CN2804120Y - Vacuum fractinal distillation purifying appts for sb - Google Patents
Vacuum fractinal distillation purifying appts for sb Download PDFInfo
- Publication number
- CN2804120Y CN2804120Y CN 200520022430 CN200520022430U CN2804120Y CN 2804120 Y CN2804120 Y CN 2804120Y CN 200520022430 CN200520022430 CN 200520022430 CN 200520022430 U CN200520022430 U CN 200520022430U CN 2804120 Y CN2804120 Y CN 2804120Y
- Authority
- CN
- China
- Prior art keywords
- condenser
- collector
- heater
- stove body
- vacuum
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Manufacture And Refinement Of Metals (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The utility model discloses a vacuum distillation and purification device for metal antimony. The device is composed of a stove body, a heating device, an evaporator, a condenser, tower plates, a vacuum chamber, a collector, a cover plate of the collector, a cooling water sleeve, an upper cover condenser and an air extraction pipe, wherein the heating device is arranged in the wall of the stove body; the evaporator is arranged on the bottom of the stove body; the collector is arranged on the upper part of the stove body; the vacuum chamber is arranged between the condenser and the stove body; the cooling water sleeve is arranged on the top of the stove body; the upper cover condenser is arranged on an upper cover of the stove body; the air extraction pipe is arranged on the central position of the upper cover condenser; the tower plates are arranged in the condenser; a condensing section is arranged between each two tower plates; the tower plates arranged in the condenser are alternately placed of large-aperture tower plates and small-aperture tower plates, and more especially, a small-aperture tower plate is arranged between two large-aperture tower plates. The device has the advantages of simple and reasonable structure, convenient manufacture and maintenance, and safe operation, and furthermore, the utility model can realize the industrialization scale production.
Description
Technical field
The utility model relates to the purifying plant of metallic antimony, more particularly, is a kind of with the purify metals device of antimony of rectification under vacuum method.
Background technology
In the prior art, vacuum distillation plant has been used for the arsenic removal and the sulphur of metallic antimony, and its method is to place copper wire and add material such as soda ash on the plumbago crucible of vacuum distilling.Form secondary pollution in this way easily, that is to say, in arsenic removal and sulphur, impurities enters again in the metallic antimony in copper wire and the soda ash, makes the purification of metallic antimony become complicated more.This is a long-term unsolved technical barrier.
Summary of the invention
The purpose of this utility model is to overcome above-mentioned shortcoming, and a kind of rectification under vacuum purifying plant of metallic antimony is provided.Use this device repeatedly vacuum distilling and other chemical substance of interpolation, the disposable Separation ﹠ Purification of finishing metallic antimony.
The purpose of this utility model is achieved by following proposal.
The utility model provides a kind of vacuum rectifying apparatus of metallic antimony, and this installs by body of heater, heating unit, and vaporizer, condenser, column plate, vacuum chamber, collector, the collector cover plate, watercooling jacket, loam cake condenser and extraction pipe are formed; Wherein, heating unit is located in the furnace body wall, and vaporizer is arranged on the bottom of body of heater, and collector is arranged on the top of body of heater, is vacuum chamber between condenser and the body of heater, and watercooling jacket places the top of body of heater; The loam cake condenser place body of heater on cover, extraction pipe is arranged on the central position of loam cake condenser; Being provided with column plate in the condenser, is a condensation segment between per two blocks of column plates.
Wherein, the column plate that is provided with in the described condenser is that wide aperture column plate and small-bore column plate are alternately placed, and promptly places a small-bore column plate between two blocks of wide aperture column plates; Described wide aperture is 0.8: 1 with the diameter ratio of crucible, and described small-bore is 0.4: 1 with the diameter ratio of crucible.
