CN201158692Y - Vacuum sublimation purification device of high purity arsenic - Google Patents
Vacuum sublimation purification device of high purity arsenic Download PDFInfo
- Publication number
- CN201158692Y CN201158692Y CNU2008200310756U CN200820031075U CN201158692Y CN 201158692 Y CN201158692 Y CN 201158692Y CN U2008200310756 U CNU2008200310756 U CN U2008200310756U CN 200820031075 U CN200820031075 U CN 200820031075U CN 201158692 Y CN201158692 Y CN 201158692Y
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- arsenic
- vacuum tank
- high purity
- condenser
- temperature control
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
A vacuum purification device of high purify arsenic comprises a heating furnace, a vacuum tank and a sublimating inner sleeve, wherein the tope portion of the vacuum tank is provided with a circulating water jacket, the vacuum tank on the lower side of the circulating water jacket is arranged in the heating furnace, and the sublimating inner sleeve is arranged in the vacuum tank. The sublimating inner sleeve comprises a charging crucible on the lower portion, a high purify arsenic imbedding condenser in the middle portion and a tail gas impurity condensing collector on the top portion, wherein a condensing purification ring of element with high boiling point and high melting point is arranged between the high purify arsenic imbedding condenser and the tail gas impurity condensing collector, a baffle plate is arranged between the high purify arsenic imbedding condenser and the tail gas impurity condensing collector, the tail gas impurity condensing collector is arranged in the circulating water jacket on the top portion of the vacuum tank, the heating furnace is provided with a volatilization temperature control region and an arsenic product temperature control region from up to bottom, and an elevated temperature curved line is set through the precision temperature controls. The utility model has reasonable structure, reasonable temperature gradient distribution and excellent evenness temperature filed and reproducibility, can obtain high quality product after one-time sublimation with the same raw arsenic, has excellent impurity separating and condensing effects and low purification cost.
Description
Technical field
The utility model relates to a kind of vacuum-sublimation purifying plant of non-ferrous metal metallurgy purification techniques, particularly a kind of high purity arsenic.
Background technology
Vacuum-sublimation belongs to a kind of in traditional special smelting technology, but its structure of different metals of purifying, technology condition differ greatly, and particularly the vacuum-sublimation of high purity arsenic is purified, and whether vacuum-sublimation temperature and thermograde variation be rationally extremely important.Sublimation temperature is too high or the inhomogeneous generation arsenic of transverse temperature quantity of steam is big, and gas rises to be accelerated, and too high raising speed can form carrying secretly of impurity, loses the purification effect; The longitudinal temperature irrational distribution can produce the secondary distillation and accelerate raising speed; Temperature gradient distribution is unreasonable, and impurity separating and condensing weak effect in the arsenic does not gently then have refining effect, or efficient is low, the rate of recovery is low, can cause dead stove when serious.
Summary of the invention
The technical problems to be solved in the utility model is at the deficiencies in the prior art, has proposed a kind of product purity height, the vacuum-sublimation purifying plant of the high purity arsenic of the high purity arsenic that refining effect is good.
The technical problems to be solved in the utility model is achieved through the following technical solutions, a kind of vacuum-sublimation purifying plant of high purity arsenic, be characterized in: comprise process furnace, cover in vacuum tank and the distillation, the top of vacuum tank is provided with cyclic water jacket, vacuum tank below the cyclic water jacket is arranged in the process furnace, be set in the vacuum tank in the distillation, cover comprises the charging crucible of bottom in the distillation, the high purity arsenic implantation condenser and the top tail gas impurity condensation collector at middle part, be provided with high boiling point high-melting-point element condensation cleaning ring between charging crucible and the high purity arsenic implantation condenser, be provided with barrier plate between high purity arsenic implantation condenser and the tail gas impurity condensation collector, tail gas impurity condensation collector is arranged in the cyclic water jacket at vacuum tank top, process furnace is provided with volatilization temperature control district from bottom to top, arsenic product temperature control district, two temperature control districts are provided with two independent heating units respectively, be provided with retaining Wen Huan between two heating units, charging crucible and high boiling point high-melting-point element condensation cleaning ring are arranged on volatilization temperature control district; High purity arsenic implantation condenser is arranged on arsenic product temperature control district; The cyclic water jacket of vacuum tank constitutes impurity and collects the temperature control district, and tail gas impurity condensation collector is arranged on impurity and collects the temperature control district.
