CN101403039B - Sublimation apparatus for metal purification - Google Patents
Sublimation apparatus for metal purification Download PDFInfo
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- CN101403039B CN101403039B CN2008101808890A CN200810180889A CN101403039B CN 101403039 B CN101403039 B CN 101403039B CN 2008101808890 A CN2008101808890 A CN 2008101808890A CN 200810180889 A CN200810180889 A CN 200810180889A CN 101403039 B CN101403039 B CN 101403039B
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Abstract
The invention provides a sublimation apparatus used for the purification of metals. The apparatus comprises a bracket, a heating furnace which is supported on the bracket, a subliming sleeve which is arranged in the heating furnace, extends along the longitudinal direction of the heating furnace and passes through the whole heating furnace, a charging container which is arranged in the subliming sleeve and is positioned in a first section of the subliming sleeve, and a condenser which is arranged in the subliming sleeve and positioned in a second section of the subliming sleeve; particularly, the heating furnace comprises a first heating furnace and a second heating furnace which are separated mutually; the temperature of the first heating furnace is different from that of the second heating furnace, wherein, the first section of the subliming sleeve is positioned in the first heating furnace and the second section of the subliming sleeve is positioned in the second heating furnace. Preferably the sublimation apparatus used for purification of metals adopts the whole horizontal structure, particularly, the heating furnace is horizontally supported on the bracket, the subliming sleeve is horizontally arranged in the heating furnace and the charging container and the condenser are respectively and horizontally arranged in the subliming sleeve.
Description
Technical field
The present invention relates to the purification of metals field, be specifically related to be used for the sublimation apparatus of purification of metals.
Background technology
Utilizing sublimation apparatus that metal is purified is purification of metals means commonly used at present.The principle of purification of metals sublimation apparatus is as follows: different metallic elements has different boiling under different vacuum conditions, and temperature and vacuum tightness by in the control process furnace are removed thereby make the lower-boiling impurity element at first evaporate, volatilize or distil; Controlled temperature makes evaporation of metal, volatilization or the distillation of wishing acquisition then, and then collects by condensation, thus the metal product that obtains purifying; Final some infusibility, difficult evaporable foreign metal remain in the charging crucible, and they also can be removed easily.
In the prior art, to the metal general vertical sublimation apparatus that adopts of purifying that distils, as shown in Figure 1.In this vertical sublimation apparatus, adopt well formula resistance furnace 10 as process furnace, the insulating cotton layer 8 that the hot spots of well formula resistance furnace 10 comprises fire brick layer 7, is arranged on the resistance wire 4 in the refractory brick 7 and surrounds fire brick layer 7.Fire brick layer 7 inside are provided with the vacuum-sublimation jar 20 that extends upwardly to well formula resistance furnace 10 outsides from the bottom of fire brick layer 7.Vacuum-sublimation jar 20 comprises the distillation sleeve pipe 1 as outer cover, is disposed with charging crucible 6 in the sleeve pipe 1 from bottom to top in distillation, covers at the grid distributor 5 on the charging crucible 6, is erected at condenser 3 above the grid distributor 5 and the low collector 2 that boils that is arranged on condenser 3 tops.Wherein, distillation sleeve pipe 1 adopts stainless steel or silica tube material to make.Temperature control in the well formula resistance furnace 10 of this sublimation apparatus is divided into three parts from bottom to top, each part need satisfy different temperature condition, yet in all-in-one-piece well formula resistance furnace 10, utilize one group of resistance wire 4 that is arranged on fire brick layer 7 realize this segmentation temperature control be very complicated and control accuracy not high, thereby make the relatively poor and operational difficulty of impurity-eliminating effect.And; for vertical sublimation apparatus; when the distillation metal in condenser 3, condense and attached to the inwall of condenser 3 on after; along with the amount of the metallic particles that adheres to is more and more; the situation that metallic particles comes off takes place through regular meeting; this also can cause disadvantageous effect to the purification of metals process, even can damage equipment.In addition, the manufacturing of vertical sublimation apparatus and assembling are all higher than complexity and manufacturing cost.
