CN203683627U - High-purity calcium vacuum distillation purifying device - Google Patents
High-purity calcium vacuum distillation purifying device Download PDFInfo
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- CN203683627U CN203683627U CN201420001685.7U CN201420001685U CN203683627U CN 203683627 U CN203683627 U CN 203683627U CN 201420001685 U CN201420001685 U CN 201420001685U CN 203683627 U CN203683627 U CN 203683627U
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- vacuum
- cold plate
- bell
- reaction tank
- distillation
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- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 54
- 239000011575 calcium Substances 0.000 title claims abstract description 54
- 238000005292 vacuum distillation Methods 0.000 title claims abstract description 20
- 238000004821 distillation Methods 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 238000009792 diffusion process Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000000746 purification Methods 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 239000011651 chromium Substances 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 238000007747 plating Methods 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 12
- 239000002184 metal Substances 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 6
- 238000001816 cooling Methods 0.000 abstract 1
- 239000012535 impurity Substances 0.000 description 9
- 239000002994 raw material Substances 0.000 description 9
- 238000009835 boiling Methods 0.000 description 7
- 238000010025 steaming Methods 0.000 description 5
- 150000002739 metals Chemical class 0.000 description 4
- 230000002829 reductive effect Effects 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- 239000000498 cooling water Substances 0.000 description 3
- 238000007872 degassing Methods 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000001883 metal evaporation Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000006200 vaporizer Substances 0.000 description 1
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The utility model discloses a high-purity calcium vacuum distillation purifying device. The device comprises a heating furnace, a distillation reaction tank in the heating furnace, a crucible placed at the bottom of the distillation reaction tank and a crucible cover with holes; the crude calcium is placed in the crucible, the upper end of the distillation reaction tank is provided with a de-vacuum pipeline for connecting the vacuum system and a reaction tank furnace cover with a section shape in an inverted convex shape, the top of the furnace cover is provided with a water-cooling sleeve, the convex surface lower end of the furnace cover is provided with a condensing plate, the outer edge of the condensing plate exposed to the convex surface lower end of the furnace cover is uniformly distributed with a plurality of holes. The vacuum system of the distillation device adopts the combination of rotary vane mechanical pump and oil diffusion pump. The device has the characteristics of being simple in structure, good in separating effect and easy to maintain. Compared with the existing device, the distillation speed is table, the product purity is high, the batch quality is table, and the obtained metal calcium is high in activity.
Description
Technical field
The utility model relates to a kind of high-purity calcium vacuum distillation purification device, belongs to metal vacuum distilation technical field.
Background technology
In numerous high-purity rare rare earth metal preparations, high-purity calcium is as desirable reductive agent, and its purity directly affects the purity of products obtained therefrom, and then affects its final use properties.Particularly, in the manufacture of some nuclear matter, high-purity calcium has indispensable status especially.At present, domestic high-purity calcium is because its water distilling apparatus structure, selection and technique is unreasonable, and often purity is not high, and batch products quality is unstable, has to depend on high price import, and is restricted.In view of this, spy develops and discloses a kind of high-purity calcium vacuum distillation plant.
Utility model content
The utility model is for domestic existing high-purity calcium product purity is not high at present, and the unsettled shortcoming of batch products quality, and a kind of high-purity calcium vacuum distillation purification device is provided.This device is not limited to the vacuum distilling of high-purity calcium and purifies, and is equally applicable to vacuum distilling other metals of purifying.
A kind of high-purity calcium vacuum distillation purification device, this device comprises distillation reaction tank in process furnace, process furnace, is placed on the crucible of distillation reaction pot bottom and crucible cover with holes, thick calcium is positioned in crucible, described distillation reaction tank upper end arranges in order to connect the vacuum-lines that goes of vacuum system, and the retort bell of cross-sectional shape for falling " protruding " shape, wherein, " protruding " shape bell top arranges water jacket, be provided with cold plate falling the convex surface lower end of " protruding " shape bell, cold plate is exposed on the outer of outside, bell convex surface lower end and is uniformly distributed some apertures.
Described process furnace is two sections of process furnace that adopt resistance wire indirect heating, have heat insulation function.
