CN104513905B - 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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- CN104513905B CN104513905B CN201510008863.8A CN201510008863A CN104513905B CN 104513905 B CN104513905 B CN 104513905B CN 201510008863 A CN201510008863 A CN 201510008863A CN 104513905 B CN104513905 B CN 104513905B
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- high purity
- antimony
- purity antimony
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P10/00—Technologies related to metal processing
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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 and in particular to a kind of high purity antimony vacuum distillation plant and its preparation work
Skill.
Background technology
At present, most of high purity antimonies adopt pyrometallurgical smelting, and its scale is big, labour intensive, severe by production environment, chemistry examination
The impact of the purity of agent, its product purity is than relatively low.In recent years, vacuum distillation method makes metal material purification ＆ isolation by traditional change
Learn process simplification and become physical process, product purity is high and be taken seriously, but existing vacuum distillation method purifies setting of high purity antimony
Standby and process, exists and yields poorly, temperature control and Stress control are not accurate, the not high problem of product quality.
Content of the invention
For the technical problem that solves the above problems, the invention provides a kind of Large Copacity antimony vacuum distillation plant and preparation work
Skill.
A kind of high purity antimony vacuum distillation plant, including cooling water circulating device, alembic, crucible, heat-insulation layer, diffusion pump,
Mechanical pump, electric-control system；It is characterized in that, set gradually crucible, tower tray, condenser, cryogenic collector in alembic from the bottom up
Device；Described separated by tower tray and condenser and crucible between；Pass through stainless steel cover between described condenser and low-temperature collectors
Plate separates, and is provided with circular port in the middle of cover plate；Resistance-heated furnace, alembic, crucible, condenser, cryogenic collector room, common group of tower tray
Become antimony retort.
Preferably, antimony retort is heated divides into three sections, it is the thermal treatment zone that temperature is 720 DEG C～750 DEG C respectively, temperature
For 350 DEG C～400 DEG C of condensing zone, temperature is 200 DEG C～260 DEG C.
Preferably, the tower tray number of plies >=2, the material selection graphite of tower tray.
Preferably, electric-control system passes through body and diffusion pump, mechanical pump, antimony retort connect, collectively form vacuum and steam
Evaporate unit, the data sampling and processing of electric control system controls vacuum distilling unit and parameter setting are complete by intelligent pid adjusting apparatus
Become, be independent of the features such as system mathematical models and controller parameter on-line automatic adjustment, system parameter variations are had relatively
Good adaptability, so temperature error scope is little, high degree of automation.
Preferably, alembic is made of stainless steel, a diameter of 300～350mm, crucible is made up of quartz, and a diameter of 250
～300mm, can load 50～60kg raw material, and high purity antimony yield is 40～50kg/ stove, and condenser is made up of quartz.
Preferably, the vacuum of alembic and vacuum distilling unit is 10-3～10-4Pa, the highest vacuum of vacuum system
Degree is up to 1.3 × 10-4pa.
Preferably, prepare the technique of high purity antimony using high purity antimony vacuum distillation plant, comprise the following steps:
Before a, distillation, crucible, tower tray, condenser washing liquid are rinsed after soaking, and are then placed within being dried in drying baker
Standby；
B, 0#～2# industry antimony is broken into fritter, loads in crucible, the amount of loading in 50～60kg, before heating to being
System carries out evacuation, and vacuum reaches 10-3～10-4During pa, start to warm up to required temperature；
C, distillation terminate, and power off and diffusion pump, after continuing evacuation 30 minutes, will connect antimony retort and vacuum
The piston of distillation unit is turned off, and then again diffusion pump is connected piston connection air with mechanical pump, finally closes mechanical pump.
After the completion of still-process, lower boiling impurity is condensate in catcher, and high boiling impurity rests in crucible, reaches
Purpose to purification antimony.
In vacuum process, preferred heating-up temperature is 700 DEG C～750 DEG C, and vacuum is 10-3～10-4pa, can fully take
Go out difficult point of foreign metals of various high low melting points in base metal, thus reaching the purpose of material purification, the purity of metallic antimony up to
≥99.99%.
Beneficial effects of the present invention, including following aspects:
(1) process is simple, equipment investment is few, safety simple to operate；
(2) processing cost is low, steady quality；
(3) product yield is big, and product purity is high, disclosure satisfy that the needs of large-scale industrial production；
(4) temperature control is completed using intelligent pid adjusting apparatus, good product consistency.
Brief description
Fig. 1 is the structural representation of the present invention.
In figure: 1- resistance-heated furnace, 2- alembic, 3- tower tray, 4- condenser, 5- low-temperature collectors, 6- crucible, 7- cooling
Water circulation system, 8- heat-insulation layer, 9- diffusion pump, 10- mechanical pump, 11- electric-control system.
Specific embodiment
As shown in figure 1, high purity antimony vacuum distillation plant includes: cooling water circulating device (7), alembic (2), crucible (6),
Heat-insulation layer (8), diffusion pump (9), mechanical pump (10), electric-control system (11)；Alembic sets gradually crucible in (2) from the bottom up
(6), tower tray (3), condenser (4), low-temperature collectors (5)；Separated by tower tray (3) between condenser (4) and crucible (6)；Cold
Separated by rustless steel cover plate between condenser (4) and low-temperature collectors (5)；Resistance-heated furnace (1), alembic (2), crucible (6),
Condenser (4), cryogenic collector room (5), tower tray (3) collectively constitute antimony retort.
