CN107557604A - Aluminum refining agent and preparation method thereof - Google Patents
Aluminum refining agent and preparation method thereof Download PDFInfo
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- CN107557604A CN107557604A CN201711035072.XA CN201711035072A CN107557604A CN 107557604 A CN107557604 A CN 107557604A CN 201711035072 A CN201711035072 A CN 201711035072A CN 107557604 A CN107557604 A CN 107557604A
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Abstract
The invention discloses a kind of aluminum refining agent and preparation method thereof, the component of refining agent includes K2MgCl4、KMgCl3、Na2SiF6、Na3AlF6、Na2CO3And CaF2.Wherein, K2MgCl4And KMgCl3Generate Low melting point eutectic at high temperature, form the basic substance of aluminum refining agent provided by the invention, can in aluminium liquid rapid dispersion and effectively remove molten aluminum in non-metallic inclusion；Na2SiF6And Na3AlF6Catabolite at high temperature can effectively reduce the interface wet ability between solid-oxide and aluminium liquid, promote oxide inclusion and aluminium liquid separation；Na2CO3CO is decomposed to give off in high temperature aluminium liquid2, can effectively go dehydrogenation；CaF2The surface tension of fused salt mixt can be increased, make the fused salt spheroidizing of absorbing oxide, be easy to and melt separation, and reduce solid slag and wrap loss caused by aluminium；Edge crack can be reduced during magnesium alloy high applied to casting, so as to which the life-span of the speed of extrusion and increase mould can be increased in extrudate.
Description
Technical field
The invention belongs to Metallic Materials Held In Shanghai technical field, is related to a kind of aluminum refining agent and preparation method thereof.
Background technology
Aluminum refining agent is a kind of white powder or granular flux for metallurgy, after plurality of inorganic salt drying process
Mixed preparing forms by a certain percentage, and aluminium and its alloy together melting, is mainly used in the hydrogen removed inside aluminium liquid and swims
Oxide slag inclusion, make aluminium liquid purer.
Aluminium and its alloy show to be easy to aoxidize and absorb the characteristic of gas in melting casting cycle, cause pole in aluminium liquid
Gas and field trash are easily formed, stomata, shrinkage cavity and porosity, crackle, poured short and seepage etc. are a series of to be lacked so that casting produces
Fall into, substantially reduce the fatigue resistance of material, plasticity, intensity and the performance such as corrosion-resistant, or even cause casting to scrap, directly affect production
The quality of product, the application enabled aluminum alloy to are extremely limited, particularly aviation alloyed aluminium material, often because occur oxide-film and
The metallurgical imperfections such as non-metallic inclusion bring potential safety hazard to airborne vehicle, influence the quality of airborne vehicle.Aluminum refining agent adds
Enter to remove gas and various non-metallic inclusions, such as oxide, carbide and boride, so as to improve the property of casting
Energy.
But existing aluminum refining agent is being refined with after purified treatment, oxide inclusion is still more.
The content of the invention
The invention provides a kind of aluminum refining agent and preparation method thereof, is refining and is purifying to solve traditional refining agent
After processing, the problem of oxide inclusion is still more.
A kind of aluminum refining agent provided by the invention includes：K2MgCl4、KMgCl3、Na2SiF6、Na3AlF6、Na2CO3With
CaF2。
According to one embodiment of present invention, the K2MgCl4、KMgCl3、Na2SiF6、Na3AlF6、Na2CO3And CaF2Press
The content of mass percent is：K2MgCl4：30~45%, KMgCl3：40~55%, Na2SiF6：3~5%, Na3AlF6：2~
5%, Na2CO3：4~6% and CaF2：2~3%.
According to one embodiment of present invention, in addition to CaMg (CO3)2And K2SiF6One or both of.
According to one embodiment of present invention, the CaMg (CO3)2And K2SiF6One or both of press quality percentage
The content of ratio is 4~19%.
