CN202705435U - Device for producing ultrahigh-purity metallic magnesium by using commercially pure magnesium - Google Patents
Device for producing ultrahigh-purity metallic magnesium by using commercially pure magnesium Download PDFInfo
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- CN202705435U CN202705435U CN2012204025381U CN201220402538U CN202705435U CN 202705435 U CN202705435 U CN 202705435U CN 2012204025381 U CN2012204025381 U CN 2012204025381U CN 201220402538 U CN201220402538 U CN 201220402538U CN 202705435 U CN202705435 U CN 202705435U
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- vacuum chamber
- plumbago crucible
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 171
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 165
- 239000011777 magnesium Substances 0.000 title claims abstract description 165
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000010439 graphite Substances 0.000 claims abstract description 62
- 239000002994 raw material Substances 0.000 claims abstract description 41
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims description 59
- 239000002184 metal Substances 0.000 claims description 58
- 241000209456 Plumbago Species 0.000 claims description 56
- 238000000034 method Methods 0.000 claims description 54
- 239000012530 fluid Substances 0.000 claims description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 14
- 229910002804 graphite Inorganic materials 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 6
- 239000007769 metal material Substances 0.000 abstract description 4
- 238000009833 condensation Methods 0.000 abstract description 3
- 230000005494 condensation Effects 0.000 abstract description 3
- 230000007123 defense Effects 0.000 abstract description 3
- 238000005292 vacuum distillation Methods 0.000 abstract description 3
- 241000196324 Embryophyta Species 0.000 description 12
- 239000007788 liquid Substances 0.000 description 7
- 229910000861 Mg alloy Inorganic materials 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- 239000000956 alloy Substances 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000013022 venting Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 150000002738 metalloids Chemical class 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000007920 subcutaneous administration Methods 0.000 description 1
- 239000000126 substance 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 belongs to the field of preparation of metal materials and particularly relates to a device for producing ultrahigh-purity metallic magnesium by using commercially pure magnesium. A vacuum chamber furnace cover is arranged at the bottom of a vacuum chamber; a raw material graphite crucible and a high-purity magnesium collector graphite crucible are arranged on the vacuum chamber furnace cover; a heating furnace I connected with a temperature controller I is arranged on the outer side of the raw material graphite crucible; a heating furnace II connected with a temperature controller II is arranged at the top of the heating furnace I; and a condenser is arrange inside the heating furnace II and is connected to the high-purity magnesium collector graphite crucible through a chute. According to the device disclosed by the utility model, vacuum distillation can be directly carried out on industrial magnesium ingots or can be carried out on industrial magnesium ingots in which a small amount of iron powder is added; and the vacuum degree of the vacuum chamber is controlled to 2-15Pa, the temperature of a condensation area is controlled to 660-750DEG C and the temperature of a raw material area is controlled to 760-850DEG C, and thus ultrahigh-purity metallic magnesium ingots are directly generated. According to the device disclosed by the utility model, the ultrahigh-purity metallic magnesium with the purity being greater than or equal to 99.99 percent by weight is obtained; and the requirements of fields such as national defense, electronics and biological engineering materials are completely met.
Description
Affiliated technical field
The utility model belongs to the metallic substance preparation field, is specifically related to a kind of device that is prepared ultra-high purity metal magnesium by pure magnesium.
Background technology
Magnesium is that all structures are minimum with density in the metal and alloy materials.Compare with other structural metallic materialss, magnesium and magnesium alloy have specific tenacity, specific rigidity is high, vibration damping, electromagnetic shielding and capability of resistance to radiation are strong, easy machining, the series of advantages such as easy recovery, having extremely important using value and wide application prospect at automobile, electronics, electrical equipment, traffic, biology, space flight, aviation and national defense and military industrial circle, is the 3rd metalloid structured material that grows up after iron and steel and aluminium alloy, and is referred to as " green engineering material of 21 century ".
Corrosion is one of major obstacle of running in actual application of magnesium and magnesium alloy, and low solidity to corrosion has seriously hindered magnesium and magnesium alloy using more widely at automobile, electronics, electrical equipment, traffic, biomedicine, space flight, aviation and national defense and military industrial circle.For example, magnesium has good bio-compatibility, and magnesium itself is that human body metabolism is necessary.But magnesium and magnesium alloy owing to too fast in the human body internal corrosion, produce a large amount of gas as human material, make the subcutaneous bubble that occurs of human body, and the key that addresses this problem is exactly to improve the purity of magnesium and alloy thereof, because high purity magnesium is difficult to corrosion.