Antimony retort is heated and is divided into three sections, is the thermal treatment zone that temperature is 720 DEG C～750 DEG C respectively, temperature be 350 DEG C～
400 DEG C of condensing zone, temperature is 200 DEG C～260 DEG C.
Tower tray (3) is two-layer, and electric-control system (11) passes through body and diffusion pump (9), mechanical pump (10), antimony retort connect
Connect, collectively form vacuum distilling unit, the vacuum of alembic (2) and vacuum distilling unit is 10-3～10-4pa.
The data sampling and processing of electric control system controls vacuum distilling unit and parameter setting are complete by intelligent pid adjusting apparatus
Become.
Prepare high purity antimony vacuum distilling technique, comprise the steps:
Before a, distillation, crucible (6), tower tray (3), condenser (4) are rinsed with after washing liquid immersion, are then placed within drying
Drying for standby in case；
B, 1# industry antimony is broken into fritter, loads in crucible (6), the amount of loading, in 55kg, is entered to system before heating
Row evacuation, vacuum reaches 1.5 × 10-4During pa, start to warm up to required temperature；
C, distillation terminate, and power off and diffusion pump (9), after continuing evacuation 30 minutes, will connect antimony retort with
The piston of vacuum distilling unit is turned off, and then again diffusion pump (9) is connected piston connection air with mechanical pump (10), finally closes
Mechanical pump (10).
After vacuum distilling technique terminates, the industrial antimony after purification is taken out from condenser, is detected, purify after tested
Antimony afterwards meets 4n antimony standard.
Table 1.4n antimony standard
It can be professional and technical personnel in the field's realization or use that above-mentioned embodiment is intended to illustrate the present invention, to above-mentioned
Embodiment is modified and be will be apparent from for those skilled in the art, therefore the present invention includes but is not limited to
Above-mentioned embodiment, any meet the claims or description description, meet with principles disclosed herein and novelty,
The method of inventive features, technique, product, each fall within protection scope of the present invention.
Claims (8)
1. the technique of high purity antimony is prepared it is characterised in that comprising the following steps using a kind of high purity antimony vacuum distillation plant:
Before a, distillation, crucible (6), tower tray (3), condenser (4) are rinsed with after washing liquid immersion, are then placed within drying baker
Drying for standby；
B, 0#～2# industry antimony is broken into fritter, loads in crucible (6), the amount of loading in 50～60kg, before heating to being
System carries out evacuation, and vacuum reaches 10-3～10-4During pa, start to warm up to required temperature；
C, distillation terminate, and power off and diffusion pump (9), after continuing evacuation 30 minutes, will connect antimony retort and vacuum
The piston of distillation unit is turned off, and then again diffusion pump (9) is connected piston connection air with mechanical pump (10), finally closes machinery
Pump (10)；
Described high purity antimony vacuum distillation plant, comprising: cooling water circulating device (7), alembic (2), crucible (6), heat-insulation layer
(8), diffusion pump (9), mechanical pump (10), electric-control system (11)；It is characterized in that, in described alembic (2) from the bottom up successively
Setting crucible (6), tower tray (3), condenser (4), low-temperature collectors (5)；Pass through tower between described condenser (4) and crucible (6)
Disk (3) separates；Separated by rustless steel cover plate between described condenser (4) and low-temperature collectors (5)；Resistance-heated furnace (1), steaming
Evaporate tank (2), crucible (6), condenser (4), cryogenic collector room (5), tower tray (3) collectively constitute antimony retort；Electric-control system passes through
Body and diffusion pump, mechanical pump, antimony retort connect, and collectively form vacuum distilling unit.
2. the technique preparing high purity antimony using a kind of high purity antimony vacuum distillation plant according to claim 1, its feature exists
In, described antimony retort is heated and is divided into three sections, is the thermal treatment zone that temperature is 720 DEG C～750 DEG C respectively, temperature be 350 DEG C～
400 DEG C of condensing zone, temperature is 200 DEG C～260 DEG C.
3. the technique preparing high purity antimony using a kind of high purity antimony vacuum distillation plant according to claim 1, its feature exists
In described tower tray (3) number of plies >=2.
4. the technique preparing high purity antimony using a kind of high purity antimony vacuum distillation plant according to claim 1 or 3, its feature
It is, the material of described tower tray (3) adopts graphite.
5. the technique preparing high purity antimony using a kind of high purity antimony vacuum distillation plant according to claim 1, its feature exists
Pass through intelligent pid adjusting apparatus in, the data sampling and processing of described electric control system controls vacuum distilling unit and parameter setting complete
Become.
6. the technique preparing high purity antimony using a kind of high purity antimony vacuum distillation plant according to claim 1, its feature exists
In described alembic (2) is made of stainless steel, a diameter of 300～350mm.
7. the technique preparing high purity antimony using a kind of high purity antimony vacuum distillation plant according to claim 1, its feature exists
In described crucible (6) is made up of quartz, a diameter of 250～300mm, and described condenser (4) is made up of quartz.
8. the technique preparing high purity antimony using a kind of high purity antimony vacuum distillation plant according to claim 1 or 6, its feature
It is, the vacuum of described alembic (2) and vacuum distilling unit is 10-3～10-4pa.
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| Application Number | Priority Date | Filing Date | Title |
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| 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 |
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| 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 CN104513905A (en) | 2015-04-15 |
| CN104513905B true CN104513905B (en) | 2017-01-18 |
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| 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 |
| 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 |
| CN113249573B (en) * | 2021-07-13 | 2022-08-09 | 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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| CN1295365C (en) * | 2005-04-30 | 2007-01-17 | 云南省通海大方科技有限公司 | Vacuum recrystallization method for purifying metallic antimony and equipment thereof |
| CN101062764B (en) * | 2006-04-29 | 2011-08-17 | 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 |
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