CN104513905A - High-purity antimony vacuum distillation equipment and preparation process thereof - Google Patents
High-purity antimony vacuum distillation equipment and preparation process thereof Download PDFInfo
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- CN104513905A CN104513905A CN201510008863.8A CN201510008863A CN104513905A CN 104513905 A CN104513905 A CN 104513905A CN 201510008863 A CN201510008863 A CN 201510008863A CN 104513905 A CN104513905 A CN 104513905A
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- antimony
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Abstract
The invention discloses high-purity antimony vacuum distillation equipment and a preparation process thereof. The high-purity antimony vacuum distillation equipment comprises a cooling water circulating device, a distillation tank, a crucible, a heat insulation layer, a diffusion pump, a mechanical pump and an electrical control system; a plurality of layers of graphite tower trays are arranged in the distillation tank; the electrical control system is used for controlling and completing data acquisition and processing of a line, parameter setting and the like through a PID (Proportion Integration Differentiation) regulating instrument. The high-purity antimony vacuum distillation equipment and the preparation process thereof have the advantages of simple process, low equipment investment, high simplicity, good convenience and safety in operation, low processing cost, stable product quality and improved yield of a single furnace, and the temperature control adopts intelligent equipment, so that the product consistence is good.
Description
Technical field
The present invention relates to high pure metal field of smelting, be specifically related to a kind of high purity antimony vacuum distillation plant and preparation technology thereof.
Background technology
At present, most of high purity antimony adopts pyrometallurgical smelting, and its scale is large, labour intensive, and severe by production environment, the impact of the purity of chemical reagent, its product purity is lower.In recent years, vacuum distillation method makes metallic substance purification & isolation be simplified to physical process by traditional chemical process, product purity is high and come into one's own, but the equipment and process method of existing vacuum distillation method purification high purity antimony, existence yields poorly, temperature control and pressure-controlling are accurate not, the problem that quality product is not high.
Summary of the invention
For the technical problem that solves the problem, the invention provides a kind of Large Copacity antimony vacuum distillation plant and preparation technology.
A kind of high purity antimony vacuum distillation plant, comprises cooling water circulating device, retort, crucible, thermal insulation layer, diffusion pump, mechanical pump, electrical control system; It is characterized in that, in retort, set gradually crucible, tower tray, condenser, low-temperature collectors from the bottom up; Described and separated by tower tray between condenser and crucible; Separated by stainless steel cover plate between described condenser and low-temperature collectors, in the middle of cover plate, be provided with circular port; Resistance heading furnace, retort, crucible, condenser, cryogenic collector room, tower tray form antimony distilling furnace jointly.
As preferably, antimony distilling furnace heating region is divided into three sections, to be temperature be respectively the heating zone of 720 DEG C ~ 750 DEG C, and temperature is the condensing zone of 350 DEG C ~ 400 DEG C, and temperature is 200 DEG C ~ 260 DEG C.
As preferably, the tower tray number of plies >=2, the material selection graphite of tower tray.
As preferably, electrical control system is connected with diffusion pump, mechanical pump, antimony distilling furnace by body, common formation vacuum distilling unit, data sampling and processing and the parameter setting of electric control system controls vacuum distilling unit are completed by Intelligent PID controller, do not rely on the feature such as system mathematical models and the on-line automatic adjustment of controller parameter, to system parameter variations, there is good adaptability, so temperature error scope is little, level of automation is high.
As preferably, retort is made up of stainless steel, and diameter is 300 ~ 350mm, and crucible is made up of quartz, and diameter is 250 ~ 300mm, can load 50 ~ 60kg raw material, and high purity antimony output is 40 ~ 50kg/ stove, and condenser is made up of quartz.
As preferably, the vacuum tightness of retort and vacuum distilling unit is 10
-3~ 10
-4pa, the maximum vacuum of vacuum system can reach 1.3 × 10
-4pa.
As preferably, adopt high purity antimony vacuum distillation plant to prepare the technique of high purity antimony, comprise the following steps:
Before A, distillation, crucible, tower tray, condenser washing lotion are rinsed after soaking, and are then placed on drying for standby in loft drier;
B, 0# ~ 2# industry antimony is broken into fritter, load in crucible, the amount of loading, at 50 ~ 60kg, vacuumizes system before heating, and vacuum tightness reaches 10
-3~ 10
-4during Pa, start to be warming up to required temperature;
C, distillation terminate, and turn off power supply and diffusion pump, after continuing to vacuumize 30 minutes, are turned off by the piston connecting antimony distilling furnace and vacuum distilling unit, and then diffusion pump is connected piston with mechanical pump is communicated with air, finally close mechanical pump.
After still-process completes, lower boiling impurity is condensate in collector, and high boiling impurity rests in crucible, reaches the object of purification antimony.
