发明提供了一种熔盐电解精炼的阴极析出物的预处理方法。所述方法包括以下步骤：在惰性气体保护的环境下，对所述阴极析出物进行破碎、球磨，以得到金属粉末和电解质粉末的混合物，其中，所述混合物的粒径为44～150μm；使用气流对混合物粉末进行风力分离，以实现金属粉末和电解质粉末的分离。本发明的优点包括：能够实现电解质和金属粉末的分离，有效降低阴极析出物中的电解质含量；而且能够减少湿法处理过程稀酸使用量以及清水洗涤次数，可提高工艺经济性、减小环境压力。
The invention provides a method for pretreatment of cathode precipitates in molten salt electrolytic refining. The method comprises the following steps: crushing and ball milling the cathode precipitates in an environment protected by an inert gas to obtain a mixture of metal powder and electrolyte powder, wherein the particle size of the mixture is 44-150 μm; using The airflow separates the mixture powder by air to realize the separation of metal powder and electrolyte powder. The advantages of the present invention include: the separation of electrolyte and metal powder can be realized, and the electrolyte content in the cathode precipitate can be effectively reduced; and the amount of dilute acid used in the wet treatment process and the number of clean water washing can be reduced, which can improve process economy and reduce environmental pollution. 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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| CN201310037177.4A CN103111354B (en) | 2013-01-31 | 2013-01-31 | Pretreatment method for cathode deposition of molten salt electrorefining |
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| CN201310037177.4A CN103111354B (en) | 2013-01-31 | 2013-01-31 | Pretreatment method for cathode deposition of molten salt electrorefining |
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| CN103111354B CN103111354B (en) | 2014-12-24 |
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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 | A wind separation method for separation of 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 |
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| 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 | A wind separation method for separation of carbon materials in molten salt |
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