Present invention also offers a kind of preparation method of aluminum refining agent, for preparing above-mentioned aluminum refining agent, bag
Include following steps：
Step 1：61.0% KCl and 39.0% MgCl are taken by mass percentage2Mixing, is warming up to 500 DEG C of meltings, so
K is made in crystallisation by cooling afterwards2MgCl4；
Step 2：43.9% KCl and 56.1% MgCl are taken by mass percentage2Mixing, is warming up to 500 DEG C of meltings, so
KMgCl is made in crystallisation by cooling afterwards3；
Step 3：Take K obtained above2MgCl4And KMgCl3, with Na2SiF6、Na3AlF6、Na2CO3And CaF2Mixing, rise
Temperature is to 600~650 DEG C of meltings, and the alloy refining is made in crystallisation by cooling after being then incubated 1~2 hour at 600~650 DEG C
Agent.
According to one embodiment of present invention, the K2MgCl4、KMgCl3、Na2SiF6、Na3AlF6、Na2CO3And CaF2Press
The content of mass percent is：K2MgCl4：30~45%, KMgCl3：40~55%, Na2SiF6：3~5%, Na3AlF6：2~
5%, Na2CO3：4~6% and CaF2：2~3%.
According to one embodiment of present invention, described KCl, MgCl2、K2MgCl4、KMgCl3、Na2SiF6、Na3AlF6、
Na2CO3And CaF2It is milled to granularity and is less than 325 mesh.
A kind of aluminum refining agent provided by the invention can include the following benefits：A kind of aluminium provided by the invention closes
Gold refining agent includes K2MgCl4、KMgCl3、Na2SiF6、Na3AlF6、Na2CO3And CaF2, wherein, K2MgCl4And KMgCl3In height
The lower generation Low melting point eutectic of temperature, forms the basic substance of aluminum refining agent provided by the invention, can be quick in aluminium liquid
Non-metallic inclusion scattered and effectively in removal molten aluminum；Na2SiF6And Na3AlF6Catabolite at high temperature can have
Effect reduces the interface wet ability between solid-oxide and aluminium liquid, promotes oxide inclusion and aluminium liquid separation；Na2CO3In high temperature
CO is decomposed to give off in aluminium liquid2, can effectively go dehydrogenation；CaF2The surface tension of fused salt mixt can be increased, make absorbing oxide
Fused salt spheroidizing, is easy to and melt separation, and reduces solid slag and wrap loss caused by aluminium.
Brief description of the drawings
Fig. 1 is a kind of schematic flow sheet of the preparation method of aluminum refining agent provided in an embodiment of the present invention.
Embodiment
A kind of aluminum refining agent provided in an embodiment of the present invention includes K2MgCl4、KMgCl3、Na2SiF6、Na3AlF6、
Na2CO3And CaF2, the content of said components by mass percentage is：K2MgCl4：30~45%, KMgCl3：40~55%,
Na2SiF6：3~5%, Na3AlF6：2~5%, Na2CO3：4~6%, CaF2：2~3%.
With anhydrous villaumite synthetic KMgCl3And K2MgCl4Based on, KMgCl3And K2MgCl4The shape in 424 DEG C and 465 DEG C
Into Low melting point eutectic, it is swift in response when in use.
Na2SiF6And Na3AlF6The characteristics of be that fusing point is of a relatively high, hygroscopicity is small, and catabolite makes solid-oxide and aluminium
Interface wet ability between liquid is reduced, and slag is easily separated with aluminium liquid, and promotes the drying of slag, and still, excessive fluoride can be sent out
Raw fierce exothermic reaction, produces toxic gas.Wherein Na3AlF6It is the main component for improving purification slagging-off ability, can adsorbs
Aluminum oxide is dissolved, surface tension when and can improves and aluminium liquid contacts, is easy to separate with aluminium liquid.
Na2SiF6Decomposed under temperature of aluminum liquid：
Na2SiF6→2NaF+SiF4
SiF4Gas is evaporated into, plays part degasification, Na2SiF6Following reaction is produced with oxide inclusion：
Na2SiF6+2Al2O3→Na3AlF6+3SiO2+AlF3
The Na of generation3AlF6There is absorption Al2O3Effect, also can and SiO2With reference to block slag is generated, it is easy to remove.
NaF can corrode Al2O3Metal body on-Al interfaces, depart from oxide-film machinery, be dissolved among refining agent, from
And have the function that efficiently to remove the gred, Trace Sodium can also be discharged and act what is gone bad.
Na2CO3CO is decomposed to give off in aluminium liquid2, bubble dehydrogenation in uphill process, simultaneously as be oxygenatedchemicals,
Also the effect of exothermic mixture can be played.
