CN107779633A - A kind of aluminium alloy high-efficiency refining agent and preparation method thereof - Google Patents

A kind of aluminium alloy high-efficiency refining agent and preparation method thereof Download PDF

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CN107779633A
CN107779633A CN201710835564.0A CN201710835564A CN107779633A CN 107779633 A CN107779633 A CN 107779633A CN 201710835564 A CN201710835564 A CN 201710835564A CN 107779633 A CN107779633 A CN 107779633A
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parts
refining agent
aluminium alloy
powder
alloy high
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梁春才
梁健
梁祥友
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GUANGXI PINGGUO ALUMINUM PRECISION CASTING Co Ltd
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GUANGXI PINGGUO ALUMINUM PRECISION CASTING Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
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Abstract

The invention discloses a kind of aluminium alloy high-efficiency refining agent and preparation method thereof, belong to aluminum alloy processing technology field.The refining agent is in units of parts by weight, including following component：30 40 parts of KCl, 20 30 parts of NaCl, KNO330 40 parts, A1F36 11 parts, MgF238 parts, Na3A1F64 10 parts, Na2SiF627 parts, 0.2 0.6 parts of FNd, F30.5 1.1 parts of La.The present invention can efficiently remove small size oxide and be mingled with, and good impurity removing effect, deaeration capability is strong, and affinability is high, can enable aluminum alloy to content in melt and be reduced to below 0.0816ml/100gAl.

Description

A kind of aluminium alloy high-efficiency refining agent and preparation method thereof
Technical field
The invention belongs to aluminum alloy processing technology field, and in particular to a kind of aluminium alloy high-efficiency refining agent and its preparation side Method.
Background technology
China ranked third in the aluminium consumption figure billboard of countries in the world, although the yield in Chinese aluminium occupy the world Second, but the aluminium that uses of China uses import mostly, is aluminium importer the biggest in the world.Why occur this existing Shape, it is primarily due on production process control, control of product quality and production scale etc. are in terms of these, Chinese aluminium row Industry is also not by a long sight compared with advanced country.Most of all, the aluminium base supply respect China in high quality shows output capacity not The problem of foot and breach are greatly main.In melting, casting cycle, aluminium and its alloy are easily oxidized and absorbed gas, this Kind of characteristic causes gas and field trash easily to be formed in aluminium liquid, then causes the shrinkage porosite of casting, stomata, crackle, shrinkage cavity etc. one Series of defect, and these defects can largely cause the performance such as the fatigue resistance of casting, intensity, plasticity, anti-corrosion substantially to become Difference, directly the quality of product can be decreased obviously, serious even can cause scrapping for whole casting, these all cause aluminium and The application of its alloy receives limitation largely.
The requirement of hydrogen content, non-metallic inclusion content in aluminium alloy can change with the difference of its purposes.As answered Aluminum alloy hydrogen content typically no more than 0.10ml/100gAl in terms of Aeronautics and Astronautics, inclusion content can not mistake Height, in the size of non-metallic inclusion requirement can not have 1-5 μm of particle and aggregation.In addition, the hydrogen content requirement of aluminium exists 0.06ml/100gAl is less than in terms of the electronics industry of high quality.As can be seen here, study gas present in aluminium and its alloy and Field trash, the mechanism of production of gas and field trash is understood, by developing efficient, inexpensive new refining agent, so as to reach The effect of the air content and non-metallic inclusion content in aluminium alloy melt is reduced, the performance for improving aluminum alloy materials is heavy to closing Want.The raising of cleaning molten technological level directly influences the raising of aluminum alloy materials metallurgical quality, and therefore, research melt is net Chemical industry skill oneself through be that countries in the world are metallurgical and founding in terms of the problem paid special attention to of scholar.
The content of the invention
It is an object of the invention to provide a kind of aluminium alloy high-efficiency refining agent and preparation method thereof, to solve in aluminium alloy The problem of hydrogen content, high non-metallic inclusion content, realize that the air content in reduction aluminium alloy melt and non-metallic inclusion contain The target of amount, improve the performance of aluminum alloy materials.