The technical problem to be solved in the present invention can also come further to realize by the following technical programs, is provided with spreader plate between the top of high boiling point high-melting-point element condensation cleaning ring and high purity arsenic implantation condenser.Make arsenic steam disperse, cushion and slow down.
The technical problem to be solved in the present invention can also come further to realize by the following technical programs, is provided with at the furnace bottom of process furnace and prevents that the bottom heating unit of isolated island phenomenon from appearring in material.
The utility model compared with prior art according to the physical property of arsenic, distils in the vacuum-sublimation closed unit, and volatilization district, arsenic product zone and impurity collecting region are set, and adopts certain vacuum tightness and accurate temperature control, configures heating curve.Arsenic is under certain vacuum tightness and temperature, from crucible, be sublimed into arsenic steam, by high boiling point high-melting-point element condensation cleaning ring, stop that high boiling point and dystectic impurity enter high purity arsenic implantation condenser, arsenic steam is crystallization on high purity arsenic implantation condenser then, crystallizations such as the Zn that lower boiling S, Se and vapour pressure are bigger, Pb, Mg are in tail gas impurity condensation collector, and have part arsenic steam with the form crystallization of β-As and γ-As in tail gas impurity condensation collector, prevent that arsenic steam from carrying out tail gas and discharging contaminate environment.The present invention is rational in infrastructure, and temperature gradient distribution is reasonable, the even favorable reproducibility of warm field distribution, and the quality product height that the arsenic distillation of same materials once can reach, the impurity separating and condensing is effective, and cost for purification is low.
Description of drawings
Fig. 1 is a structure diagram of the present utility model.
Embodiment
A kind of vacuum-sublimation purifying plant of high purity arsenic, comprise process furnace 1, cover 9 in vacuum tank 2 and the distillation, the top of vacuum tank 2 is provided with cyclic water jacket 6, vacuum tank below the cyclic water jacket 6 is arranged in the process furnace 1, cover 9 is located in the vacuum tank 2 in the distillation, cover 9 comprises the charging crucible 13 of bottom in the distillation, the high purity arsenic implantation condenser 3 and the top tail gas impurity condensation collector 7 at middle part, be provided with high boiling point high-melting-point element condensation cleaning ring 11 between charging crucible 13 and the high purity arsenic implantation condenser 3, be provided with barrier plate 5 between high purity arsenic implantation condenser 3 and the tail gas impurity condensation collector 7, tail gas impurity condensation collector 7 is arranged in the cyclic water jacket 6 at vacuum tank top, the process furnace 1 white supreme down volatilization temperature control district that is provided with, arsenic product temperature control district, two temperature control districts are provided with two independent heating units 12 respectively, 8, be provided with retaining temperature ring 10 between two heating units, charging crucible 13 is arranged on volatilization temperature control district with high boiling point high-melting-point element condensation cleaning ring 11; High purity arsenic implantation condenser 3 is arranged on arsenic product temperature control district; The cyclic water jacket 6 of vacuum tank constitutes impurity and collects the temperature control district, and tail gas impurity condensation collector 7 is arranged on impurity and collects the temperature control district.Be provided with at the furnace bottom of process furnace 1 and prevent that the bottom heating unit 14 of isolated island phenomenon from appearring in material.
Between the top of high boiling point high-melting-point element condensation cleaning ring 11 and high purity arsenic implantation condenser, be provided with spreader plate 4.Make arsenic steam disperse, cushion and slow down.Be provided with barrier plate between high purity arsenic implantation condenser and the tail gas impurity condensation collector.Improve the condensation efficiency of arsenic steam, prevent that a large amount of arsenic steam is flushed to cold zone and forms β-As and γ-As, and make crystallizations such as lower boiling S, Se and vapour pressure bigger Zn, Pb, Mg in tail gas impurity condensation collector at high purity arsenic implantation condenser.
The temperature of impurity collecting region is controlled by the circulating water cooling device that is arranged on vacuum tank top, controls its temperature less than 180 ℃.
By the control of temperature and pressure, control the raising speed of arsenic steam, raising speed generally is controlled at 1～3mm/s, and the production cycle was generally 12～15 hours.