At present, the preparation method of the high purity magnesium of industrial employing mainly contains flux-refining method, electrolytic refining process, additive degree of depth purifying method and induction furnace refining method.Adopt aforesaid method to prepare having the problem of a maximum in the process of producing high purity metal magnesium is to produce easily secondary pollution, in order to address this problem, the production of high purity magnesium also has the method that adopts vacuum distilling, according to present production technique and device, secondary pollution still appears in high purity magnesium easily in the remelting casting cycle, and purity also is difficult to break through 99.99wt%.
The utility model content
The purpose of this utility model is for satisfying metal material field to the requirement of producing high purity metal magnesium purity, a kind of device that is prepared ultra-high purity metal magnesium (more than or equal to 99.99wt%) by pure magnesium is provided, not only can solve the problem of secondary pollution, and can obviously reduce impurity content in the high purity magnesium, make the purity of magnesium in the producing high purity metal magnesium more than or equal to 99.99wt%.
The technical solution of the utility model is as follows:
A kind of device that is prepared ultra-high purity metal magnesium by pure magnesium, this device comprises: vacuum chamber bell, raw material plumbago crucible, process furnace I, process furnace II, condenser, temperature regulator I, temperature regulator II, vacuum chamber, high purity magnesium collector plumbago crucible, and concrete structure is as follows:
The bottom of vacuum chamber arranges the vacuum chamber bell, be fire door down, the vacuum chamber bell is provided with raw material plumbago crucible, high purity magnesium collector plumbago crucible, the process furnace I that the arranged outside of raw material plumbago crucible links to each other with the temperature regulator I, the top of process furnace I arranges the process furnace II that links to each other with the temperature regulator II, the inside of process furnace II arranges condenser, and condenser is connected to high purity magnesium collector plumbago crucible by chute.
Describedly prepare the device of ultra-high purity metal magnesium by pure magnesium, raw material plumbago crucible and high purity magnesium collector plumbago crucible are fixed on vacuum chamber bell top, and high purity magnesium collector plumbago crucible is positioned at the heating unit outside.
Describedly prepare the device of ultra-high purity metal magnesium by pure magnesium, vacuum chamber bell below connecting fluid pressure device.
Describedly prepare the device of ultra-high purity metal magnesium by pure magnesium, pure magnesium is equipped with in the inside of raw material plumbago crucible, collects producing high purity metal magnesium in the high purity magnesium collector plumbago crucible.
Describedly prepare the device of ultra-high purity metal magnesium by pure magnesium, the vacuum chamber side is communicated with vacuum system by pipeline.
That utilizes described device prepares the method for ultra-high purity metal magnesium by pure magnesium, it is that raw material is made purity more than or equal to 99.99wt% ultra-high purity metal magnesium that the method adopts industrial magnesium ingot, directly industrial magnesium ingot or the technical pure magnesium ingot that adds a small amount of iron powder are carried out vacuum distillation, the vacuum degree control of vacuum chamber is at 2-15Pa, the condenser zone temperature is controlled at 660-750 ° of C, the raw material regional temperature is controlled at 760-850 ° of C, thereby directly generates the ultra-high purity metal magnesium ingot.
Describedly prepare the method for ultra-high purity metal magnesium by pure magnesium, resistive heating is all adopted in condenser zone and raw material zone, and by different temperature regulator temperature controls, can accurately control distillation and the condensation of MAGNESIUM METAL.
