CN103526036A - Vertical efficient vacuum distillation system for removing impurities from indium - Google Patents
Vertical efficient vacuum distillation system for removing impurities from indium Download PDFInfo
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- CN103526036A CN103526036A CN201310537643.5A CN201310537643A CN103526036A CN 103526036 A CN103526036 A CN 103526036A CN 201310537643 A CN201310537643 A CN 201310537643A CN 103526036 A CN103526036 A CN 103526036A
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Abstract
The invention discloses a vertical efficient vacuum distillation system for removing impurities from indium. The vertical efficient vacuum distillation system comprises a vacuum furnace, a dust collector and a vacuum pump, wherein the vacuum furnace is communicated with the dust collector, and the dust collector is communicated with the vacuum pump. The vacuum furnace comprises a stainless steel furnace body, a graphite crucible, a stainless steel collector, a condenser, an upper cover, a connecting flange, a fire-resistant material layer and a thermal insulation layer, wherein the fire-resistant material layer is arranged on the periphery of the stainless steel furnace body and the bottom face of the stainless steel furnace body, electric heating wires are embedded into the fire-resistant material layer, the periphery of the fire-resistant material layer is wrapped by the thermal insulation layer, the condenser is connected with the stainless steel furnace body through the connecting flange, positioning lugs are arranged on the inner wall of the condenser, the upper cover is arranged on the condenser, a through hole for conducting vacuumizing is formed in the upper cover, the graphite crucible is arranged in the stainless steel furnace body through supporting legs, and the stainless steel collector is arranged on the graphite crucible. The vertical efficient vacuum distillation system has a very good impurity removing effect, the impurity removing rate can reach 99.999%, and the requirement of 5N high-purity indium for the rough indium purity existing before electrolytic refining is conducted can be completely met.
Description
Technical field
The present invention relates to a kind of indium electrorefining initial vacuum except using mixedly vertical high-efficiency vacuum Distallation systm.
Background technology
Indium ingot because of its light perviousness and electroconductibility strong, mainly for the production of ITO target, produce liquid-crystal display and flat screens.Indium ingot can also be for electronic semi-conductor field, scolder and alloy field, research industry.In addition, because its softer character needs in the industry of filler metal also for tooled joint at some, as: the vacuum gap filling material under comparatively high temps.In actual application, more and more higher to the purity requirement of indium, generally need purity 5N(99.999%) more than, most of impurity such as cadmium all requires below 0.00003%.
Impurity in thick indium is mainly to adopt the method for electrolysis to remove, but because standard potential and the indium of inpurity cadmium and thallium are very approaching, by the method for electrolysis, is removed and be difficult to reach requirement.Traditional method is to adopt chemical process, utilizes the complexing under glycerine protection of potassiumiodide and potassium to remove cadmium; Utilize ammonium chloride and zinc chloride to remove thallium.Not only the long-acting rate of technical process is low for this method, and the loss of indium is large, and impurity-eliminating effect is poor, and environmental pollution is large, and removal of impurities process can produce pungent stink, harmful to HUMAN HEALTH.
In current disclosed patent documentation, Chinese patent application 200810143986.2 " a kind of high purity indium removes method and the device of cadmium and thallium in producing " discloses a kind of method and device that utilizes vacuum to remove cadmium and thallium, the device adopting in this patent mainly has the following disadvantages: unreasonable structure, do not design suitable collector stroke (titanium plate height) and heating stroke (crucible height), impurity-eliminating effect is bad.Also have crucible bottom face to contact with body of heater, between there is no space, be unfavorable for forming upward air stream, affect impurity-eliminating effect.Especially suitability is not strong, does not have a universal significance.Industrial material is not only to contain single contaminant conventionally, and when plurality of impurities is mixed in together while occurring, this device is not described terms of settlement.
Summary of the invention
The technical problem to be solved in the present invention is: provide the vertical high-efficiency vacuum Distallation systm for indium removing impurities of a kind of reasonable in design, good impurity removing effect, to solve above-mentioned the deficiencies in the prior art part.
