CN101560610B - Method of refining high-purity magnesium - Google Patents
Method of refining high-purity magnesium Download PDFInfo
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- CN101560610B CN101560610B CN200910074442XA CN200910074442A CN101560610B CN 101560610 B CN101560610 B CN 101560610B CN 200910074442X A CN200910074442X A CN 200910074442XA CN 200910074442 A CN200910074442 A CN 200910074442A CN 101560610 B CN101560610 B CN 101560610B
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Abstract
The invention relates to a method for refining high-purity magnesium, which comprises the following steps: aiming at the characteristics of easy oxidization and volatile of pure magnesium, taking crude magnesium as a raw material, using a refining agent, and refining the crude magnesium in a vacuum smelting furnace; at an atmosphere that the pressure of argon is 100 Pa, under the conditions of bottom argon stirring and water circulation cooling, completing the refining and casting of the pure magnesium; and cutting under the protection of argon, and preparing the high-purity magnesium after electrolytic oxidization and epoxide resin impregnation and sealing, wherein the purity of the magnesium is 99.99 percent. The method makes the preparing and refining of the high-purity magnesium possible, and the refining temperature is 720 DEG C and the casting temperature is 680 DEG C; and the method fills the scientific research blank for refining the high-purity magnesium, and is an ideal method for refining and preparing the high-purity magnesium.
Description
Technical field
The present invention relates to a kind of method of refining of high-purity magnesium, belong to the technical field of smelting non-ferrous metal and cast molding.
Background technology
In non-ferrous metal, magnesium is one of light metal, light specific gravity, density are low, specific tenacity and specific rigidity height, heat-conductivity conducting is good, have good damping shock absorption and capability of electromagnetic shielding, be easy to die cast, cutting ability is good, is easy to recycling, can be made into Magnuminium with other element couplings, in aerospace, traffic, electron device, instrument, Communication Equipment, be used widely.
Magnesium is one of element distributed more widely in the earth's crust, the store content of magnesium is than horn of plenty, take up an area of 2.1% of shell weight, in the magnesium-smelting silicothermic process process, earlier with magnesium ore-rhombspar fragmentation, again with the dolomite calcination after the fragmentation, make magnesium calcined dolomite, again the magnesium calcined dolomite reduction is obtained crude magnesium, crude magnesium is through refining, make pure magnesium, magnesium is applied industrial with pure magnesium form, contains trace impurity in the pure magnesium, iron for example, silicon, nickel, copper, aluminium, chlorine, manganese, impurity such as titanium have detrimentally affect to the mechanical property of magnesium, magnesium oxide surpasses at 0.1% o'clock can reduce mechanical property, nickel content surpass 0.01% or potassium content surpass 0.03% the tensile strength of magnesium is reduced, so the crude magnesium refining is a crucial melting link.
Magnesium is because easily oxidation, volatile, refining, casting process complexity make high-purity magnesium be refined into a great problem, and also there are a lot of technical deficiencies in high-purity magnesium refining at present.
Summary of the invention
Goal of the invention
Purpose of the present invention is exactly at disadvantages of background technology, adopts new method of refining, at full closeding state, carries out the high-purity magnesium refining under argon shield, and is cast into ingot, with purity and the performance that increases substantially magnesium.