A kind of aluminum refining agent provided in an embodiment of the present invention can also include CaMg (CO3)2And K2SiF6In one kind
Or two kinds, wherein, CaMg (CO3)2Effect and Na2CO3Effect in aluminium liquid is similar, K2SiF6Effect and Na2SiF6Make
With similar, CaMg (CO3)2And K2SiF6One or both of content by mass percentage be 4~19%.
A kind of aluminum refining agent provided in an embodiment of the present invention is that low melting point efficiently removes the gred aluminum refining agent, is applied to
Inert gas-refining agent is mixed to blow purifying method, and the refining effect that inert gas-refining agent is mixed to blow purifying method is pure by inert gas itself
The restriction of degree, although using strict purification measures, also always contain a certain amount of moisture and oxygen, this gas is blown into
After aluminium liquid, thin and compact oxide-film can be formed in the bubble surface being blown into, so as to hinder the hydrogen in melt to enter in bubble, is made
Outgassing rate is had a greatly reduced quality.
If a certain amount of aluminum refining agent provided in an embodiment of the present invention, gas are introduced while inert gas is blown into
The refining agent film that bubble surface can be melted is surrounded, and can separate the contact of moisture and oxygen with aluminium liquid in bubble, being allowed to can not
Formed oxide-film, even if there is oxide generation, can also be refined agent film and be adsorbed, can effectively remove molten aluminum, almag,
Sodium, lithium and calcium in alumin(i)um zinc alloy, coordinate inert gas refining sodium content minimum can be reduced into below 1ppm in casting,
And various non-metallic inclusions can be removed, such as oxide, carbide and boride, efficiently removing for melt can be greatly increased
Slag degassing effect, so as to effectively improve the effect of refining.
The efficient slagging-off ability of refining agent be by suction-operated of the refining agent to oxide inclusion in melt and dissolution,
And mutual chemical action is determined.
Because oxide inclusion is not wetted by aluminum, the interfacial tension between the two is very big, and the embodiment of the present invention carries
It is wetting to oxide inclusion for low melting point refining agent, and interfacial tension between the two is very small, in refining agent absorption melt
Oxide inclusion after, the surface free energy of system can be made reduce, therefore, the refining agent has the energy of automatic absorbing oxide inclusion
Power, meanwhile, and because the interfacial tension of the refining agent and aluminium liquid is very big, it is good with absorption property, and the ability that efficiently removes the gred is strong,
The characteristics of aluminium slag good separating effect.
Low melting point refining agent degasification feature is mainly manifested in three aspects：
(1) refining agent is with oxidizing slag, such as γ-Al2O3Complex compound γ-the Al of formation2O3XH removing, and remove by oxygen
Change and be mingled with absorbed part complexing H；
(2) refining agent, which produces, decomposes or forms gaseous products when being interacted with melt, so as to be diffused dehydrogenation；
(3) atomic hydrogen of dissolving is caused to become to be more prone to Atmospheric Diffusion because bath surface oxide-film is dissolved.
The embodiment of the present invention additionally provides a kind of preparation method of aluminum refining agent, for preparing above-mentioned alloy refining
Agent, it is a kind of flow chart of the preparation method of aluminum refining agent provided in an embodiment of the present invention referring to Fig. 1, including following step
Suddenly：
Step 1：Step 1：61.0% KCl and 39.0% MgCl are taken by mass percentage2Mixing, is warming up to 500 DEG C
Melt, then K is made in crystallisation by cooling2MgCl4；
Step 2：43.9% KCl and 56.1% MgCl are taken by mass percentage2Mixing, is warming up to 500 DEG C of meltings, so
KMgCl is made in crystallisation by cooling afterwards3；
Step 3：Take K obtained above2MgCl4And KMgCl3, with Na2SiF6、Na3AlF6、Na2CO3And CaF2Mixing, rise
Temperature is to 600~650 DEG C of meltings, and aluminum refining agent is made in crystallisation by cooling after being then incubated 1~2 hour at 600~650 DEG C.
Wherein, K2MgCl4、KMgCl3、Na2SiF6、Na3AlF6、Na2CO3And CaF2Content by mass percentage is：
K2MgCl4：30~45%, KMgCl3：40~55%, Na2SiF6：3~5%, Na3AlF6：2~5%, Na2CO3：4~6% Hes
CaF2：2~3%.