The vacuum system of described water distilling apparatus adopts the combination of rotary vane mechanical pump and oil diffusion pump, the vacuum system of going vacuum-lines to connect is made up of two stage pump, and primary pump is rotary vane mechanical pump, and two stage pump is oil diffusion pump.
The outer of described cold plate is uniformly distributed some apertures, and small aperture is not less than 10mm, and little hole number is not less than 16.
On described crucible cover, be uniformly distributed some apertures, small aperture is not less than 10mm, and little hole number is not less than 20.
Described cold plate external diameter is slightly less than furnace wall internal diameter, is not more than 3mm with the difference of furnace wall internal diameter.
The external diameter of described bell convex surface lower end is less than cold plate external diameter, and is not less than 50mm with the difference of cold plate external diameter.
Between distillation reaction tank and retort bell, be provided with sealing-ring, the water jacket that bell top arranges in order to protect sealing-ring, maintains the low-temperature condition of bell lower surface, in order to collect lower boiling, high saturated vapor pressure impurity simultaneously.
Described retort bell and distillation reaction tank material are stainless steel, and all take inwall chromium plating processing; Described crucible, crucible cover and cold plate material are High-Purity Molybdenum.
Cold plate is in order to collect major metal.Cold plate outer is uniformly distributed a series of apertures, and in still-process, lower boiling, high saturated vapor pressure impurity will finally be condensate in bell lower surface place through set aperture.The effect of crucible cover is to reduce the vaporator rate of metal, guarantees carrying out smoothly of distillation.
Adopt the utility model device to carry out high-purity calcium vacuum distilling and purify, comprise following steps:
1) system Pressure Rise Rate test: guarantee that system Pressure Rise Rate is 0.6Pa/h; As higher in system Pressure Rise Rate, need water distilling apparatus to hunt leak.
2) shove charge: in the kiln environment of humidity < 2%, the lower shove charge of Ar gas protection, and lift to process furnace; Temperature is room temperature;
3) dehydration degasification: connect vacuum system, open rotary vane mechanical pump and cooling water recirculation system, as system vacuum degree <10Pa, and oil diffusion pump heating is while exceeding 40 minutes, opens oil diffusion pump; When showing on vacuumometer that vacuum tightness reaches 10
-3～10
-2when Pa, close vacuum butterfly valve, and process furnace upper-lower section resistance wire is switched on simultaneously; Control electric current and make retort temperature in 1 hour, rise to 200 ℃, and be incubated 0.5 hour in the time of 200 ℃, remove the adsorbable gas of apparatus surface and some volatile substances;
4) fore-distillation: continue energising heating, make process furnace hypomere and epimere temperature all rise to 700 ℃, make the volatilization of lower boiling in thick calcium, high saturation vapour pressure impurity, and be condensate on bell lower surface through the set aperture in cold plate outer;
5) distillation: close process furnace epimere heating current, adopt the mode of air-cooled temperature control to make epimere temperature be reduced to 550～600 ℃, the heating of hypomere continuation simultaneously makes its temperature rise to 850 ℃, makes calcium metal evaporation, and is condensate on cold plate;
6) come out of the stove: after still-process finishes, cut off process furnace resistance wire power supply, water distilling apparatus is naturally cooled to after room temperature, in water distilling apparatus retort, pass into Ar gas to concora crush, and whole water distilling apparatus is transported in the kiln environment that temperature is room temperature, humidity < 2% and is come out of the stove.
In described fore-distillation step, the amount of steaming is controlled at 5～10wt.% of the thick calcium of raw material.
In described distilation steps, the amount of steaming is controlled at 80～90wt.% of the thick calcium of raw material.
The utlity model has apparatus structure simple, be easy to safeguard, good separating effect, and the advantage such as batch steady quality.Adopt high-purity calcium vacuum distillation purification device of the present utility model, by a vacuum distilling, can obtain that purity reaches 99.998%, calcium activity reaches high-purity calcium of 99.5%, compared with existing apparatus, the utility model distillation rate is stable, product purity is high, batch products steady quality, gained calcium metal activity are high.In addition, vacuum distillation purification device of the present utility model is not limited to the purification of high-purity calcium, and the vacuum distilling that is equally applicable to other metals is purified.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the high-purity calcium vacuum distillation plant of the utility model.
Fig. 2 is the schematic diagram of the utility model crucible cover.