Technical scheme
The chemical substance material that the present invention uses is crude magnesium, refining agent, boron nitride, acetone, deionized water, zirconium white, argon gas, Vaseline, Resins, epoxy, steeping fluid, and its consumption is as follows: with gram, milliliter, centimetre
3Be measure unit
Crude magnesium: Mg 2000g ± 5g
Refining agent: 300g ± 2g
Boron nitride: BN 500g ± 10g
Acetone: CH
3COCH
32000ml ± 100ml
Deionized water: H
2O 20000ml ± 100ml
Vaseline: 1000ml ± 10ml
Zirconium white filter screen: 800 * 200 * 2mm
Resins, epoxy: 1000ml ± 10ml
Steeping fluid: 2000ml ± 50ml
Argon gas: Ar 200000cm
3± 100cm
3
The crude magnesium method of refining is as follows:
(1) selected raw chemical material
Crude magnesium: solid-state solid 99.48%
Refining agent: solid-state solid 99.8%
Boron nitride: solid-state solid 98.0%
Acetone: liquid liquid 99.0%
Deionized water: liquid liquid 99.0%
Vaseline: liquid liquid 96.0%
Zirconium white filter screen: 500 orders
Resins, epoxy: liquid liquid 99.0%
Steeping fluid: liquid liquid 99.0%
Argon gas: gaseous state gas 99.9%
(2) raw material preprocessing, cutting crude magnesium
Crude magnesium is cut into the bar shaped bulk, and bulk is of a size of 80 * 20 * 10mm;
(3) clean vacuum smelting furnace
1. open the vacuum melting furnace bell, with suction cleaner suction in-furnace dust dirt and objectionable impurities, time 10min;
2. scrub body of heater, furnace chamber, bell with deionized water, dry then, make its cleaning;
3. scrub, clean fire door, furnace wall, bell inwall with acetone, dry then, make the smelting furnace inner chamber be in clean state;
(4) cleaning smelting pot
1. with metal slice, metallic brush cleaning smelting pot inside and outside wall scar, impurity;
2. with suction cleaner suction crucible inside and outside wall dust;
3. use deionized water cleaning crucible inwall, make its cleaning, dry then;
(5) handle casting die, put the zirconium white filter screen
1. clean casting mould
To the stainless steel mould die cavity that casting is used, reject residue and objectionable impurities with metallic brush, metal slice;
2. scrub mold cavity and outside with deionized water, make it clean, dry then;
3. prepare, apply releasing agent
The preparation releasing agent: boron nitride 200g+ deionized water 500ml becomes liquid;
Apply releasing agent: in mold cavity, evenly spray releasing agent with spraying machine, releasing agent thickness is 0.1mm, dries standby;
4. the zirconium white filter screen is rolled into doline, places the die casting mouth;
(6) preheating casting die
Place loft drier to carry out preheating open-close type casting die assembling back integral body, 180 ℃ ± 5 ℃ of preheating temperatures, warm up time 30min ± 2min;
(7) put pure magnesium raw material
Pure MAG block 2000g vertically places smelting pot with strip;
Refining agent 60g is placed bar shaped MAG block slit;
(8) put casting die
Preheating and the casting die that applied the releasing agent boron nitride are placed the below, right side of smelting pot, be beneficial to the position of crucible uphill casting;
(9) put connection tunger tube up and down
1. connect the argon gas pneumatic tube of upper of furnace body;
2. connect the argon gas bottom blowpipe of crucible bottom;
(10) smelting furnace vacuumizes
1. melting fire door, bell internal orifice are evenly smeared Vaseline, cover then, make its sealing;
2. open vacuum pump, extract furnace air out, time 60min ± 2min makes vacuum tightness in the stove≤10
-2Pa.
(11) input protection gas---argon gas in stove
Open the argon gas pneumatic tube of upper of furnace body, input speed 100cm
3/ min makes to be in the argon gas atmosphere in the furnace chamber;
After the argon gas input, ar pressure continues to remain on 100Pa in the furnace chamber;
(12) the water cycle condensing works of unlatching smelting furnace outside carries out the body of heater cooling;
(13) pure magnesium refining
1. open the smelting furnace crucible heater, make the interior temperature of smelting pot begin to heat up by 20 ℃, 10 ℃/min of heat-up rate is warming up to 720 ℃ ± 5 ℃, heating-up time 70min ± 2min, and thermocouple measurement shows temperature in the stove;
2. open the smelting furnace air outlet; Viewing window is observed melting, casting situation;
3. after crude magnesium all melts, from the charging opening adding refining agent 30g on smelting furnace top;
4. the argon gas bottom blowpipe of crucible bottom is opened in crude magnesium, refining agent fusing back, is blown into argon gas, is blown into speed 100cm
3/ min makes that the magnesium melt becomes whipped state in the crucible, continues argon blowing time 10min ± 1min, makes that impurity fully contacts in refining agent and the magnesium;