To solve above technical problem, the present invention uses following technical scheme：
A kind of aluminium alloy high-efficiency refining agent, in units of parts by weight, including following component：KCl 30-40 parts, NaCl 20-30 parts, KNO330-40 parts, A1F36-11 parts, MgF23-8 parts, Na3A1F64-10 parts, Na2SiF62-7 parts, FNd 0.2-0.6 parts, F3La 0.5-1.1 parts.
Preferably, the refining agent is in units of parts by weight, including following component：KCl 33-38 parts, NaCl 24-27 Part, KNO332-35 parts, A1F37-10 parts, MgF24-6 parts, Na3A1F65-7 parts, Na2SiF63-5 parts, FNd 0.3-0.5 Part, F3La 0.7-0.9 parts.
It is highly preferred that the refining agent is in units of parts by weight, including following component：35 parts of KCl, 26 parts of NaCl, KNO333 parts, A1F38 parts, MgF25 parts, Na3A1F66 parts, Na2SiF64 parts, 0.4 part of FNd, F30.8 part of La.
Further, the preparation method of the aluminium alloy high-efficiency refining agent, comprises the following steps：
S1：By La2O3It is dissolved in hydrochloric acid and is diluted to 120-130g/L, heated solution adds 48% to 72-75 DEG C Hydrofluoric acid, stirring, obtain sediment, then sediment is washed, filtered, is dried, is crushed, vacuum dehydration obtains F3La powder；
S2：By Nd2O3It is dissolved in hydrochloric acid and is diluted to 120-130g/L, heated solution adds 48% to 72-75 DEG C Hydrofluoric acid, stirring, obtains sediment, then sediment is washed, filtered, is dried, is crushed, the obtained FNd powder of vacuum dehydration；
S3：By KCl, NaCl, KNO3、A1F3、MgF2、Na3A1F6、Na2SiF6Powder is put into mixer and is stirred, mixing Uniformly, sieve；
S4：The powder being well mixed in step S3 is placed in drying oven and dried, is cooled down after being incubated 30min, is sieved, Produce aluminium alloy high-efficiency refining agent.
Preferably, the dehydration in step S1 and S2 is carried out under conditions of vacuum is 0.5-0.8MPa.
Preferably, F in step S1 and S23La powder and FNd dried bean noodles are dry to water content≤2%, are crushed to granularity≤2mm.
Preferably, powder crosses 10-20 mesh sieves in step S3.
Preferably, powder is dried under 200-260 DEG C of temperature conditionss in step S4, is dried to water content≤2%, after 10-20 mesh sieves.
It is highly preferred that powder is dried under 250 DEG C of temperature conditionss.
The invention has the advantages that：
1. the present invention uses Na2SiF6Dissolve A12O3, FNd and F3La reduces A12O3Technical scheme, using its mainly into Divide and do not chemically reacted with Al, and the generation of itself heat energy is not fused to the gas N of aluminium alloy melt at high temperature2、CO2, NO, rise To refining catharsis, it can efficiently remove small size oxide and be mingled with, good impurity removing effect, deaeration capability is stronger, and it is refined Ability significantly improves, and can enable aluminum alloy to content in melt and be reduced to below 0.0816ml/100gAl.
2. the refining agent of the present invention is the most rational combination of media drawn after repetition test and meticulously screening, slagging-off Effect is more than 90%, and refining agent does not chemically react with metal and furnace lining, controls heating effect, reduces iron loss, melting The microstructure compactness of aluminium alloy round cast ingot afterwards is uniform, substantially without loose, slag inclusion the defects of, add aluminium alloy round cast ingot The uniformity of interior tissue and the refinement of crystal grain, improve the quality and processing characteristics of rear process aluminium extrusion alloy profile.
Embodiment
The embodiment of the present invention is described further with reference to embodiment, following examples are only used for more Clearly demonstrate technical scheme, and can not be limited the scope of the invention with this.