Fig. 3 is the schematic diagram of the utility model cold plate.
Main Reference numeral:
1 water jacket 2 sealing-rings
3 bell lower surface 4 cold plates
5 distillation reaction tank 6 crucible covers
7 thick calcium 8 crucibles
9 process furnace 10 remove vacuum-lines
Embodiment
Below in conjunction with accompanying drawing, the utility model is described in further detail:
As shown in Figure 1, the high-purity calcium vacuum distillation purification device of the utility model, comprise adopt resistance wire indirect heating, there is distillation reaction tank 5, the crucible 8 that is placed on distillation reaction tank 5 bottoms and crucible cover 6 in two sections of process furnace 9, the process furnace 9 of heat insulation function, be positioned over that thick calcium 7, distillation reaction tank 5 upper ends in crucible 8 are provided with to connect vacuum system remove vacuum-lines 10, and be shaped as down the retort bell of " protruding " shape.Wherein, " protruding " shape bell top arranges water jacket 1, between distillation reaction tank 5 and retort bell, is provided with sealing-ring 2, and water jacket 1 is in order to protect sealing-ring 2, maintain the low-temperature condition of bell lower surface 3, in order to collect lower boiling, high saturated vapor pressure impurity simultaneously; Be provided with cold plate 4 in bell " protruding " face lower end, cold plate 4 is exposed on the outer outside bell convex surface lower end and is uniformly distributed some apertures, in order to collect major metal.
The vacuum system of going vacuum-lines 10 to connect is made up of two stage pump, and primary pump is rotary vane mechanical pump, and two stage pump is oil diffusion pump.
As shown in Figure 2, on crucible cover 6, be uniformly distributed a series of apertures, its role is to reduce the vaporator rate of metal, guarantee carrying out smoothly of distillation.On crucible cover 6, small aperture is not less than 10mm, and quantity is not less than 20.
As shown in Figure 3, cold plate 4 outers are uniformly distributed a series of apertures, and in still-process, lower boiling, high saturated vapor pressure impurity will finally be condensate in bell lower surface 3 places through set aperture.Wherein, the outer small aperture of cold plate 4 is not less than 10mm, and quantity is not less than 16.
Above-mentioned cold plate external diameter is slightly less than furnace wall internal diameter, is not more than 3mm with the difference of furnace wall internal diameter.The external diameter of bell convex surface lower end is less than cold plate external diameter, and is not less than 50mm with the difference of cold plate external diameter.
Above-mentioned distillation reaction tank 5 and bell all can adopt stainless steel to make, and inwall is taked chromium plating processing.Cold plate 4, crucible 8 and crucible cover 6 all adopt High-Purity Molybdenum to make.
Adopt said apparatus, carry out high-purity calcium vacuum distilling and purify, comprise following steps:
1) system Pressure Rise Rate test: guarantee system Pressure Rise Rate 0.6Pa/h.As higher in system Pressure Rise Rate, need water distilling apparatus to hunt leak.
2) shove charge: be in the kiln environment of room temperature, humidity < 2% in temperature, the lower shove charge of Ar gas protection, and lift to process furnace.
3) dehydration degasification: connect vacuum system, open rotary vane mechanical pump and cooling water recirculation system, as system vacuum degree <10Pa, and oil diffusion pump heating is while exceeding 40 minutes, opens oil diffusion pump.When showing on vacuumometer that vacuum tightness reaches 10
-3～10
-2when Pa, close vacuum butterfly valve, and process furnace upper-lower section resistance wire is switched on simultaneously.Control electric current and make retort temperature in 1 hour, rise to 200 ℃, and be incubated 0.5 hour in the time of 200 ℃, removing apparatus surface can adsorbable gas and some volatile substances.
4) fore-distillation: continue energising heating, make process furnace hypomere and epimere temperature all rise to 700 ℃, impel the volatilization of lower boiling in thick calcium, high saturation vapour pressure impurity, and be condensate in smoothly on bell lower surface 3 through the set aperture in cold plate 4 outers.
5) distillation: close process furnace epimere heating current, adopt the mode of air-cooled temperature control to make epimere temperature be reduced to 550～600 ℃, continue hypomere continuation heating simultaneously and make its temperature rise to 850 ℃, calcium metal start vaporizer, and be condensate on set cold plate 4.