Detailed preparation process is illustrated with embodiment below.
Embodiment 1
Step 1：Weigh 18.3kg KCl and 11.7kg MgCl2Mixing and ball milling to granularity is less than 325 mesh, heats up 500 DEG C and melts
Melt, crystallized after cooling, 30kg K are made in the particle for being crushed to 2~5mm2MgCl4；
Step 2：Weigh 24.1kg KCl and 30.9kg MgCl2, first by 24.1kg KCl and 15.4kg MgCl2Mixing
It is milled to granularity and is less than 325 mesh, is warming up to 500 DEG C of meltings, adds remaining 15.5kg MgCl2Until all meltings, cooling
After crystallize, 55kg KMgCl are made in the particle for being crushed to 5~10mm3；
Step 3：Weigh 30kg K2MgCl4、55kg KMgCl3、3kg Na2SiF6、5kg Na3AlF6、4kg Na2CO3With
3kg CaF2, above several material mixing and ball millings to 325 mesh, 600~650 DEG C of meltings will be warming up to, 1 is incubated at 600~650 DEG C
Remove the crystallization water within~2 hours, crystallized after cooling, the aluminium conjunction that the embodiment of the present invention 1 provides is made after being crushed to 2~5mm particle
Gold refining agent.
Embodiment 2
Step 1：Weigh 27.5kg KCl and 17.5kg MgCl2Mixing and ball milling to granularity is less than 325 mesh, heats up 500 DEG C and melts
Melt, crystallized after cooling, be crushed to the obtained 45kg K of 2~5mm particles2MgCl4；
Step 2：Weigh KCl 17.6kg and 22.4kg MgCl2, first by 17.6kg KCl and 11.2kg MgCl2Mixing
It is milled to granularity and is less than 325 mesh, is warming up to 500 DEG C of meltings, adds remaining 11.2kg MgCl2Until all meltings, cooling
After crystallize, 40kg KMgCl are made in the particle for being crushed to 2~5mm3；
Step 3：Weigh 45kg K2MgCl4、40kg KMgCl3、5kg Na2SiF6、2kg Na3AlF6、6kg Na2CO3With
2kg CaF2, above several material mixing and ball millings to 325 mesh, 600~650 DEG C of meltings will be warming up to, 1 is incubated at 600~650 DEG C
Remove the crystallization water within~2 hours, crystallized after cooling, the aluminium conjunction that the embodiment of the present invention 2 provides is made after being crushed to 2~5mm particle
Gold refining agent.
Embodiment 3
Step 1：Weigh 22.9kg KCl and 14.6kg MgCl2Mixing and ball milling to granularity is less than 325 mesh, heats up 500 DEG C and melts
Melt, crystallized after cooling, 37.5kg K are made in the particle for being crushed to 2~5mm2MgCl4；
Step 2：Weigh 20.9kg KCl and 26.6kg MgCl2, first by 20.9kg KCl and 13.3kg MgCl2Mixing
It is milled to granularity and is less than 325 mesh, is warming up to 500 DEG C of meltings, adds remaining 13.3kg MgCl2Until all meltings, cooling
After crystallize, 47.5kg KMgCl are made in the particle for being crushed to 2~5mm3；
Step 3：Weigh 37.5kg K2MgCl4、47.5kg KMgCl3、4kg Na2SiF6、3.5kg Na3AlF6、5kg
Na2CO3With 2.5kg CaF2, will more than several material mixing and ball millings to 325 mesh, be warming up to 600~650 DEG C of meltings, 600~
650 DEG C of insulations remove the crystallization water in 1~2 hour, are crystallized after cooling, and the embodiment of the present invention 3 is made after being crushed to 2~5mm particle
The aluminum refining agent of offer.
In summary, a kind of aluminum refining agent provided in an embodiment of the present invention includes K2MgCl4、KMgCl3、Na2SiF6、
Na3AlF6、Na2CO3And CaF2, wherein, K2MgCl4And KMgCl3Low melting point eutectic is generated at high temperature, is formed the present invention and is provided
Aluminum refining agent basic substance, can in aluminium liquid rapid dispersion and effectively remove molten aluminum in nonmetal inclusion
Thing；Na2SiF6And Na3AlF6Catabolite at high temperature can effectively reduce the interface profit between solid-oxide and aluminium liquid
It is moist, promote oxide inclusion and aluminium liquid separation；Na2CO3CO is decomposed to give off in high temperature aluminium liquid2, can effectively go dehydrogenation；
CaF2The surface tension of fused salt mixt can be increased, make the fused salt spheroidizing of absorbing oxide, be easy to and melt separation, reduction are solid
Slag wrap aluminium and caused by loss.