In embodiment, a kind of aluminium alloy high-efficiency refining agent, in units of parts by weight, including following component：KCl 30-40 Part, NaCl 20-30 parts, KNO330-40 parts, A1F36-11 parts, MgF23-8 parts, Na3A1F64-10 parts, Na2SiF62-7 parts, FNd 0.2-0.6 parts, F3La 0.5-1.1 parts；
The preparation method of aluminium alloy high-efficiency refining agent comprising above raw material and component, comprises the following steps：
S1：By La2O3It is dissolved in hydrochloric acid and is diluted to 120-130g/L, heated solution adds 48% to 72-75 DEG C Hydrofluoric acid, stirring, obtain sediment, then sediment is washed, filtered, dry to water content≤2%, be crushed to granularity≤2mm, Vacuum is dehydrated to obtain F under conditions of being 0.5-0.8MPa3La powder；
S2：By Nd2O3It is dissolved in hydrochloric acid and is diluted to 120-130g/L, heated solution adds 48% to 72-75 DEG C Hydrofluoric acid, stirring, obtain sediment, then sediment is washed, filtered, dry to water content≤2%, be crushed to granularity≤2mm, Vacuum carries out being dehydrated obtained FNd powder under conditions of being 0.5-0.8MPa；
S3：By KCl, NaCl, KNO3、A1F3、MgF2、Na3A1F6、Na2SiF6Powder is put into mixer and is stirred, mixing Uniformly, 10-20 mesh sieves are crossed；
S4：The powder being well mixed in step S3 is placed in the drying oven that temperature is 200-260 DEG C and dried, is dried To water content≤2%, cooled down after being incubated 30min, after 10-20 mesh sieves, produce aluminium alloy high-efficiency refining agent.
Embodiment 1
A kind of aluminium alloy high-efficiency refining agent, in units of parts by weight, including following component：30 parts of KCl, NaCl 30 Part, KNO330 parts, A1F311 parts, MgF24 parts, Na3A1F65 parts, Na2SiF67 parts, 0.2 part of FNd, F3La0.7 parts；
The preparation method of aluminium alloy high-efficiency refining agent comprising above raw material and component, comprises the following steps：
S1：By La2O3It is dissolved in hydrochloric acid and is diluted to 120g/L, heated solution adds 48% hydrofluoric acid to 75 DEG C, Stirring, obtains sediment, then sediment is washed, filtered, dries to water content≤2%, be crushed to granularity≤2mm, in vacuum To be dehydrated to obtain F under conditions of 0.6MPa3La powder；
S2：By Nd2O3It is dissolved in hydrochloric acid and is diluted to 120g/L, heated solution adds 48% hydrofluoric acid to 75 DEG C, Stirring, obtains sediment, then sediment is washed, filtered, dries to water content≤2%, be crushed to granularity≤2mm, in vacuum To carry out being dehydrated obtained FNd powder under conditions of 0.6MPa；
S3：By KCl, NaCl, KNO3、A1F3、MgF2、Na3A1F6、Na2SiF6Powder is put into mixer and is stirred, mixing Uniformly, 10 mesh sieves are crossed；
S4：It is to be dried in 260 DEG C of drying oven that the powder being well mixed in step S3 is placed on into temperature, is dried to containing Water≤2%, cooled down after being incubated 30min, after 10 mesh sieves, produce aluminium alloy high-efficiency refining agent.
Embodiment 2
A kind of aluminium alloy high-efficiency refining agent, in units of parts by weight, including following component：40 parts of KCl, NaCl 24 Part, KNO340 parts, A1F37 parts, MgF23 parts, Na3A1F64 parts, Na2SiF63 parts, 0.6 part of FNd, F30.5 part of La；
The preparation method of aluminium alloy high-efficiency refining agent comprising above raw material and component, comprises the following steps：
S1：By La2O3It is dissolved in hydrochloric acid and is diluted to 130g/L, heated solution adds 48% hydrofluoric acid to 74 DEG C, Stirring, obtains sediment, then sediment is washed, filtered, dries to water content≤2%, be crushed to granularity≤2mm, in vacuum To be dehydrated to obtain F under conditions of 0.5MPa3La powder；
S2：By Nd2O3It is dissolved in hydrochloric acid and is diluted to 130g/L, heated solution adds 48% hydrofluoric acid to 74 DEG C, Stirring, obtains sediment, then sediment is washed, filtered, dries to water content≤2%, be crushed to granularity≤2mm, in vacuum To carry out being dehydrated obtained FNd powder under conditions of 0.5MPa；
S3：By KCl, NaCl, KNO3、A1F3、MgF2、Na3A1F6、Na2SiF6Powder is put into mixer and is stirred, mixing Uniformly, 20 mesh sieves are crossed；
S4：It is to be dried in 250 DEG C of drying oven that the powder being well mixed in step S3 is placed on into temperature, is dried to containing Water≤2%, cooled down after being incubated 30min, after 20 mesh sieves, produce aluminium alloy high-efficiency refining agent.