In vacuum process, preferred Heating temperature is 700 DEG C ~ 750 DEG C, and vacuum tightness is 10-3 ~ 10-4Pa, fully can take out various high low melting point difficulty point foreign metal in base metal, thus reaches the object that material purifies, the purity of metallic antimony can reach >=and 99.99%.
Beneficial effect of the present invention, comprises following several aspect:
(1) technique is simple, and facility investment is few, safety simple to operate;
(2) tooling cost is low, steady quality;
(3) product production is large, and product purity is high, can meet the needs of large-scale commercial production;
(4) temperature controls to adopt intelligent PID adjusting apparatus to complete, good product consistency.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
In figure: 1-resistance heading furnace, 2-retort, 3-tower tray, 4-condenser, 5-low-temperature collectors, 6-crucible, 7-cooling water recirculation system, 8-thermal insulation layer, 9-diffusion pump, 10-mechanical pump, 11-electrical control system.
Embodiment
As shown in Figure 1, high purity antimony vacuum distillation plant comprises: cooling water circulating device (7), retort (2), crucible (6), thermal insulation layer (8), diffusion pump (9), mechanical pump (10), electrical control system (11); Crucible (6), tower tray (3), condenser (4), low-temperature collectors (5) is set gradually from the bottom up in retort (2); Separated by tower tray (3) between condenser (4) and crucible (6); Separated by stainless steel cover plate between condenser (4) and low-temperature collectors (5); Resistance heading furnace (1), retort (2), crucible (6), condenser (4), cryogenic collector room (5), tower tray (3) be composition antimony distilling furnace jointly.
Antimony distilling furnace heating region is divided into three sections, to be temperature be respectively the heating zone of 720 DEG C ~ 750 DEG C, and temperature is the condensing zone of 350 DEG C ~ 400 DEG C, and temperature is 200 DEG C ~ 260 DEG C.
Tower tray (3) is for two-layer, and electrical control system (11) is connected with diffusion pump (9), mechanical pump (10), antimony distilling furnace by body, and common formation vacuum distilling unit, the vacuum tightness of retort (2) and vacuum distilling unit is 10
-3~ 10
-4pa.
Data sampling and processing and the parameter setting of electric control system controls vacuum distilling unit are completed by Intelligent PID controller.
Prepare high purity antimony vacuum distilling technique, comprise the steps:
Before A, distillation, crucible (6), tower tray (3), condenser (4) rinse after soaking by washing lotion, are then placed on drying for standby in loft drier;
B, 1# industry antimony is broken into fritter, load in crucible (6), the amount of loading, at 55kg, vacuumizes system before heating, and vacuum tightness reaches 1.5 × 10
-4during Pa, start to be warming up to required temperature;
C, distillation terminate, turn off power supply and diffusion pump (9), after continuing to vacuumize 30 minutes, the piston connecting antimony distilling furnace and vacuum distilling unit is turned off, and then diffusion pump (9) is connected piston with mechanical pump (10) is communicated with air, finally close mechanical pump (10).
After vacuum distilling technique terminates, taken out from condenser by the industrial antimony after purifying, detect, the antimony after purifying after tested meets 4N antimony standard.
Table 1.4N antimony standard
Above-mentioned embodiment is intended to illustrate that the present invention can be professional and technical personnel in the field and realizes or use; modifying to above-mentioned embodiment will be apparent for those skilled in the art; therefore the present invention includes but be not limited to above-mentioned embodiment; any these claims or specification sheets of meeting describes; meet and principle disclosed herein and novelty, the method for inventive features, technique, product, all fall within protection scope of the present invention.
Claims (10)
1. a high purity antimony vacuum distillation plant, comprises cooling water circulating device (7), retort (2), crucible (6), thermal insulation layer (8), diffusion pump (9), mechanical pump (10), electrical control system (11); It is characterized in that, in described retort (2), set gradually crucible (6), tower tray (3), condenser (4), low-temperature collectors (5) from the bottom up; Described and separated by tower tray (3) between condenser (4) and crucible (6); Separated by stainless steel cover plate between described condenser (4) and low-temperature collectors (5); Described resistance heading furnace (1), retort (2), crucible (6), condenser (4), cryogenic collector room (5), tower tray (3) be composition antimony distilling furnace jointly.
2. a kind of high purity antimony vacuum distillation plant according to claim 1, it is characterized in that: described antimony distilling furnace heating region is divided into three sections, to be temperature be respectively the heating zone of 720 DEG C ~ 750 DEG C, temperature is the condensing zone of 350 DEG C ~ 400 DEG C, and temperature is 200 DEG C ~ 260 DEG C.
3. a kind of high purity antimony vacuum distillation plant according to claim 1, is characterized in that: described tower tray (3) number of plies >=2.
4. a kind of high purity antimony vacuum distillation plant according to claim 1 or 3, is characterized in that: the material of described tower tray (3) adopts graphite.