5. close the argon gas bottom blowpipe, stop to stir, make the magnesium melt constant temperature in the crucible leave standstill 10min ± 1min;
6. adjust crucible heater power, make it cooling, reduce to 680 ℃ ± 5 ℃, begin casting then;
7. in the melting furnace chamber, under argon gas atmosphere, the crucible that will fill the magnesium melt is aimed at the casting die of bottom right sidepiece, and the magnesium melt is poured into the zirconium white filter screen and the inner chamber of stainless steel mould, observes the casting situation by viewing window, waters to stop after full;
8. closing crucible well heater, in argon gas atmosphere, the mould after the casting cools to 200 ℃ ± 5 ℃ with the furnace;
(14) come out of the stove
Close vacuum pump, argon gas pneumatic tube, open the melting bell, take out and burn casting mould;
(15) cooling
The casting die that ingot casting is housed is cooled to 20 ℃ ± 3 ℃ in physical environment;
(16) die sinking, the demoulding, get ingot
Open the open-close type stainless steel mould, ingot casting is taken out in the ingot casting demoulding;
(17) cleaning, finishing under argon shield, cut into ingot
The magnesium ingot casting is placed in the argon gas case, and the input argon gas, input speed 100cm
2/ min;
In the argon gas case,, make surface finishing with the fine sandpaper ingot casting of polishing;
In the argon gas case, use the cut mechanically magnesium ingot, cylindrical magnesium ingot is of a size of Φ 100 * 200mm;
In the argon gas case, with deerskin polishing magnesium ingot surface, making surfaceness is Ra0.32-0.64um;
(18) use electrolytic anodising process, with epoxy resin impregnated protection magnesium ingot
1. in the electrolytic anodization groove, add steeping fluid 2000ml, connect anode, negative electrode, current density 1.8-2.5A/m
2, voltage≤85V, 20 ℃ of temperature, time 10min;
2. after electrolytic anodization is handled, take out magnesium ingot, use epoxy resin impregnatedly then, dry then;
(19) detect, analyze, characterize, contrast
Magnesium ingot after the refining is detected its composition, color and luster, purity, foreign matter content, metallographic structure, chemical physics performance;
Carry out chemical composition analysis with spectrograph
Carry out metallographic structure analysis with metaloscope
Magnesium purity is: 99.99%
(20) storage package
The high purity magnesium ingot of preparation is packed with soft material, placed clean environment, waterproof, protection against the tide, anti-oxidation, acid-proof alkali salt erosion, 20 ℃ ± 3 ℃ of storing temps, relative temperature≤10%.
The refining of described high-purity magnesium, casting are carried out in vacuum melting furnace, are that stove seat 2, top are bell 11 in the bottom of smelting furnace 1; In the smelting furnace 1 is furnace chamber 3, and the middle part is a casting die 16 for smelting pot 14, right lower quadrant in the furnace chamber 3; Be provided with vacuum orifice 12, dedusting mouth 6, bottom blowing mouth 26, upper right quarter at the left part of smelting furnace 1 and be provided with water cycle cooling vent 13; Be provided with argon gas mouth 7, feeder 8, thermopair 9, viewing window 10, air outlet 18 on bell 11, feeder 8, thermopair 9 stretch in the smelting pot 14; Smelting pot 14 peripheries are for resistance heater 15, bottom are provided with argon blowing hole 19, inside is magnesium liquid 5; Casting die 16 tops are that pouring gate 17, inside are magnesium ingot 4; In the furnace chamber 3 is argon gas 25; Smelting furnace 1 left part is provided with argon bottle 24, and argon bottle 24 tops connect argon gas mouth 7 by argon gas valve 23, tunger tube 22, and argon bottle 24 connects the argon blowing hole 19 of bottom blowing mouth 26 and smelting pot bottom by argon gas valve 21, bottom blowpipe 20; Vacuum orifice 12 connects vacuum pump by pipeline; Water cycle condensate port 13 connects the water cycle condensing works by pipeline.
The refining of described high-purity magnesium, refining temperature is 720 ℃ ± 5 ℃, pouring temperature is 680 ℃ ± 5 ℃, and ar pressure continues to remain on 100Pa in the smelting furnace, finishes melting, the casting of high-purity magnesium in argon gas atmosphere, under the argon gas bottom blowing is stirred, under the water cycle cooling.
Described refining agent is by magnesium chloride Mg Cl
2, potassium chloride (KCl), sodium chloride nacl, calcium chloride CaCl
2, bariumchloride BaCl
2, bifluoride calcium CaF
2Form.
The electrolytic anodization of described high-purity magnesium, epoxy resin-impregnated are that the high purity magnesium ingot is immersed in the electrolyzer, and steeping fluid is by potassium hydroxide KOH, aluminium hydroxide Al (HO)
3, Potassium monofluoride KF, phosphoric acid H
3PO
4Form in proportion, use epoxy resin impregnated sealing then.