The technical scheme solving the problems of the technologies described above is:
Vertical high-efficiency vacuum Distallation systm for a kind of indium removing impurities, comprise vacuum oven, particle collector and vacuum pump, described vacuum oven is communicated with particle collector, particle collector is communicated with vacuum pump, described vacuum oven comprises stainless steel body of heater, plumbago crucible, stainless steel collector, condenser, upper cover, joint flange, refractory masses and thermal insulation layer, described refractory masses is arranged on stainless steel body of heater periphery and bottom surface, in described refractory masses, be inlaid with electrothermal oven silk, thermal insulation layer is wrapped in refractory masses periphery, described condenser is connected with stainless steel body of heater by joint flange, on described condenser inwall, be provided with chucking lug, upper cover is arranged on condenser, on cover the through hole having for vacuumizing, described plumbago crucible is arranged in stainless steel body of heater by feet, plumbago crucible outer wall contacts with stainless steel inboard wall of furnace body, described stainless steel collector comprises cylindrical collector and is positioned at the upper collector of cylindrical collector top, on upper collector, have venting hole, described cylindrical collector is placed on plumbago crucible, cylindrical collector outer wall contacts with condenser inwall, upper collector is placed on chucking lug, the height H 3 of described cylindrical collector is 400 ~ 600mm, described plumbago crucible sidewall end face and the distance H of material bed end face 2 are 400 ~ 600mm, described plumbago crucible bottom surface to the distance H 4 of stainless steel body of heater inner bottom surface is 5-10mm.
The diameter of the venting hole of described upper collector is 4 ~ 7mm, and described upper collector lower surface to the distance of cylindrical collector top end face is 5-10mm.
Described particle collector comprises housing, inlet pipe and adds the pure aluminium silicate weighting material filling in housing, described inlet pipe is inserted in pure aluminium silicate weighting material through housing, air distributor is also installed in inlet pipe, on the housing of described pure aluminium silicate weighting material top, also offer pneumatic outlet, the inlet pipe of described particle collector is communicated with the upper cover through hole of vacuum oven, and described particle collector pneumatic outlet is communicated with vacuum pump.
In described particle collector housing, the height H 5 of pure aluminium silicate weighting material is 450 ~ 500mm, and the depth H 6 that described inlet pipe is inserted pure aluminium silicate weighting material is 350 ~ 370mm.
Owing to adopting technique scheme, the present invention's indium removing impurities has good impurity-eliminating effect with vertical high-efficiency vacuum Distallation systm, and impurities removing efficiency can reach 99.999%, can meet the requirement to thick indium purity before electrorefining of 5N high purity indium completely.Its beneficial effect is specifically described below:
1, the stroke of collector of the present invention (being the height of cylindrical collector) is designed to 400 ~ 600mm.Setting under vacuum degree condition, after being heated to certain temperature, reach the evaporation of can escaping of metal ion that evaporation presses from metallic solution.The cold rapid condensation of metal vapors chance of evaporation enters collector and reaches impurity-eliminating effect.If collector stroke is too short, condensed metal there will be and returns moltenly, affects impurity-eliminating effect; If collector stroke is long, the evaporation of the metal vapors of evaporation can be not enough to arrive at collector not, does not reach equally removal of impurities object.The distance H 2 of plumbago crucible sidewall top and material melting liquid level is 400 ~ 600mm, is heating stroke, enough escape heat energy is provided to up metal vapors.The trip is too short, and evaporation energy is inadequate; The trip is long, and energy surplus increases unit cost.Plumbago crucible is supported and can be improved internal gas flow direction by feet, is convenient to form upward air stream.
2, adopt the present invention to carry out removal of impurities work; in process, do not need to use any poisonous and hazardous chemical reagent; and whole removal of impurities process is to carry out in complete totally enclosed device; whole production process safety and environmental protection; can be because of the operator that exert an influence of toxic gas healthy, and be also conducive to environment protection.
Below, in conjunction with the accompanying drawings and embodiments a kind of indium removing impurities of the present invention is further described with the technical characterictic of vertical high-efficiency vacuum Distallation systm.
Accompanying drawing explanation
Fig. 1: vertical high-efficiency vacuum Distallation systm structural representation for a kind of indium removing impurities of the present invention.
Fig. 2: vacuum oven structural representation.