Summary of the invention
The purpose of this invention is to provide a kind of novel sublimation apparatus that is used for purification of metals, this equipment adopts the process furnace of separate type to carry out temperature control; Further, provide a kind of sublimation apparatus that is used for purification of metals, it adopts horizontal type structure to replace vertical structure of the prior art.
At above-mentioned purpose, according to the invention provides a kind of sublimation apparatus that is used for purification of metals, this sublimation apparatus comprises: support; Be supported in the process furnace on the support; The distillation sleeve pipe is arranged in the process furnace and extends through whole process furnace along the longitudinal direction of process furnace; Charge cask is arranged in the distillation sleeve pipe and is arranged in distillation telescopic first section; Condenser is arranged in the distillation sleeve pipe and is arranged in distillation telescopic second section; Especially, process furnace comprises first process furnace and second process furnace that is separated from each other, and the temperature in first process furnace and second process furnace is different, wherein, distillation telescopic first section is arranged in first process furnace, and distillation telescopic second section is arranged in second process furnace.
Preferably, according to the sublimation apparatus that is used for purification of metals of the present invention, wherein, the whole horizontal type structure that adopts of sublimation apparatus, particularly, process furnace flatly is supported on the support, distillation sleeve water level land is arranged in the process furnace, and charge cask and condenser all flatly are arranged in the distillation sleeve pipe.
Preferably, according to the sublimation apparatus that is used for purification of metals of the present invention, wherein, have transition zone between distillation telescopic first section and second section, this transition zone is between first process furnace and second process furnace and be exposed in the external environment.
Preferably, according to the sublimation apparatus that is used for purification of metals of the present invention, wherein, distillation telescopic first section has cylindrical shape, and distillation telescopic second section has towards the telescopic exit end cone shape of chap gradually that distils.
Preferably, according to the sublimation apparatus that is used for purification of metals of the present invention, wherein, the condenser that is arranged in second section has towards the tapered cone shape of distillation telescopic exit end.
Preferably, according to the sublimation apparatus that is used for purification of metals of the present invention, wherein, process furnace comprises near distillation telescopic flame retardant coating and the thermal insulation layer that is centered around the flame retardant coating outside, is provided with resistance wire in the flame retardant coating.
Preferably, according to the sublimation apparatus that is used for purification of metals of the present invention, wherein, resistance wire is the resistance wire of diameter 8mm.
Preferably, according to the sublimation apparatus that is used for purification of metals of the present invention, wherein, flame retardant coating is formed by refractory brick, and thermal insulation layer is formed by insulating cotton.
Preferably, according to the sublimation apparatus that is used for purification of metals of the present invention, wherein, the distillation sleeve pipe is made by quartz material or stainless material.
Preferably, according to the sublimation apparatus that is used for purification of metals of the present invention, wherein, charge cask is a crucible.
The present invention has following useful technique effect:
The process furnace that is used for the sublimation apparatus of purification of metals according to the present invention is a split-type structural,, has comprised two complete separated portions that is, can adopt different Heating temperatures in these two separate parts, and can not influence each other; Simultaneously, the temperature in each process furnace part can keep constant relatively, and control mode is simple thereby be convenient to accurate control, thereby improves refining effect; And this sublimation apparatus adopts horizontal type structure to replace vertical structure of the prior art, and this helps the assembling of equipment and reduces manufacturing cost, also helps the raising refining effect simultaneously.
Should be appreciated that above generality is described and the following detailed description is all enumerated and illustrative, purpose is for to the claimed further instruction that the invention provides.
Description of drawings
Accompanying drawing constitutes the part of this specification sheets, is used to help further understand the present invention.These accompanying drawings illustrate some embodiments of the present invention, and are used for illustrating principle of the present invention with specification sheets.Identical in the accompanying drawings parts are represented with identical label.In the accompanying drawing:
Fig. 1 shows the result schematic diagram that is used for the vertical sublimation apparatus of purification of metals of the prior art;
Fig. 2 shows the structural representation that is used for the sublimation apparatus of purification of metals according to of the present invention.