Beneficial effect
The present invention compares with background technology has tangible advance; it is the characteristic at magnesium; light specific gravity; easily oxidation; volatile; melting; the practical situation of casting process complexity; in argon gas atmosphere; under the argon gas bottom blowing is stirred; under the water cycle state of cooling; in vacuum melting furnace, finish the fusing of pure magnesium; refining; be cast into ingot; under argon shield, carry out cutting then; and carry out electrolytic anodization and handle, the epoxy resin-impregnated sealing is to increase substantially the purity of magnesium; make the microcosmic metallographic structure of pure magnesium more even; crystal grain is refinement more, and compactness is better, and the purity of magnesium can reach 99.99%; the mechanical property of magnesium is more stable; make the preparation high-purity magnesium become possibility, this method of refining has been filled up the scientific research blank of similar technology, is the method for refining of very good high-purity magnesium.
Description of drawings
Fig. 1 is high-purity magnesium refining and casting state graph
Fig. 2 is smelting temperature, pouring temperature and time coordinate graph of a relation
Fig. 3 is casting die and filter structure figure
Fig. 4 is high purity magnesium ingot and crude magnesium ingot square section metallographic structure comparison diagram
Fig. 5 is high-purity magnesium and crude magnesium chemical ingredients comparison diagram
Shown in the figure, list of numerals is as follows:
1, smelting furnace, 2, the stove seat, 3, furnace chamber, 4, magnesium ingot, 5, magnesium liquid, 6, the dedusting mouth, 7, the argon gas mouth, 8, feeder, 9, thermopair, 10, viewing window, 11, bell, 12, the water cycle prolong, 13, vacuum orifice, 14, smelting pot, 15, resistance heater, 16, casting die, 17, pouring gate, 18, the air outlet, 19, argon blowing hole, 20, bottom blowpipe, 21, the Argon valve, 22, tunger tube, 23, the argon gas valve, 24, argon bottle, 25, argon gas, 26, the bottom blowing mouth, 27, casting die, 28, pouring gate, 29, filter screen, 30, mold cavity, 31, movable rack, 32, movable rack, 33, magnesium liquid.
Embodiment
The present invention will be further described below in conjunction with accompanying drawing:
Shown in Figure 1, be vacuum melting furnace melting and casting state graph, smelting furnace is a rounded cylindrical, want strict between body of heater and the bell and clean with acetone, with the Vaseline sealing, strict clean in the furnace chamber, earlier take out dirt taking out the dirt mouth, clean with deionized water then and dry.
Water cycle condensate port and water cycle condensing works UNICOM to guarantee that furnace chamber temperature is constant when intensification, melting, the casting, guarantee safety.
Vacuum orifice and the sliding vane rotary pump that vacuumizes, lobe pump, protect diffusing pump, pneumavalve, strainer and connect, constant to guarantee vacuum tightness, ar pressure in the melting furnace chamber.
The air outlet is unimpeded, is the outlet of waste gas in the stove, also is the cavity pressure adjustment mouth in the refining process.
Feeder is the inlet that adds raw material and refining agent, and thermopair is to measure the interior temperature of crucible, check at any time, to keep homo(io)thermism in the crucible.
Viewing window is to observe melting in the furnace chamber, casting state, so that operation accurately.
The argon gas mouth connects argon bottle, to guarantee argon gas abundance in the furnace chamber; Argon blowing hole connects Argon valve, argon bottle by bottom blowpipe, to guarantee Argon amount abundance, makes the magnesium liquid in the crucible be in agitated conditions, and impurity is fully contacted with refining agent, prevents precipitation.
During casting magnesium liquid, crucible will tilt 90 °, aims at pouring gate and zirconium white filter screen on the casting die, slowly cast, filter, water full till.
Electrolytic anodization, be to use epoxy resin impregnated sealing then with steeping fluid electrolysis dipping in that the high purity magnesium ingot is outside, to increase the anticorrosive and wear resistance of magnesium ingot.
Shown in Figure 2, be refining, pouring temperature and time coordinate graph of a relation, refining is since 20 ℃ of intensifications, be the A point, 10 ℃/min of heat-up rate is when temperature rises to 720 ℃, be the B point, leave standstill 10min at this temperature constant temperature, i.e. the B-C section, be cooled to 680 ℃ then, promptly the D point is cast in this temperature, the casting postcooling is as for 200 ℃, i.e. E point is at this temperature blow-on delivery, in natural air, be cooled to 20 ℃ then, i.e. the F point.