Fig. 3: particle collector structural representation.
Fig. 4: particle collector inlet pipe and air distributor vertical view.
In figure: I-vacuum oven, II-particle collector, III-vacuum pump.
1-upper cover, 101-through hole, 2-condenser, 3-stainless steel collector, the upper collector of 31-, 311-venting hole, 32-chucking lug, 33-cylindrical collector, 4-joint flange, 5-stainless steel body of heater, 6-refractory masses, 7-electrothermal oven silk, 8-plumbago crucible, 9-thermal insulation layer, 10-feet, 11-housing, 12-pure aluminium silicate weighting material, 13-pneumatic outlet, 14-air distributor, 15-inlet pipe.
A-is material bed.
In Fig. 2, arrow represents gas flow direction.
Embodiment
Embodiment 1: vertical high-efficiency vacuum Distallation systm for a kind of indium removing impurities, comprise vacuum oven I, particle collector II and vacuum pump III, described vacuum oven is communicated with particle collector, particle collector is communicated with vacuum pump, described vacuum oven comprises stainless steel body of heater 5, plumbago crucible 8, stainless steel collector 3, condenser 2, upper cover 1, joint flange 4, refractory masses 6 and thermal insulation layer 9, described refractory masses 6 is arranged on stainless steel body of heater 8 peripheries and bottom surface, in described refractory masses, be inlaid with electrothermal oven silk 7, thermal insulation layer is wrapped in refractory masses periphery, described condenser 3 is connected with stainless steel body of heater by water-cooled joint flange 4, on described condenser 2 inwalls, be welded with chucking lug 32, upper cover 1 is arranged on condenser, on cover the through hole 101 having for vacuumizing, described plumbago crucible 8 is arranged in stainless steel body of heater by feet 10, plumbago crucible outer wall contacts with stainless steel inboard wall of furnace body, described stainless steel collector 3 comprises cylindrical collector 33 and is positioned at the upper collector 31 of cylindrical collector top, on upper collector, have venting hole 311, described cylindrical collector is placed on plumbago crucible 8, cylindrical collector outer wall contacts with condenser 2 inwalls, upper collector is placed on chucking lug, the effect of chucking lug is to support upper collector.
The height H 3 of described cylindrical collector 33 is 400 ~ 600mm, and described plumbago crucible sidewall end face and the distance H of material bed end face 2 are 400 ~ 600mm, and described upper collector lower surface to the distance of cylindrical collector top end face is 5-10mm.Described plumbago crucible bottom surface is 5 ~ 10mm to the distance H 4 of stainless steel body of heater inner bottom surface, and the diameter of the venting hole 311 of described upper collector is 4 ~ 7mm.The quantity of described venting hole can be determined according to practical situation, is generally 4-5; Described venting hole can uniformly be arranged in circle, can be arranged in straight line, also can arrange by other shapes.
Described particle collector comprises housing 11, inlet pipe 15 and adds the pure aluminium silicate weighting material 12 filling in housing, described inlet pipe is inserted in pure aluminium silicate weighting material through housing, conical air distributor 14 is also installed in inlet pipe, the effect of air distributor is to make air-flow to inlet pipe diffusion around, does not concentrate away tube hub.On the housing of described pure aluminium silicate weighting material top, also offer pneumatic outlet 13, the inlet pipe 15 of described particle collector is communicated with the upper cover through hole 101 of vacuum oven, and described particle collector pneumatic outlet 13 is communicated with vacuum pump.In described particle collector housing, the height H 5 of pure aluminium silicate weighting material is 480mm, and the depth H 6 that described inlet pipe is inserted pure aluminium silicate weighting material is 360mm.
Adopt the present invention to be suitable for intermittently impurity removal process, first material is put into plumbago crucible, then plumbago crucible is put into vacuum oven and carried out removing impurities, after removing impurities finishes, then material is poured out from plumbago crucible.
As a kind of conversion of the present embodiment, described particle collector also can adopt the particle collector of other structures, as long as can guarantee dust collecting effect, the gas that makes to enter in vacuum pump meets the requirements.