6) come out of the stove: after still-process finishes, cut off process furnace resistance wire power supply, water distilling apparatus is naturally cooled to after room temperature, in water distilling apparatus retort, pass into Ar gas to concora crush, and whole water distilling apparatus is transported in kiln environment and is come out of the stove.
The amount of steaming of above-mentioned fore-distillation step is controlled at 5～10wt.% of the thick calcium of raw material.The amount of steaming of distilation steps is controlled at 80～90wt.% of the thick calcium of raw material.
Embodiment 1
Adopt the high-purity calcium vacuum distillation purification device of the utility model, carry out high-purity calcium vacuum distilling and purify, its step is as follows:
1) system Pressure Rise Rate test: guarantee that system Pressure Rise Rate is 0.6Pa/h.As higher in system Pressure Rise Rate, need water distilling apparatus to hunt leak.
2) shove charge: be in the kiln environment of room temperature, humidity < 2% in temperature, the lower shove charge of Ar gas protection, and lift to process furnace, the purity > 99% of the thick calcium of raw material, foreign matter content is in table 1.
3) dehydration degasification: connect vacuum system, open rotary vane mechanical pump and cooling water recirculation system, as system vacuum degree <10Pa, and oil diffusion pump heating is while exceeding 40 minutes, opens oil diffusion pump.When showing on vacuumometer that vacuum tightness reaches 10
-3～10
-2when Pa, close vacuum butterfly valve, and process furnace upper-lower section resistance wire is switched on simultaneously.Control electric current and make retort temperature in 1 hour, rise to 200 ℃, and be incubated 0.5 hour in the time of 200 ℃, removing apparatus surface can adsorbable gas and some volatile substances.
4) fore-distillation: continue energising heating, make process furnace hypomere and epimere temperature all rise to 700 ℃, be incubated 40 minutes.Lower boiling, the volatilization of high saturation vapour pressure impurity in thick calcium, and be condensate in smoothly on bell lower surface 3 through the set aperture in cold plate 4 outers.
5) distillation: close process furnace epimere heating current, adopt the mode of air-cooled temperature control to make epimere temperature be reduced to 550～600 ℃, continue hypomere continuation heating simultaneously and make its temperature rise to 850 ℃, be incubated 1 hour.Calcium metal evaporation, and be condensate on set cold plate 4.
6) come out of the stove: after still-process finishes, cut off process furnace resistance wire power supply, water distilling apparatus is naturally cooled to after room temperature, in water distilling apparatus retort, pass into Ar gas to concora crush, and whole water distilling apparatus is transported in kiln environment and is come out of the stove and sampling analysis.
After a vacuum distilling, the thick calcium of raw material and the high-purity calcium impurities content balance of gained data are in table 1.
The thick calcium of table 1 raw material and high-purity calcium impurities content balance
In above-mentioned specific embodiment, fore-distillation step and distilation steps soaking time are respectively 40 minutes and 1 hour, are to determine according to raw material input amount.Institute's basis principle is to control fore-distillation and distill the amount of steaming the 5～10wt.% and the 80～90wt.% that are respectively the thick calcium of raw material.
Above-mentioned specific embodiment is only explanation technical conceive of the present utility model and feature; content of the present utility model is not limited to the vacuum distilling of high-purity calcium and purifies; be equally applicable to other metals; allly be applied to the purify behavior of other metals of vacuum distilling after converting or modify according to the utility model content and spirit, within all should being encompassed in protection domain of the present utility model.
Claims (8)
1. a high-purity calcium vacuum distillation purification device, it is characterized in that: this device comprises distillation reaction tank in process furnace, process furnace, is placed on the crucible of distillation reaction pot bottom and crucible cover with holes, thick calcium is positioned in crucible, described distillation reaction tank upper end arranges in order to connect the vacuum-lines that goes of vacuum system, and the retort bell of cross-sectional shape for falling " protruding " shape, bell top arranges water jacket, convex surface lower end at bell is provided with cold plate, and cold plate is exposed on the outer outside bell convex surface lower end and is uniformly distributed some apertures.
2. high-purity calcium vacuum distillation purification device as claimed in claim 1, is characterized in that: described process furnace is two sections of process furnace that adopt resistance wire indirect heating, have heat insulation function.