Shown in Figure 3, be the casting die structure iron, be mold cavity 30 in the mould 27, both sides are movable rack 31,32, top is pouring gate 28, is zirconium white filter screen 29 in the pouring gate 28, is magnesium liquid 33 in the mold cavity 30; Mold cavity 30 is cylindrical, mountain font mold cavity four magnesium ingots of can casting simultaneously, and filter screen 29 usefulness zirconium white or ceramic material are advisable with 〉=500 orders, with impurity in the filtering magnesium liquid, reach 99.99% to guarantee magnesium purity.
Shown in Figure 4, be high purity magnesium ingot and crude magnesium ingot square section metallographic structure comparison diagram, among the figure as can be known: high-purity magnesium grain refining, density are even, and inclusion-free manifests, and crude magnesium crystal grain is coarse loose.
Shown in Figure 5, be high-purity magnesium and crude magnesium chemical ingredients comparison diagram, among the figure as can be known: the foreign matter content of high-purity magnesium obviously reduces, and the impurity summation of high-purity magnesium is less than 0.01%.
Claims (4)
1. the method for refining of a high-purity magnesium, it is characterized in that: the chemical substance material that uses is crude magnesium, refining agent, boron nitride, acetone, deionized water, zirconium white, argon gas, Vaseline, Resins, epoxy, steeping fluid, and described steeping fluid is by potassium hydroxide KOH, aluminium hydroxide Al (HO)
3, Potassium monofluoride KF, phosphoric acid H
3PO
4Form in proportion, use epoxy resin impregnated sealing then, its consumption is as follows: with gram, milliliter, centimetre
3Be measure unit
Crude magnesium: Mg 2000g ± 5g
Refining agent: 300g ± 2g
Boron nitride: BN 500g ± 10g
Acetone: CH
3COCH
32000ml ± 100ml
Deionized water: H
2O 20000ml ± 100ml
Vaseline: 1000ml ± 10ml
Zirconium white filter screen: 800 * 200 * 2mm
Resins, epoxy: 1000ml ± 10ml
Steeping fluid: 2000ml ± 50ml
Argon gas: Ar 200000cm
3± 100cm
3
The crude magnesium method of refining is as follows:
(1) selected raw chemical material
Crude magnesium: solid-state solid 99.48%
Refining agent: solid-state solid 99.8%
Boron nitride: solid-state solid 98.0%
Acetone: liquid liquid 99.0%
Deionized water: liquid liquid 99.0%
Vaseline: liquid liquid 96.0%
Zirconium white filter screen: 500 orders
Resins, epoxy: liquid liquid 99.0%
Steeping fluid: liquid liquid 99.0%
Argon gas: gaseous state gas 99.9%
(2) raw material preprocessing, cutting crude magnesium
Crude magnesium is cut into the bar shaped bulk, and bulk is of a size of 80 * 20 * 10mm;
(3) clean vacuum smelting furnace
1. open the vacuum melting furnace bell, with suction cleaner suction in-furnace dust dirt and objectionable impurities, time 10min;
2. scrub body of heater, furnace chamber, bell with deionized water, dry then, make its cleaning;
3. scrub, clean fire door, furnace wall, bell inwall with acetone, dry then, make the smelting furnace inner chamber be in clean state;
(4) cleaning smelting pot
1. with metal slice, metallic brush cleaning smelting pot inside and outside wall scar, impurity;
2. with suction cleaner suction crucible inside and outside wall dust;
3. use deionized water cleaning crucible inwall, make its cleaning, dry then;
(5) handle casting die, put the zirconium white filter screen
1. clean casting mould
To the stainless steel mould die cavity that casting is used, reject residue and objectionable impurities with metallic brush, metal slice;
2. scrub mold cavity and outside with deionized water, make it clean, dry then;
3. prepare, apply releasing agent
The preparation releasing agent: boron nitride 200g+ deionized water 500ml becomes liquid;
Apply releasing agent: in mold cavity, evenly spray releasing agent with spraying machine, releasing agent thickness is 0.1mm, dries standby;
4. the zirconium white filter screen is rolled into doline, places the die casting mouth;
(6) preheating casting die
Place loft drier to carry out preheating open-close type casting die assembling back integral body, 180 ℃ ± 5 ℃ of preheating temperatures, warm up time 30min ± 2min;
(7) put the crude magnesium raw material
2000g vertically places smelting pot with strip crude magnesium piece;
Refining agent 60g is placed bar shaped crude magnesium piece slit;
(8) put casting die