Claims (3)
1. the vacuum-sublimation purifying plant of a high purity arsenic, it is characterized in that: comprise process furnace (1), cover (9) in vacuum tank (2) and the distillation, the top of vacuum tank (2) is provided with cyclic water jacket (6), vacuum tank below the cyclic water jacket (6) is arranged in the process furnace (1), cover (9) is located in the vacuum tank (2) in the distillation, cover (9) comprises the charging crucible (13) of bottom in the distillation, the high purity arsenic implantation condenser (3) and the top tail gas impurity condensation collector (7) at middle part, be provided with high boiling point high-melting-point element condensation cleaning ring (11) between charging crucible (13) and the high purity arsenic implantation condenser (3), be provided with barrier plate (5) between high purity arsenic implantation condenser (3) and the tail gas impurity condensation collector (7), tail gas impurity condensation collector (7) is arranged in the cyclic water jacket (6) at vacuum tank top, process furnace (1) is provided with volatilization temperature control district from bottom to top, arsenic product temperature control district, two temperature control districts are provided with two independent heating units (12 respectively, 8), be provided with retaining Wen Huan (10) between two heating units, charging crucible (13) is arranged on volatilization temperature control district with high boiling point high-melting-point element condensation cleaning ring (11); High purity arsenic implantation condenser (3) is arranged on arsenic product temperature control district; The cyclic water jacket (6) of vacuum tank (2) constitutes impurity and collects the temperature control district, and tail gas impurity condensation collector (7) is arranged on impurity and collects the temperature control district.
2. the vacuum-sublimation purifying plant of high purity arsenic according to claim 1 is characterized in that: be provided with spreader plate (4) between the top of high boiling point high-melting-point element condensation cleaning ring (11) and high purity arsenic implantation condenser (3).
3. the vacuum-sublimation purifying plant of high purity arsenic according to claim 1 is characterized in that: the furnace bottom at process furnace (1) is provided with bottom heating unit (14).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNU2008200310756U CN201158692Y (en) | 2008-01-25 | 2008-01-25 | Vacuum sublimation purification device of high purity arsenic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNU2008200310756U CN201158692Y (en) | 2008-01-25 | 2008-01-25 | Vacuum sublimation purification device of high purity arsenic |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN201158692Y true CN201158692Y (en) | 2008-12-03 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNU2008200310756U Expired - Lifetime CN201158692Y (en) | 2008-01-25 | 2008-01-25 | Vacuum sublimation purification device of high purity arsenic |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101225479B (en) * | 2008-01-25 | 2010-06-02 | 郑桂昌 | Vacuum sublimation purifying method for high-purity arsenic and vacuum sublimation furnace thereof |
| CN106381469A (en) * | 2016-12-15 | 2017-02-08 | 衡阳华砷科技有限公司 | Arsenic sectional material machining method |
| CN107881351A (en) * | 2017-11-30 | 2018-04-06 | 广东先导先进材料股份有限公司 | The device for deoxidizing and method of high purity arsenic |
| CN110657669A (en) * | 2018-12-12 | 2020-01-07 | 株洲诺天电热科技有限公司 | Horizontal collecting device for two-side surfaces of solid pure object electric heating equipment |
| CN110657668A (en) * | 2018-12-12 | 2020-01-07 | 株洲诺天电热科技有限公司 | Horizontal side collecting method for solid purified substances of electric heating equipment |
| CN110671933A (en) * | 2018-12-12 | 2020-01-10 | 株洲诺天电热科技有限公司 | Method for collecting solid-state purified matter on two lateral sides of horizontal electric heating equipment |
-
2008
- 2008-01-25 CN CNU2008200310756U patent/CN201158692Y/en not_active Expired - Lifetime
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101225479B (en) * | 2008-01-25 | 2010-06-02 | 郑桂昌 | Vacuum sublimation purifying method for high-purity arsenic and vacuum sublimation furnace thereof |
| CN106381469A (en) * | 2016-12-15 | 2017-02-08 | 衡阳华砷科技有限公司 | Arsenic sectional material machining method |
| CN106381469B (en) * | 2016-12-15 | 2018-12-07 | 衡阳华砷科技有限公司 | Arsenic shape extrusion method |
| CN107881351A (en) * | 2017-11-30 | 2018-04-06 | 广东先导先进材料股份有限公司 | The device for deoxidizing and method of high purity arsenic |
| CN110657669A (en) * | 2018-12-12 | 2020-01-07 | 株洲诺天电热科技有限公司 | Horizontal collecting device for two-side surfaces of solid pure object electric heating equipment |
| CN110657668A (en) * | 2018-12-12 | 2020-01-07 | 株洲诺天电热科技有限公司 | Horizontal side collecting method for solid purified substances of electric heating equipment |
| CN110671933A (en) * | 2018-12-12 | 2020-01-10 | 株洲诺天电热科技有限公司 | Method for collecting solid-state purified matter on two lateral sides of horizontal electric heating equipment |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20081203 Effective date of abandoning: 20080125 |