The utility model compared with prior art has following beneficial effect:
1. need not repeatedly to distill and add other chemical substance, the disposable antimony of purifying metals of energy, technology is simple, and constant product quality, purity reach more than 99.99%, save material, and have reduced energy consumption, and be free from environmental pollution;
2. purifying plant of the present utility model is simple and reasonable, and making and maintenance are all very convenient, and operational safety is reliable, can realize commercial scale production;
3. the metallic antimony of existing preparation more than 99.99%, because the equipment and materials harshness, be difficult to enlarge and produce, the unitized construction equipment that the utility model adopts, solved the technical barrier that equipment enlarges, make the single device yearly capacity reach 100 tons, be equivalent to 8～10 times of legacy equipment.The rate of recovery is brought up to more than 10～15%.
Description of drawings
Fig. 1 is the structural representation of vacuum rectifying apparatus of the present utility model.
Among the figure: 1 extraction pipe, 2 loam cake condensers, 3 watercooling jackets, 4 collector cover plates, 5 bodies of heater, 6 collectors, 7 heating units, 8 vacuum chambers, 9 column plates, 10 condensers, 11 vaporizers.
Embodiment
Describe principle of work of the present utility model and device details in detail below in conjunction with Fig. 1 and embodiment.But content of the present utility model is not limited thereto.
The ultimate principle of rectification and purification of the present utility model is: various elements are under uniform temp, has different vapour pressures, utilize the difference characteristic of vaporization temperature and condensing temperature, thereby impurity element is separated with metallic antimony reach the purification purpose, represent vaporization temperature with t, when t＜1, the impurity evaporation temperature is less than metallic antimony; When t＞1, the impurity evaporation temperature is greater than metallic antimony; When t=1, be the vaporization temperature of metallic antimony.
During the utility model work, the extraction pipe outlet is connected by the inlet of conduit with a diffusion pump, the diffusion pump outlet connects with the inlet of a vacuum mechanical pump; Industrial antimony is broken for the irregular bulk of Φ 20～Φ 40, pack into and be placed in the vaporizer of vertical vacuum rectifying furnace behind the crucible, column plate, condenser, collector and collector cover plate are put into a hand basket, again hand basket is placed in the vacuum chamber, build the vacuum cover plate; Start heating unit successively, vacuum mechanical pump and diffusion pump, evaporator temperature is controlled to be 700 ℃～800 ℃, vacuum chamber pressure is controlled to be 0.1Pa～1.0Pa, makes the metallic antimony fusion, forms the metallic antimony steam, under the effect of diffusion pump and vacuum mechanical pump, along rising on the column plate hole; Vaporization temperature is higher than the impurity of metallic antimony and stays in the crucible; Along with metallic antimony steam constantly rises, the 1st～3 condensation segment, temperature is controlled to be 500 ℃～600 ℃, and metallic antimony steam is at 2,3 sections condenser intercrystallines; The 4th condensation segment temperature is controlled to be 300 ℃～400 ℃; Metallic antimony in the steam that continues to rise is at the 4th section condenser intercrystalline; The impurity that vaporization temperature is lower than metallic antimony continues evaporation, enters collector, and the temperature of collector is controlled at 120 ℃～150 ℃, makes all crystallizations in collector of impurity steam; After the rectifying 12～18 hours, stop to heat; When treating that temperature is reduced to 100 ℃～120 ℃, the diffusion pump of stopping successively and vacuum mechanical pump are opened purging valve and vacuum chamber loam cake; In vacuum chamber, take out hand basket, in order condenser and metallic antimony are taken the packaging chamber simultaneously, gently condenser and metallic antimony are peeled off, promptly obtain grade and be the metallic antimony more than 99.99%.
350 kilograms of 1# industry antimony are broken to the irregular bulk of Φ 20～Φ 40, place in the vaporizer 11, column plate 9, condenser 10, collector 6 and collector cover plate 4 are put well successively, start heating unit 7, the temperature of vaporizer is controlled at 750 ℃, makes the fusion of metal antimony regulus, forms vapour pressure.Vacuum chamber pressure is controlled to be 1Pa.First, second and third section temperature is controlled at 550 ℃, and the 4th section temperature control is at 350 ℃.