Embodiment
Now with reference to accompanying drawing the specific embodiment of the present invention is described.
Fig. 2 shows the sublimation apparatus that is used for purification of metals according to of the present invention, and this equipment is used for the purification of high purity metal, in particular for the purification of purity at the metal more than 99.999% (as: As, Sb, Te etc.).Preferably, as shown in Figure 2, the sublimation apparatus that is used for purification of metals according to the present invention has adopted horizontal type structure, and it comprises: support 7; Flatly be supported in process furnace 3 on the support 7; Distillation sleeve pipe 8 flatly is arranged in the process furnace 3 and extends through whole process furnace 3 along the longitudinal direction of process furnace 3; Charging crucible (charge cask) 1, it is inner and be arranged in heated zones (first section) 8a of distillation sleeve pipe 8 flatly to be arranged on distillation sleeve pipe 8; Condenser 6 flatly is arranged in the distillation sleeve pipe 8 and is arranged in condensation section (second section) 8b of distillation sleeve pipe 8.Particularly, according to orientation shown in Figure 2, above-mentioned heated zones 8a and condensation section 8b lay respectively at left side and the right side at distillation sleeve pipe 8, promptly, charging crucible 1 is arranged on the left part of distillation sleeve pipe 8, and condenser 6 is arranged on the right side part of distillation sleeve pipe 8, and charging crucible 1 is in identical level height basically with condenser 6.
Especially, according to sublimation apparatus of the present invention, wherein process furnace 3 comprises distillation process furnace (first process furnace) 3a and condensation process furnace (second process furnace) 3b that is separated from each other, and these two process furnace 3a, 3b are separated from each other as two independent parts.Particularly, distillation process furnace 3a is different with temperature in the condensation process furnace 3b, and the temperature among the distillation process furnace 3a sublimation temperature with the metal of required purification usually is consistent, and the condensing temperature of the common metal with required purification of the temperature in the condensation process furnace is consistent.Under the situation of the metal of having determined required purification, the temperature among distillation process furnace 3a and the condensation process furnace 3b has just remained unchanged substantially.Owing to adopted this separated structures, the control of the temperature of process furnace 3 is more prone to, and can accurately control the temperature in the stove, simultaneously because two process furnace 3a and 3b structurally are isolating fully, influencing each other on therefore, can occurrence temperature between the two.
It should be noted that according to principle of the present invention, though sublimation apparatus preferably adopts horizontal type structure, also can adopt vertical structure, it can realize the required technique effect that reaches of the present invention equally.
Continuation is with reference to Fig. 2, thereby the distillation section 8a that can see distillation sleeve pipe 8 is arranged in distillation process furnace 3a is heated to the metal of required purification by distillation process furnace 3a sublimation temperature, and thereby the condensation section 8b of distillation sleeve pipe 8 is arranged in the condensation process furnace 3b process furnace 3b that is condensed and is heated to the condensing temperature of the metal of required purification, then the metal of required purification is subjected to heat sublimation in distillation section 8a, moves into condensation section 8b and then condensation-crystallization under the effect of thermograde and concentration gradient.Further, has transition zone 8c between distillation section 8a and the condensation section 8b, this transition zone 8c is distilling between process furnace 3a and the condensation process furnace 3b and is being exposed in the external environment, this is exposed to extraneous transition zone 8c can play the effect in temperature isolation district, and temperature effect between section 8a and the condensation section 8b effectively prevents to distil.
In addition, when the metal of required purification gradually when condensation is adhered to and be accumulated on the inwall of the condenser 6 that is arranged in condensation section 8b, because the sublimation apparatus that is used for purification of metals according to the present invention adopts horizontal type structure, the agglomerative metallic particles can not drop and gets back to the charging crucible 1 that is arranged in heated zones 8a owing to the effect of gravity, thereby has improved refining effect.And easier processing of horizontal type structure and assembling, structural stability is also better.Simultaneously because the assembling of horizontal type structure is more prone to realization and easier maintenance, therefore can correspondingly reduce the slit between the condensation section 8b of condenser 6 and the sleeve pipe 8 that distils, thereby can reduce of the leakage of gasiform metal, thereby can reduce the crystalline polamer of distillation sleeve pipe 8 outsides to a certain extent from the slit.