Describedly prepare the method for ultra-high purity metal magnesium by pure magnesium, concrete steps are as follows:
1) vacuum chamber bell (fire door) is moved down by hydraulic efficiency plant, expose the raw material plumbago crucible that holds pure magnesium and the high purity magnesium collector plumbago crucible that holds ultra-high purity metal magnesium, industrial magnesium ingot or the technical pure magnesium ingot that adds a small amount of iron powder are put into the raw material plumbago crucible, and high purity magnesium collector plumbago crucible cleaned out, then by hydraulic efficiency plant the vacuum chamber bell is closed;
2) heating before, by vacuum system vacuum chamber is vacuumized first, and with vacuum keep at 2-15Pa;
3) by the process furnace II condenser zone is heated, and by the temperature regulator II condenser zone temperature is controlled at 660-750 ° of C; Then by the process furnace I raw material plumbago crucible zone that holds pure magnesium is heated, and by the temperature regulator I temperature is controlled at 760-850 ° of C;
4) when magnesium steam contacts with condenser, will form liquid ultra-high purity metal magnesium, liquid ultra-high purity metal magnesium constantly flows in the plumbago crucible along the chute of condenser inside, and is frozen into the ultra-high purity metal magnesium ingot;
5) the ultra-high purity metal magnesium distilled time was controlled in 5 hours, at first stops to vacuumize, and venting, then open fire door by hydraulic efficiency plant, from plumbago crucible, take out the ultra-high purity metal magnesium after solidifying;
6) again industrial magnesium ingot or the technical pure magnesium ingot that adds a small amount of iron powder are put into plumbago crucible, and plumbago crucible is cleaned out, then by hydraulic efficiency plant fire door is closed repeated experiments.
Describedly prepare the method for ultra-high purity metal magnesium by pure magnesium, the raw material plumbago crucible just enters in the process furnace I, and the condenser region is condenser zone, heats by the process furnace II.
Describedly prepare the method for ultra-high purity metal magnesium by pure magnesium, add in the technical pure magnesium ingot of a small amount of iron powder, the addition of iron powder accounts for 0.001-0.01wt%.
The utility model compared with prior art, its advantage mainly contains:
1, the utility model prepares the apparatus and method of ultra-high purity metal magnesium by pure magnesium, and condenser zone and raw material zone are adopted respectively resistive heating, and by different temperature regulator temperature controls, can accurately control distillation and the condensation of MAGNESIUM METAL.
2, the utility model is prepared the apparatus and method of ultra-high purity metal magnesium by pure magnesium, when the condenser zone temperature is controlled at 660-750 ° of C, magnesium steam contacts with condenser, form liquid ultra-high purity metal magnesium, liquid ultra-high purity metal magnesium constantly flows in the plumbago crucible along the chute of condenser inside, and be frozen into ultra-high purity metal magnesium ingot, the secondary pollution that can avoid remelting to cause.
3, the utility model is prepared the apparatus and method of ultra-high purity metal magnesium by pure magnesium, easy to operate when fully taking into account industrial production, fire door down, and raw material plumbago crucible and high purity magnesium are collected crucible be fixed on the fire door top, the fire door below is connected with hydraulic efficiency plant, can freely open up and down fire door, be convenient to charging and take out ultra-pure magnesium ingot.
4, the assembling of the utility model crystallizer is simple, is convenient to safeguard.
5, the utility model main technologic parameters: vacuum tightness 2-15Pa, 660-750 ° of C of condenser zone temperature, 760-850 ° of C of raw material regional temperature.The preparation method that the utility model provides and device are used for the preparation of ultra-high purity metal magnesium, can obtain purity more than or equal to 99.99wt% ultra-high purity metal magnesium, can satisfy the demand in the fields such as national defence, electronics and biological engineering material fully.
Description of drawings
Fig. 1 is the cross-sectional schematic of the utility model producing high purity metal magnesium device that the preparation method adopts.
Wherein, (1) vacuum chamber bell; (2) hydraulic efficiency plant; (3) raw material plumbago crucible; (4) process furnace I; (5) pure magnesium; (6) process furnace II; (7) condenser; (8) temperature regulator I; (9) temperature regulator II; (10) vacuum chamber; (11) vacuum system; (12) high purity magnesium collector plumbago crucible; (13) producing high purity metal magnesium.