Metallic antimony fusion evaporation, under the effect of diffusion pump and vacuum mechanical pump, the antimony steam is upwards evaporation along the column plate hole.The impurity of t＞1 that first block of wide aperture column plate will be evaporated simultaneously with antimony separates, it is stayed in the crucible, the effect of second block of small-bore column plate makes t in the steam be slightly larger than 1 impurity element further to separate, stay on first section condenser, few part metallic antimony is arranged in the first condensation segment crystallization, be subjected to temperature effect and evaporate once more with the crystallization on second and third section condenser of most antimony steam.The 4th section condenser temperature is controlled to be 350 ℃ has a spot of t to be slightly less than 1 impurity element crystallization, because temperature effect, impurity evaporates once more, enters collector, and the impurity element of t＜1 is all condensations in 120 ℃ of conditions at the collector controlled temperature.
By 15 hours rectifying, stop to heat.One, two, three condensation segment temperature are dropped to below 150 ℃, open purging valve and vacuum chamber loam cake, the hand basket in the vacuum chamber is proposed, take out collector, condenser and metallic antimony successively.First section condenser is one group; Second and third, four sections condensers are one group; Respectively two groups metallic antimony and condenser are peeled off gently, obtained two groups of metallic antimonies.
The little metal antimony that one section condenser obtains reclaims rectifying again, and two, three, four sections condensers obtain 320 kilograms of the metallic antimonies of grade 99.99%.See Table 1 with glow discharge mass spectrometry instrument detected result.
Table 1.
| The impurity title | Ag | Au* | Cd | Cu | Fe | Mg | Ni | Pb | Zn | Mn | As | S | Si | Bi |
| Content≤PPm | 0.15 | 1.2 | 2.0 | 0.1 | 1.5 | 0.04 | 0.7 | 9.0 | 4.2 | 0.5 | 9.8 | 1.3 | 3.2 | 4.8 |
* exist and disturb
Embodiment 2
Repeat embodiment 1, following difference is arranged: vacuum chamber pressure is controlled at 0.5Pa, and the 1st～3 condensation segment temperature is controlled at 600 ℃, and the 4th condensation segment temperature is controlled at 400 ℃; Obtain the metallic antimony 120 kg of grade 99.999% at 2,3 condensation segments.See Table 2 with glow discharge mass spectrometry instrument detected result.
Table 2.
| The impurity title | Ag | Au* | Cd | Cu | Fe | Mg | Ni | Pb | Zn | Mn | As | S | Si | Bi |
| Content≤PPm | 0.03 | 0.3 | 0.8 | 0.5 | 0.5 | 0.2 | 0.2 | 0.2 | 0.4 | 0.03 | 1.2 | 0.6 | 0.5 | 0.1 |
* exist and disturb
Claims (2)
1. the rectification under vacuum purifying plant of a metallic antimony, it is characterized in that this device is by body of heater (5), heating unit (7), vaporizer (11), condenser (10), column plate (9), vacuum chamber (8), collector (6), collector cover plate (4), watercooling jacket (3), loam cake condenser (2) and extraction pipe (1) are formed; Wherein, heating unit (7) is located in body of heater (5) wall, and vaporizer (11) is arranged on the bottom of body of heater (5), and collector (6) is arranged on the top of body of heater (5), be vacuum chamber (8) between condenser (10) and the body of heater (5), watercooling jacket (3) places the top of body of heater (5); Loam cake condenser (2) place body of heater (5) on cover, extraction pipe (1) is arranged on the central position of loam cake condenser; Being provided with column plate (9) in the condenser (10), is a condensation segment between per two blocks of column plates.