3. high-purity calcium vacuum distillation purification device as claimed in claim 1, is characterized in that: described vacuum system is made up of two stage pump, and primary pump is rotary vane mechanical pump, and two stage pump is oil diffusion pump.
4. high-purity calcium vacuum distillation purification device as claimed in claim 1, is characterized in that: the outer of described cold plate is uniformly distributed aperture, and small aperture is not less than 10mm, and little hole number is not less than 16.
5. high-purity calcium vacuum distillation purification device as claimed in claim 1, is characterized in that: on described crucible cover, be uniformly distributed aperture, small aperture is not less than 10mm, and little hole number is not less than 20.
6. high-purity calcium vacuum distillation purification device as claimed in claim 1, is characterized in that: between described distillation reaction tank and retort bell, sealing-ring is set.
7. high-purity calcium vacuum distillation purification device as claimed in claim 1, is characterized in that: described distillation reaction tank and retort bell material are stainless steel, and all takes inwall chromium plating processing; Described crucible, crucible cover and cold plate material are High-Purity Molybdenum.
8. high-purity calcium vacuum distillation purification device as claimed in claim 1, is characterized in that: described cold plate external diameter is less than furnace wall internal diameter, is not more than 3mm with the difference of furnace wall internal diameter; The external diameter of described bell convex surface lower end is less than cold plate external diameter, is not less than 50mm with the difference of cold plate external diameter.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420001685.7U CN203683627U (en) | 2014-01-02 | 2014-01-02 | High-purity calcium vacuum distillation purifying device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420001685.7U CN203683627U (en) | 2014-01-02 | 2014-01-02 | High-purity calcium vacuum distillation purifying device |
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| CN203683627U true CN203683627U (en) | 2014-07-02 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104296525A (en) * | 2014-11-11 | 2015-01-21 | 河北城大金属集团有限公司 | Alloy vacuum separation furnace |
| CN104498741A (en) * | 2015-01-12 | 2015-04-08 | 罗英明 | Rare earth purification method and electric heating furnace |
| JP2018059177A (en) * | 2016-10-07 | 2018-04-12 | 太平洋セメント株式会社 | Production device of alkali earth metal and production method |
| CN111218559A (en) * | 2018-11-26 | 2020-06-02 | 广东先导稀材股份有限公司 | Melt evaporation device and method |
-
2014
- 2014-01-02 CN CN201420001685.7U patent/CN203683627U/en not_active Expired - Lifetime
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104296525A (en) * | 2014-11-11 | 2015-01-21 | 河北城大金属集团有限公司 | Alloy vacuum separation furnace |
| CN104498741A (en) * | 2015-01-12 | 2015-04-08 | 罗英明 | Rare earth purification method and electric heating furnace |
| CN104498741B (en) * | 2015-01-12 | 2017-10-24 | 罗英明 | A kind of rare earth method of purification and electrothermal furnace |
| JP2018059177A (en) * | 2016-10-07 | 2018-04-12 | 太平洋セメント株式会社 | Production device of alkali earth metal and production method |
| CN111218559A (en) * | 2018-11-26 | 2020-06-02 | 广东先导稀材股份有限公司 | Melt evaporation device and method |
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Effective date of registration: 20190621 Address after: 101407 No. 11 Xingke East Street, Yanqi Economic Development Zone, Huairou District, Beijing Patentee after: YOUYAN ENGINEERING TECHNOLOGY RESEARCH INSTITUTE Co.,Ltd. Address before: No. 2, Xinjie street, Xicheng District, Beijing, Beijing Patentee before: General Research Institute for Nonferrous Metals |
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Effective date of registration: 20210408 Address after: 101407 No. 11 Xingke East Street, Yanqi Economic Development Zone, Huairou District, Beijing Patentee after: Youyan resources and Environment Technology Research Institute (Beijing) Co.,Ltd. Address before: 101407 No. 11 Xingke East Street, Yanqi Economic Development Zone, Huairou District, Beijing Patentee before: YOUYAN ENGINEERING TECHNOLOGY RESEARCH INSTITUTE Co.,Ltd. |
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Granted publication date: 20140702 |
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| CX01 | Expiry of patent term |