Embodiment
As shown in Figure 1, the utility model prepares the device that the method for ultra-high purity metal magnesium adopts by pure magnesium, mainly comprise: vacuum chamber bell (1), hydraulic efficiency plant (2), raw material plumbago crucible (3), process furnace I (4), pure magnesium (5), process furnace II (6), condenser (7), temperature regulator I (8), temperature regulator II (9), vacuum chamber (10), vacuum system (11), high purity magnesium collector plumbago crucible (12), producing high purity metal magnesium (13), concrete structure is as follows:
The bottom of vacuum chamber (10) arranges vacuum chamber bell (1), be fire door down, vacuum chamber bell (1) below connecting fluid pressure device (2), vacuum chamber bell (1) is provided with raw material plumbago crucible (3), high purity magnesium collector plumbago crucible (12), the process furnace I (4) that the arranged outside of raw material plumbago crucible (3) links to each other with temperature regulator I (8), pure magnesium (5) is equipped with in the inside of raw material plumbago crucible (3), the top of process furnace I (4) arranges the process furnace II (6) that links to each other with temperature regulator II (9), the inside of process furnace II (6) arranges condenser (7), condenser (7) is connected to high purity magnesium collector plumbago crucible (12) by chute, collects producing high purity metal magnesium (13) in the high purity magnesium collector plumbago crucible (12).In addition, vacuum chamber (10) side is communicated with vacuum system (11) by pipeline.
The utility model prepares the method for ultra-high purity metal magnesium by pure magnesium, and it is that raw material is made purity more than or equal to 99.99wt% ultra-high purity metal magnesium that the method adopts industrial magnesium ingot, and can directly generate the ultra-high purity metal magnesium ingot, and concrete steps are as follows:
1) vacuum chamber bell (1) (fire door) is moved down by hydraulic efficiency plant (2), expose the raw material plumbago crucible (3) that holds pure magnesium and the high purity magnesium collector plumbago crucible (12) that holds ultra-high purity metal magnesium, industrial magnesium ingot (is perhaps added the technical pure magnesium ingot of a small amount of iron powder, the addition of iron powder accounts for 0.001-0.01wt%) put into raw material plumbago crucible (3), and high purity magnesium collector plumbago crucible (12) cleaned out, then by hydraulic efficiency plant (2) vacuum chamber bell (1) is closed; Raw material plumbago crucible (3) just enters in the process furnace I (4), and condenser (7) region is condenser zone, can heat by process furnace II (6);
2) heating before, by vacuum system (11) vacuum chamber (10) is vacuumized first, and with vacuum keep at 2-15Pa;
3) by process furnace II (6) condenser zone is heated, and by temperature regulator II (9) the condenser zone temperature is controlled at 660-750 ° of C; Then by process furnace I (4) raw material plumbago crucible (3) zone that holds pure magnesium is heated, and by temperature regulator I (8) temperature is controlled at 760-850 ° of C;
4) when magnesium steam and condenser (7) when contacting, will form liquid ultra-high purity metal magnesium, liquid ultra-high purity metal magnesium constantly flows in the high purity magnesium collector plumbago crucible (12) along the inner chute of condenser (7), and is frozen into the ultra-high purity metal magnesium ingot;
5) the ultra-high purity metal magnesium distilled time was controlled in 5 hours, at first stops to vacuumize, and venting, then open fire door by hydraulic efficiency plant (2), from high purity magnesium collector plumbago crucible (12), take out the ultra-high purity metal magnesium after solidifying; And again industrial magnesium ingot (perhaps adding the technical pure magnesium ingot of a small amount of iron powder) is put into raw material plumbago crucible (3), and high purity magnesium collector plumbago crucible (12) is cleaned out, then by hydraulic efficiency plant fire door is closed repeated experiments.
Further, described a kind of method that is prepared ultra-high purity metal magnesium by pure magnesium, directly industrial magnesium ingot (is perhaps added the technical pure magnesium ingot of a small amount of iron powder, the addition of iron powder accounts for 0.001-0.01wt%) carry out vacuum distillation, the key of method is to control the vacuum degree control of vacuum chamber at 2-15Pa, the condenser zone temperature is controlled at 660-750 ° of C, the raw material regional temperature is controlled at 760-850 ° of C.
Further, describedly prepare the device that the method for ultra-high purity metal magnesium adopts by pure magnesium, resistive heating is all adopted in condenser zone and raw material zone, and by different temperature regulator temperature controls, liquid ultra-high purity metal magnesium collection device is positioned at the heating unit outside; In addition, can freely open fire door by hydraulic efficiency plant, be convenient to charging and take out ultra-pure magnesium ingot.
In the utility model, raw material plumbago crucible (3) and collect high purity magnesium collector plumbago crucible (12) material be " three height " graphite (three height refer to high-density, high purity, high strength, as: isostatic pressing formed graphite etc.), can prevent secondary pollution.