2. the rectification under vacuum purifying plant of metallic antimony according to claim 1, it is characterized in that the column plate (9) that is provided with in the described condenser (10) is that wide aperture column plate and small-bore column plate are alternately placed, and promptly places a small-bore column plate between two blocks of wide aperture column plates; Described wide aperture is 0.8: 1 with the diameter ratio of crucible, and described small-bore is 0.4: 1 with the diameter ratio of crucible.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200520022430 CN2804120Y (en) | 2005-04-30 | 2005-04-30 | Vacuum fractinal distillation purifying appts for sb |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200520022430 CN2804120Y (en) | 2005-04-30 | 2005-04-30 | Vacuum fractinal distillation purifying appts for sb |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN2804120Y true CN2804120Y (en) | 2006-08-09 |
Family
ID=36909416
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200520022430 Expired - Fee Related CN2804120Y (en) | 2005-04-30 | 2005-04-30 | Vacuum fractinal distillation purifying appts for sb |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN2804120Y (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108452546A (en) * | 2018-04-09 | 2018-08-28 | 昆山佳鹿石英有限公司 | Antimony purifies rectifier unit and the method using device purification antimony |
| CN111424184A (en) * | 2020-04-17 | 2020-07-17 | 包头稀土研究院 | Vacuum smelting furnace and method for preparing high-purity metal ytterbium by one-time continuous reduction distillation |
-
2005
- 2005-04-30 CN CN 200520022430 patent/CN2804120Y/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108452546A (en) * | 2018-04-09 | 2018-08-28 | 昆山佳鹿石英有限公司 | Antimony purifies rectifier unit and the method using device purification antimony |
| CN111424184A (en) * | 2020-04-17 | 2020-07-17 | 包头稀土研究院 | Vacuum smelting furnace and method for preparing high-purity metal ytterbium by one-time continuous reduction distillation |
| CN111424184B (en) * | 2020-04-17 | 2022-04-22 | 包头稀土研究院 | Method for preparing high-purity metal ytterbium by one-time continuous reduction distillation |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1295365C (en) | Vacuum recrystallization method for purifying metallic antimony and equipment thereof | |
| CN1317405C (en) | High vacuum in-situ two-step refining process for high purity material | |
| CN107574319A (en) | High purity magnesium semi-continuous distillation production method | |
| CN1059709C (en) | Method and equipment for vacuum distillation puritying metallic lithium | |
| US6805833B2 (en) | Apparatus for enhanced purification of high-purity metals | |
| CN201088871Y (en) | Vacuum sublimation purifying furnace | |
| CN1884596A (en) | Very-pure metal lithium refining and purification process | |
| CN2804120Y (en) | Vacuum fractinal distillation purifying appts for sb | |
| CN207062351U (en) | A kind of vacuum drying oven of two sections of distillations | |
| CN108069828A (en) | A kind of production biodiesel byproduct crude glycerin high-purity purification technique | |
| CN200967833Y (en) | Special equipment for super-pure metal lithium refining purification technique | |
| CN1260380C (en) | Method for removing sodium from coarse lithium by gas agitation under condition of vacuum, distillation at moderate temperature | |
| CN101225479A (en) | Vacuum sublimation purifying method for high-purity arsenic and vacuum sublimation furnace thereof | |
| CN209548746U (en) | A kind of Novel benzene removing tower | |
| CN117298634A (en) | Vacuum distillation device for preparing high-purity metal by air extraction type gradient condensation | |
| JPH06108175A (en) | Refining method for crude zinc and its device | |
| CN214913498U (en) | Fractionating equipment | |
| CN107218809A (en) | A kind of many metal distillation temperature control condensed components evaporate single crude product vacuum drying oven | |
| CN207062352U (en) | A kind of vacuum drying oven of two sections of distillations multi-stage condensing | |
| CN2225006Y (en) | Vacuum distillating furnace for treating alloy with high lead content and low tin content | |
| CN115976340B (en) | Device and method for separating antimony from crude arsenic by vacuum distillation | |
| CN1791555A (en) | Method and device for treating water | |
| CN101886181A (en) | Vacuum distillation purification furnace for metal lithium | |
| CN2748444Y (en) | Water distilling tower for injection | |
| CN211896471U (en) | Acid effluent treatment plant is smelted to tombarthite |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20060809 Termination date: 20100430 |