Preheating and the casting die that applied the releasing agent boron nitride are placed the below, right side of smelting pot, be beneficial to the position of crucible uphill casting;
(9) put connection tunger tube up and down
1. connect the argon gas pneumatic tube of upper of furnace body;
2. connect the argon gas bottom blowpipe of crucible bottom;
(10) smelting furnace vacuumizes
1. melting fire door, bell internal orifice are evenly smeared Vaseline, cover then, make its sealing;
2. open vacuum pump, extract furnace air out, time 60min ± 2min makes vacuum tightness in the stove≤10
-2Pa;
(11) input protection gas---argon gas in stove
Open the argon gas pneumatic tube of upper of furnace body, input speed 100cm
3/ min makes to be in the argon gas atmosphere in the furnace chamber;
After the argon gas input, ar pressure continues to remain on 100Pa in the furnace chamber;
(12) the water cycle condensing works of unlatching smelting furnace outside carries out the body of heater cooling;
(13) pure magnesium refining
1. open the smelting furnace crucible heater, make the interior temperature of smelting pot begin to heat up by 20 ℃, 10 ℃/min of heat-up rate is warming up to 720 ℃ ± 5 ℃, heating-up time 70min ± 2min, and thermocouple measurement shows temperature in the stove;
2. open the smelting furnace air outlet; Viewing window is observed melting, casting situation;
3. after crude magnesium all melts, from the charging opening adding refining agent 30g on smelting furnace top;
4. the argon gas bottom blowpipe of crucible bottom is opened in crude magnesium, refining agent fusing back, is blown into argon gas, is blown into speed 100cm
3/ min makes that the magnesium melt becomes whipped state in the crucible, continues argon blowing time 10min ± 1min, makes that impurity fully contacts in refining agent and the magnesium;
5. close the argon gas bottom blowpipe, stop to stir, make the magnesium melt constant temperature in the crucible leave standstill 10min ± 1min;
6. adjust crucible heater power, make it cooling, reduce to 680 ℃ ± 5 ℃, begin casting then;
7. in the melting furnace chamber, under argon gas atmosphere, the crucible that will fill the magnesium melt is aimed at the casting die of bottom right sidepiece, and the magnesium melt is poured into the zirconium white filter screen and the inner chamber of stainless steel mould, observes the casting situation by viewing window, waters to stop after full;
8. closing crucible well heater, in argon gas atmosphere, the mould after the casting cools to 200 ℃ ± 5 ℃ with the furnace;
(14) come out of the stove
Close vacuum pump, argon gas pneumatic tube, open the melting bell, take out and burn casting mould;
(15) cooling
The casting die that ingot casting is housed is cooled to 20 ℃ ± 3 ℃ in physical environment;
(16) die sinking, the demoulding, get ingot
Open the open-close type stainless steel mould, ingot casting is taken out in the ingot casting demoulding;
(17) cleaning, finishing under argon shield, cut into ingot
The magnesium ingot casting is placed in the argon gas case, and the input argon gas, input speed 100cm
2/ min;
In the argon gas case,, make surface finishing with the fine sandpaper ingot casting of polishing;
In the argon gas case, use the cut mechanically magnesium ingot, cylindrical magnesium ingot is of a size of Φ 100 * 200mm;
In the argon gas case, with deerskin polishing magnesium ingot surface, making surfaceness is Ra0.32-0.64um;
(18) use electrolytic anodising process, with epoxy resin impregnated protection magnesium ingot
1. in the electrolytic anodization groove, add steeping fluid 2000ml, connect anode, negative electrode, current density 1.8-2.5A/m
2, voltage≤85V, 20 ℃ of temperature, time 10min;
2. after electrolytic anodization is handled, take out magnesium ingot, use epoxy resin impregnatedly then, dry then;
(19) detect, analyze, characterize, contrast
Magnesium ingot after the refining is detected its composition, color and luster, purity, foreign matter content, metallographic structure, chemical physics performance;
Carry out chemical composition analysis with spectrograph
Carry out metallographic structure analysis with metaloscope
Magnesium purity is: 99.99%
(20) storage package
The high purity magnesium ingot of preparation is packed with soft material, placed clean environment, waterproof, protection against the tide, anti-oxidation, acid-proof alkali salt erosion, 20 ℃ ± 3 ℃ of storing temps, relative temperature≤10%.