In the present embodiment, raw material is the pure magnesium of 99.95wt%, and the raw material regional temperature is controlled at 760 ° of C, and the condenser zone temperature is controlled at 680 ° of C, and vacuum degree control is at 5Pa.Can obtain highly purified MAGNESIUM METAL by this technique, each element quality percentage composition sees Table 1# sample in 1.
In the present embodiment, raw material is for adding the pure magnesium of 0.005wt% straight iron powder, and the raw material regional temperature is controlled at 800 ° of C, and the condenser zone temperature is controlled at 700 ° of C, and vacuum degree control is at 8Pa.Can obtain highly purified MAGNESIUM METAL by this technique, each element quality percentage composition sees Table 2# sample in 1.
Table 1 high purity magnesium chemical analysis results
Embodiment result shows, the method for preparing producing high purity metal magnesium and the device thereof that the utility model proposes, and can prepare purity is 99.99wt% or above producing high purity metal magnesium, and easy to operate, is conducive to enterprise scale production.
Claims (5)
1. device that is prepared ultra-high purity metal magnesium by pure magnesium, it is characterized in that, this device comprises: vacuum chamber bell (1), raw material plumbago crucible (3), process furnace I (4), process furnace II (6), condenser (7), temperature regulator I (8), temperature regulator II (9), vacuum chamber (10), high purity magnesium collector plumbago crucible (12), and concrete structure is as follows:
The bottom of vacuum chamber (10) arranges vacuum chamber bell (1), be fire door down, vacuum chamber bell (1) is provided with raw material plumbago crucible (3), high purity magnesium collector plumbago crucible (12), the process furnace I (4) that the arranged outside of raw material plumbago crucible (3) links to each other with temperature regulator I (8), the top of process furnace I (4) arranges the process furnace II (6) that links to each other with temperature regulator II (9), the inside of process furnace II (6) arranges condenser (7), and condenser (7) is connected to high purity magnesium collector plumbago crucible (12) by chute.
2. according to the device that is prepared ultra-high purity metal magnesium by pure magnesium claimed in claim 1, it is characterized in that, raw material plumbago crucible (3) and high purity magnesium collector plumbago crucible (12) are fixed on vacuum chamber bell top, and high purity magnesium collector plumbago crucible (12) is positioned at the heating unit outside.
3. prepare the device of ultra-high purity metal magnesium according to claimed in claim 1 by pure magnesium, it is characterized in that, vacuum chamber bell (1) below connecting fluid pressure device (2).
4. prepare the device of ultra-high purity metal magnesium according to claimed in claim 1 by pure magnesium, it is characterized in that pure magnesium (5) is equipped with in the inside of raw material plumbago crucible (3), collect producing high purity metal magnesium (13) in the high purity magnesium collector plumbago crucible (12).
5. prepare the device of ultra-high purity metal magnesium according to claimed in claim 1 by pure magnesium, it is characterized in that vacuum chamber (10) side is communicated with vacuum system (11) by pipeline.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012204025381U CN202705435U (en) | 2012-08-14 | 2012-08-14 | Device for producing ultrahigh-purity metallic magnesium by using commercially pure magnesium |
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| CN2012204025381U CN202705435U (en) | 2012-08-14 | 2012-08-14 | Device for producing ultrahigh-purity metallic magnesium by using commercially pure magnesium |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103952612A (en) * | 2014-04-15 | 2014-07-30 | 西安科技大学 | Preparation method and preparation device of ultra-pure magnesium-zinc binary alloy |
| CN111334672A (en) * | 2020-03-09 | 2020-06-26 | 西格马(河南)高温科技集团有限公司 | Energy-saving magnesium purification device and purification process thereof |
-
2012
- 2012-08-14 CN CN2012204025381U patent/CN202705435U/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103952612A (en) * | 2014-04-15 | 2014-07-30 | 西安科技大学 | Preparation method and preparation device of ultra-pure magnesium-zinc binary alloy |
| CN103952612B (en) * | 2014-04-15 | 2017-01-04 | 西安科技大学 | The preparation method of ultrapure magnesium zinc bianry alloy and preparation facilities |
| CN111334672A (en) * | 2020-03-09 | 2020-06-26 | 西格马(河南)高温科技集团有限公司 | Energy-saving magnesium purification device and purification process thereof |
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130130 Termination date: 20170814 |