In addition, applied to inert gas-refining agent is mixed blow purifying method when, chlorine can be substituted to carry out furnace refining, reduced
The use of chlorine in refining process；Edge crack can be reduced in the high magnesium alloy of casting, so that can in extrudate
Increase the speed of extrusion and the life-span of increase mould.
Invention described above embodiment is not intended to limit the scope of the present invention..
Claims (7)
- A kind of 1. aluminum refining agent, it is characterised in that including：K2MgCl4、KMgCl3、Na2SiF6、Na3AlF6、Na2CO3With CaF2。
- 2. aluminum refining agent according to claim 1, it is characterised in that the K2MgCl4、KMgCl3、Na2SiF6、 Na3AlF6、Na2CO3And CaF2Content by mass percentage is：K2MgCl4：30~45%, KMgCl3：40~55%, Na2SiF6：3~5%, Na3AlF6：2~5%, Na2CO3：4~6% and CaF2：2~3%.
- 3. aluminum refining agent according to claim 1, it is characterised in that also including CaMg (CO3)2And K2SiF6In one Kind or two kinds.
- 4. aluminum refining agent according to claim 3, it is characterised in that the CaMg (CO3)2And K2SiF6In one kind Or two kinds of contents by mass percentage are 4~19%.
- 5. a kind of preparation method of aluminum refining agent, for preparing the aluminum refining agent described in claim 1, its feature exists In comprising the following steps：Step 1：61.0% KCl and 39.0% MgCl are taken by mass percentage2Mixing, is warming up to 500 DEG C of meltings, Ran Houleng But crystallize and K is made2MgCl4；Step 2：43.9% KCl and 56.1% MgCl are taken by mass percentage2Mixing, is warming up to 500 DEG C of meltings, Ran Houleng But crystallize and KMgCl is made3；Step 3：Take K obtained above2MgCl4And KMgCl3, with Na2SiF6、Na3AlF6、Na2CO3And CaF2Mixing, is warming up to 600~650 DEG C of meltings, the aluminum refining agent is made in crystallisation by cooling after being then incubated 1~2 hour at 600~650 DEG C.
- 6. the preparation method of aluminum refining agent according to claim 5, it is characterised in that the K2MgCl4、KMgCl3、 Na2SiF6、Na3AlF6、Na2CO3And CaF2Content by mass percentage is：K2MgCl4：30~45%, KMgCl3：40~ 55%, Na2SiF6：3~5%, Na3AlF6：2~5%, Na2CO3：4~6% and CaF2：2~3%.
- 7. the preparation method of aluminum refining agent according to claim 5, it is characterised in that described KCl, MgCl2、 K2MgCl4、KMgCl3、Na2SiF6、Na3AlF6、Na2CO3And CaF2It is milled to granularity and is less than 325 mesh.
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Cited By (6)
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| CN111041264A (en) * | 2020-01-16 | 2020-04-21 | 深圳市新星轻合金材料股份有限公司 | Preparation method of aluminum alloy refining agent |
| CN111072048A (en) * | 2020-01-16 | 2020-04-28 | 深圳市新星轻合金材料股份有限公司 | K2MgCl4Preparation method of (1) |
| CN111118327A (en) * | 2020-01-16 | 2020-05-08 | 深圳市新星轻合金材料股份有限公司 | K3Mg2Cl7Preparation method of (1) |
| CN111155010A (en) * | 2020-01-16 | 2020-05-15 | 深圳市新星轻合金材料股份有限公司 | Preparation method of magnesium-aluminum-titanium alloy |
| CN111233013A (en) * | 2020-01-16 | 2020-06-05 | 深圳市新星轻合金材料股份有限公司 | KMgCl3Preparation method of (1) |
| CN113214801A (en) * | 2021-05-19 | 2021-08-06 | 中国科学院上海应用物理研究所 | Low cost MgCl based on bischofite2Preparation method of (E) -KCl eutectic salt |
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