2. the method for refining of a kind of high-purity magnesium according to claim 1 is characterized in that: the refining of described high-purity magnesium, casting are carried out in vacuum melting furnace, are that stove seat (2), top are bell (11) in the bottom of smelting furnace (1); In the smelting furnace (1) is furnace chamber (3), and the middle part is casting die (16) for smelting pot (14), right lower quadrant in the furnace chamber (3); Be provided with vacuum orifice (12), dedusting mouth (6), bottom blowing mouth (26), upper right quarter at the left part of smelting furnace 1 and be provided with water cycle cooling vent (13); Be provided with argon gas mouth (7), feeder (8), thermopair (9), viewing window (10), air outlet (18) on bell (11), feeder (8), thermopair (9) stretch in the smelting pot (14); Smelting pot (14) periphery is for resistance heater (15), bottom are provided with argon blowing hole (19), inside is magnesium liquid (5); Casting die (16) top is that pouring gate (17), inside are magnesium ingot (4); In the furnace chamber (3) is argon gas (25); Smelting furnace (1) left part is provided with argon bottle (24), argon bottle (24) top connects argon gas mouth (7) by argon gas valve (23), tunger tube (22), and argon bottle (24) connects the argon blowing hole (19) of bottom blowing mouth (26) and smelting pot bottom by argon gas valve (21), bottom blowpipe (20); Vacuum orifice (12) connects vacuum pump by pipeline; Water cycle condensate port (13) connects the water cycle condensing works by pipeline.
3. the method for refining of a kind of high-purity magnesium according to claim 1, it is characterized in that: the refining of described high-purity magnesium, refining temperature is 720 ℃ ± 5 ℃, pouring temperature is 680 ℃ ± 5 ℃, ar pressure continues to remain on 100Pa in the smelting furnace, finishes melting, the casting of high-purity magnesium in argon gas atmosphere, under the argon gas bottom blowing is stirred, under the water cycle cooling.
4. the method for refining of a kind of high-purity magnesium according to claim 1, it is characterized in that: described refining agent is by magnesium chloride Mg Cl
2, potassium chloride (KCl), sodium chloride nacl, calcium chloride CaCl
2, bariumchloride BaCl
2, bifluoride calcium CaF
2Form.
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|---|---|---|---|
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102296184B (en) * | 2011-09-15 | 2012-10-03 | 重庆大学 | Solvent-free magnesium alloy purification method |
| CN102398022B (en) * | 2011-11-03 | 2015-04-15 | 大同普罗卡特精华科技有限公司 | Casting method of a magnesium anode for a water heater |
| CN102634679A (en) * | 2012-04-28 | 2012-08-15 | 昆明理工大学 | Method for vacuum-refining and purifying magnesium metal |
| US9090953B2 (en) * | 2012-08-14 | 2015-07-28 | Ati Properties, Inc. | Methods for reducing impurities in magnesium, purified magnesium, and zirconium metal production |
| CN105400980A (en) * | 2015-11-16 | 2016-03-16 | 上海航天精密机械研究所 | Cast magnesium alloy refining device and refining method based on device |
| CN105734331A (en) * | 2016-05-05 | 2016-07-06 | 北京交通大学 | Aluminum alloy calcium remover as well as preparation method and use method thereof |
| CN105921720B (en) * | 2016-05-20 | 2017-10-20 | 河南理工大学 | A kind of magnesium alloy thin wall pieces preparation method |
| CN106756076B (en) * | 2017-04-01 | 2018-08-21 | 攀钢集团研究院有限公司 | Magnesium reducing agent fluxing agent and preparation method thereof |
| CN107586970A (en) * | 2017-09-06 | 2018-01-16 | 长沙科力威蒸馏技术有限公司 | A kind of method for purifying magnesium |
| CN108842064A (en) * | 2018-07-12 | 2018-11-20 | 五台云海镁业有限公司 | A kind of high purity magnesium and its production technology |
| CN115109939A (en) * | 2022-07-11 | 2022-09-27 | 上海交通大学四川研究院 | Smelting method of low-radioactivity background metal material |
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2009
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