Claims (4)
1. a vertical high-efficiency vacuum Distallation systm for indium removing impurities, it is characterized in that: comprise vacuum oven (I), particle collector (II) and vacuum pump (III), described vacuum oven is communicated with particle collector, particle collector is communicated with vacuum pump, described vacuum oven comprises stainless steel body of heater (5), plumbago crucible (8), stainless steel collector (3), condenser (2), upper cover (1), joint flange (4), refractory masses (6) and thermal insulation layer (9), described refractory masses (6) is arranged on stainless steel body of heater (8) periphery and bottom surface, in described refractory masses, be inlaid with electrothermal oven silk (7), thermal insulation layer is wrapped in refractory masses periphery, described condenser (3) is connected with stainless steel body of heater by joint flange (4), on described condenser (2) inwall, be provided with chucking lug (32), upper cover (1) is arranged on condenser, on cover the through hole (101) having for vacuumizing, described plumbago crucible (80) is arranged in stainless steel body of heater by feet (10), plumbago crucible outer wall contacts with stainless steel inboard wall of furnace body, described stainless steel collector (3) comprises cylindrical collector (33) and is positioned at the upper collector (31) of cylindrical collector top, on upper collector, have venting hole (311), described cylindrical collector is placed on plumbago crucible (8), cylindrical collector outer wall contacts with condenser (2) inwall, upper collector is placed on chucking lug, the height H 3 of described cylindrical collector (33) is 400 ~ 600mm, described plumbago crucible sidewall end face and the distance H of material bed end face 2 are 400 ~ 600mm, described plumbago crucible bottom surface to the distance H 4 of stainless steel body of heater inner bottom surface is 5-10mm.
2. vertical high-efficiency vacuum Distallation systm for a kind of indium removing impurities according to claim 1, it is characterized in that: the diameter of the venting hole of described upper collector (311) is 4 ~ 7mm, described upper collector lower surface to the distance of cylindrical collector top end face is 5-10mm.
3. vertical high-efficiency vacuum Distallation systm for a kind of indium removing impurities according to claim 1 and 2, it is characterized in that: described particle collector comprises housing (11), inlet pipe (15) and add the pure aluminium silicate weighting material (12) filling in housing, described inlet pipe is inserted in pure aluminium silicate weighting material through housing, air distributor (14) is also installed in inlet pipe, on the housing of described pure aluminium silicate weighting material top, also offer pneumatic outlet (13), the inlet pipe of described particle collector (15) is communicated with the upper cover through hole (101) of vacuum oven, described particle collector pneumatic outlet (13) is communicated with vacuum pump.
4. vertical high-efficiency vacuum Distallation systm for a kind of indium removing impurities according to claim 3, it is characterized in that: in described particle collector housing, the height H 5 of pure aluminium silicate weighting material is 450 ~ 500mm, the depth H 6 that described inlet pipe is inserted pure aluminium silicate weighting material is 350 ~ 370mm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106591588A (en) * | 2017-01-10 | 2017-04-26 | 峨眉山市元素新材料科技有限公司 | Vacuum distillation device for preparing 6N indium |
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| WO1996026297A1 (en) * | 1995-02-21 | 1996-08-29 | Materials Research Corporation | Ultra high purity magnesium and vacuum distillation purification method and apparatus |
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- 2013-11-04 CN CN201310537643.5A patent/CN103526036B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996026297A1 (en) * | 1995-02-21 | 1996-08-29 | Materials Research Corporation | Ultra high purity magnesium and vacuum distillation purification method and apparatus |
| JP3121816B1 (en) * | 2000-02-08 | 2001-01-09 | 川崎重工業株式会社 | Metal distillation apparatus and method |
| JP2002212647A (en) * | 2001-01-23 | 2002-07-31 | Dowa Mining Co Ltd | Highly refining method for high purity metal and refining apparatus therefor |
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Non-Patent Citations (1)
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| 李冬生 等: "真空蒸馏法从粗铟中脱除镉锌铊铅的研究", 《真空科学与技术学报》, vol. 32, no. 4, 30 April 2012 (2012-04-30), pages 296 - 300 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106591588A (en) * | 2017-01-10 | 2017-04-26 | 峨眉山市元素新材料科技有限公司 | Vacuum distillation device for preparing 6N indium |
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