5. a kind of high purity antimony vacuum distillation plant according to claim 1, is characterized in that: described electrical control system (11) is connected with diffusion pump (9), mechanical pump (10), antimony distilling furnace by body, jointly forms vacuum distilling unit.
6. a kind of high purity antimony vacuum distillation plant according to claim 1 or 5, is characterized in that: data sampling and processing and the parameter setting of described electric control system controls vacuum distilling unit are completed by Intelligent PID controller.
7. a kind of high purity antimony vacuum distillation plant according to claim 1, it is characterized in that: described retort (2) is made up of stainless steel, diameter is 300 ~ 350mm.
8. a kind of high purity antimony vacuum distillation plant according to claim 1, it is characterized in that: described crucible (6) is made up of quartz, diameter is 250 ~ 300mm, and described condenser (4) is made up of quartz.
9. a kind of high purity antimony vacuum distillation plant according to claim 1 or 5, is characterized in that: the vacuum tightness of described retort (2) and vacuum distilling unit is 10
-3~ 10
-4pa.
10. adopt a kind of high purity antimony vacuum distillation plant described in claim 1 or 5 to prepare the technique of high purity antimony, it is characterized in that comprising the following steps:
Before distillation, crucible (6), tower tray (3), condenser (4) rinse after soaking by washing lotion, are then placed on drying for standby in loft drier;
0# ~ 2# industry antimony is broken into fritter, and load in crucible (6), the amount of loading, at 50 ~ 60kg, vacuumizes system before heating, and vacuum tightness reaches 10
-3~ 10
-4during Pa, start to be warming up to required temperature;
Distillation terminates, turn off power supply and diffusion pump (9), after continuing to vacuumize 30 minutes, the piston connecting antimony distilling furnace and vacuum distilling unit is turned off, and then diffusion pump (9) is connected piston with mechanical pump (10) is communicated with air, finally close mechanical pump (10).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510008863.8A CN104513905B (en) | 2015-01-08 | 2015-01-08 | High-purity antimony vacuum distillation equipment and preparation process thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510008863.8A CN104513905B (en) | 2015-01-08 | 2015-01-08 | High-purity antimony vacuum distillation equipment and preparation process thereof |
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| CN104513905A true CN104513905A (en) | 2015-04-15 |
| CN104513905B CN104513905B (en) | 2017-01-18 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107640749A (en) * | 2017-09-14 | 2018-01-30 | 成都汉普高新材料有限公司 | A kind of high-purity tellurium dioxide and preparation method thereof |
| CN108950242A (en) * | 2018-07-10 | 2018-12-07 | 成都中建材光电材料有限公司 | A kind of preparation facilities of high purity zinc |
| CN113249573A (en) * | 2021-07-13 | 2021-08-13 | 赣州中新矿业有限公司 | Recovery unit of tungsten and cobalt in cobalt alloy waste material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1687469A (en) * | 2005-04-30 | 2005-10-26 | 云南省通海大方科技有限公司 | Vacuum recrystallization method for purifying metallic antimony and equipment thereof |
| CN101062764A (en) * | 2006-04-29 | 2007-10-31 | 成都汉普高新材料有限公司 | Tellurium retort |
| CN101565781A (en) * | 2008-12-10 | 2009-10-28 | 株洲科迪亚实业有限公司 | Method and device for producing high-purity antimony |
-
2015
- 2015-01-08 CN CN201510008863.8A patent/CN104513905B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1687469A (en) * | 2005-04-30 | 2005-10-26 | 云南省通海大方科技有限公司 | Vacuum recrystallization method for purifying metallic antimony and equipment thereof |
| CN101062764A (en) * | 2006-04-29 | 2007-10-31 | 成都汉普高新材料有限公司 | Tellurium retort |
| CN101565781A (en) * | 2008-12-10 | 2009-10-28 | 株洲科迪亚实业有限公司 | Method and device for producing high-purity antimony |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107640749A (en) * | 2017-09-14 | 2018-01-30 | 成都汉普高新材料有限公司 | A kind of high-purity tellurium dioxide and preparation method thereof |
| CN107640749B (en) * | 2017-09-14 | 2020-11-27 | 成都汉普高新材料有限公司 | High-purity tellurium dioxide and preparation method thereof |
| CN108950242A (en) * | 2018-07-10 | 2018-12-07 | 成都中建材光电材料有限公司 | A kind of preparation facilities of high purity zinc |
| CN108950242B (en) * | 2018-07-10 | 2021-04-06 | 成都中建材光电材料有限公司 | Preparation device of high-purity zinc |
| CN113249573A (en) * | 2021-07-13 | 2021-08-13 | 赣州中新矿业有限公司 | Recovery unit of tungsten and cobalt in cobalt alloy waste material |
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|---|---|
| CN104513905B (en) | 2017-01-18 |
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