Preferably, according to the horizontal sublimation apparatus that is used for purification of metals of the present invention, the distillation section 8a of distillation sleeve pipe 8 has cylindrical outer shape, condensation section 8b have towards the distillation sleeve pipe 8 exit end 8d gradually the cone shape of chap (this exit end 8d with the outside condensing works communicate, lower boiling foreign metal will be collected in this outside condensing works).Correspondingly, the condenser 6 that is arranged among the condensation section 8b also has the structure of cone shape, and 8b is opposite with the condensation section, and the cone shape of condenser 6 is tapered towards the exit end 8d of distillation sleeve pipe 8, as shown in Figure 2.The structure of this circular cone type is in order to take out condenser 6 more easily, and the impact effect that causes of pyramidal structure helps the rapid coagulation of metal gas, and these and prior art are similar, have just repeated no more at this.
Two separate part 3a, 3b of process furnace 3 include the thermal insulation layer 4 that is in inboard flame retardant coating 5 and is in the outside, and particularly, flame retardant coating 5 is formed by refractory brick, and thermal insulation layer 4 is formed by insulating cotton.Be provided with the resistance wire 2 that is used to heat in the flame retardant coating 5, used resistance wire is the resistance wire of diameter 8mm, and the mode with high current low voltage when heating is powered to resistance wire 2.Preferably, distillation sleeve pipe 8 is made by quartz material or stainless material.
Working process according to the horizontal sublimation apparatus that is used for purification of metals of the present invention is as follows.After heating began, the temperature among the distillation section 8a was elevated to the sublimation temperature of the metal that needs purification gradually, and the temperature among the condensation section 8b is elevated to the condensing temperature (this temperature is higher than the condensing temperature of lower boiling foreign metal) of the metal that needs purification.Be heated in the process of intensification at distillation sleeve pipe 8, at first volatilize lower boiling foreign metal in the raw material in the charging crucible 1 among the distillation section 8a, the steam of this foreign metal at first enters condensation section 8b and passes this section (because the temperature among the condensation section 8b is higher than the condensing temperature of foreign metal) and then enter condensation-crystallization in the external condensation device by exit end 8d.Subsequently, when distillation section 8a reached the sublimation temperature that need purify metals, this metal just evaporated from the raw material of charging crucible 1, and then enters condensation section 8b and condensation-crystallization under thermograde and concentration gradient effect.Final residual in the crucible 1 is exactly the foreign metal that boiling point is higher than the temperature in the distillation section 8a in charging.Thereby finished purification operations to metal.
This sublimation apparatus technology is applicable to the smelting purification of multiple elemental metals such as As, Sb, Te, is applicable to commercial scale production.Being example with the production of high purity arsenic below describes the actual purification effect of horizontal sublimation apparatus of the present invention, and the processing parameter of purification and the data of concrete outcome are as follows:
Raw material: 5N arsenic (〉=99.999%)
Weight of loading: 5kg
Production cycle: 8～10h
Output product: 7N arsenic (〉=99.99999%)
Product weight: 4.80～4.96kg
Direct yield: 96%～99.2%
Quality product: adopt inductively coupled plasma mass spectrograph (ICP-MS) to detect, foreign matter content reaches 7N arsenic national standard.As shown in the table:
The final product performance that obtain show, the horizontal sublimation apparatus that is used for purification of metals according to the present invention has quite good refining effect, the quality product qualification rate can reach more than 90%, and can implement many covers and produce continuously, all operations all must carry out in strict accordance with working specification standard ground certainly.
Be the preferred embodiments of the present invention only below, be not limited to the present invention, for a person skilled in the art, the present invention can have various changes and variation.All any modifications of being done within the spirit and principles in the present invention, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. sublimation apparatus that is used for purification of metals, described sublimation apparatus comprises:
Support (7);
Process furnace (3) is supported on the described support;
Distillation sleeve pipe (8) is arranged in the described process furnace and extends through whole described process furnace along the longitudinal direction of described process furnace;
Charge cask (1) is arranged in the described distillation sleeve pipe and is arranged in described distillation telescopic first section (8a);
Condenser (6) is arranged in the described distillation sleeve pipe and is arranged in described distillation telescopic second section (8b);
It is characterized in that, described process furnace (3) comprises first process furnace (3a) and second process furnace (3b) that is separated from each other, temperature in described first process furnace and described second process furnace is different, wherein, described distillation telescopic first section is arranged in described first process furnace, described distillation telescopic second section is arranged in described second process furnace, have transition zone (8c) between described distillation telescopic first section and second section, described transition zone is between described first process furnace and second process furnace and be exposed in the external environment.
2. the sublimation apparatus that is used for purification of metals according to claim 1, it is characterized in that, the whole horizontal type structure that adopts of described sublimation apparatus, wherein, process furnace flatly is supported on the described support, described distillation sleeve water level land is arranged in the described process furnace, and described charge cask and described condenser all flatly are arranged in the described distillation sleeve pipe.
3. the sublimation apparatus that is used for purification of metals according to claim 1 and 2, it is characterized in that, described distillation telescopic first section has cylindrical shape, and described distillation telescopic second section has towards described distillation telescopic exit end (8d) cone shape of chap gradually.
4. the sublimation apparatus that is used for purification of metals according to claim 3 is characterized in that, the described condenser that is arranged in described second section has towards the tapered cone shape of described distillation telescopic exit end (8d).
5. the sublimation apparatus that is used for purification of metals according to claim 1 and 2, it is characterized in that, described process furnace comprises close described distillation telescopic flame retardant coating (5) and is centered around the thermal insulation layer (4) in the described flame retardant coating outside, is provided with resistance wire (2) in the described flame retardant coating.
6. the sublimation apparatus that is used for purification of metals according to claim 5 is characterized in that, described resistance wire is the resistance wire of diameter 8mm.
7. the sublimation apparatus that is used for purification of metals according to claim 5 is characterized in that described flame retardant coating is formed by refractory brick, and described thermal insulation layer is formed by insulating cotton.
8. the sublimation apparatus that is used for purification of metals according to claim 1 and 2 is characterized in that, described distillation sleeve pipe is made by quartz material or stainless material.
9. the sublimation apparatus that is used for purification of metals according to claim 1 is characterized in that, described charge cask is a crucible.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101808890A CN101403039B (en) | 2008-11-26 | 2008-11-26 | Sublimation apparatus for metal purification |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101808890A CN101403039B (en) | 2008-11-26 | 2008-11-26 | Sublimation apparatus for metal purification |
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| Publication Number | Publication Date |
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| CN101403039A CN101403039A (en) | 2009-04-08 |
| CN101403039B true CN101403039B (en) | 2010-09-01 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108854136B (en) * | 2018-07-20 | 2021-02-26 | 合肥欧莱迪光电技术有限公司 | Special equipment for purifying visible organic small molecules in high vacuum in open mode |
| CN108677027B (en) * | 2018-07-31 | 2024-01-05 | 核工业理化工程研究院 | Multistage evaporator for alkali metal purification and multistage evaporation method |
| CN109011679B (en) * | 2018-09-30 | 2024-05-31 | 深圳普瑞材料技术有限公司 | Collecting device for sublimation and purification of organic compound |
| CN113970240B (en) * | 2021-11-02 | 2023-11-28 | 中国铝业股份有限公司 | Vertical reduction furnace, magnesium smelting reduction rate improving method, storage medium and electronic equipment |
| CN113999981A (en) * | 2021-11-02 | 2022-02-01 | 广东先导微电子科技有限公司 | Impurity removal method for high-purity metal through vacuum sublimation |
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