Embodiment 3
A kind of aluminium alloy high-efficiency refining agent, in units of parts by weight, including following component：33 parts of KCl, NaCl 20 Part, KNO332 parts, A1F36 parts, MgF28 parts, Na3A1F610 parts, Na2SiF62 parts, 0.3 part of FNd, F31.1 parts of La；
The preparation method of aluminium alloy high-efficiency refining agent comprising above raw material and component, comprises the following steps：
S1：By La2O3It is dissolved in hydrochloric acid and is diluted to 125g/L, heated solution adds 48% hydrofluoric acid to 72 DEG C, Stirring, obtains sediment, then sediment is washed, filtered, dries to water content≤2%, be crushed to granularity≤2mm, in vacuum To be dehydrated to obtain F under conditions of 0.8MPa3La powder；
S2：By Nd2O3It is dissolved in hydrochloric acid and is diluted to 125g/L, heated solution adds 48% hydrofluoric acid to 72 DEG C, Stirring, obtains sediment, then sediment is washed, filtered, dries to water content≤2%, be crushed to granularity≤2mm, in vacuum To carry out being dehydrated obtained FNd powder under conditions of 0.8MPa；
S3：By KCl, NaCl, KNO3、A1F3、MgF2、Na3A1F6、Na2SiF6Powder is put into mixer and is stirred, mixing Uniformly, 20 mesh sieves are crossed；
S4：It is to be dried in 200 DEG C of drying oven that the powder being well mixed in step S3 is placed on into temperature, is dried to containing Water≤2%, cooled down after being incubated 30min, after 20 mesh sieves, produce aluminium alloy high-efficiency refining agent.
Embodiment 4
A kind of aluminium alloy high-efficiency refining agent, in units of parts by weight, including following component：38 parts of KCl, NaCl 27 Part, KNO335 parts, A1F310 parts, MgF26 parts, Na3A1F67 parts, Na2SiF65 parts, 0.5 part of FNd, F30.9 part of La；
The preparation method of aluminium alloy high-efficiency refining agent comprising above raw material and component, comprises the following steps：
S1：By La2O3It is dissolved in hydrochloric acid and is diluted to 125g/L, heated solution adds 48% hydrofluoric acid to 75 DEG C, Stirring, obtains sediment, then sediment is washed, filtered, dries to water content≤2%, be crushed to granularity≤2mm, in vacuum To be dehydrated to obtain F under conditions of 0.5MPa3La powder；
S2：By Nd2O3It is dissolved in hydrochloric acid and is diluted to 125g/L, heated solution adds 48% hydrofluoric acid to 75 DEG C, Stirring, obtains sediment, then sediment is washed, filtered, dries to water content≤2%, be crushed to granularity≤2mm, in vacuum To carry out being dehydrated obtained FNd powder under conditions of 0.5MPa；
S3：By KCl, NaCl, KNO3、A1F3、MgF2、Na3A1F6、Na2SiF6Powder is put into mixer and is stirred, mixing Uniformly, 10 mesh sieves are crossed；
S4：It is to be dried in 200 DEG C of drying oven that the powder being well mixed in step S3 is placed on into temperature, is dried to containing Water≤2%, cooled down after being incubated 30min, after 10 mesh sieves, produce aluminium alloy high-efficiency refining agent.
Embodiment 5
A kind of aluminium alloy high-efficiency refining agent, in units of parts by weight, including following component：35 parts of KCl, NaCl 26 Part, KNO333 parts, A1F38 parts, MgF25 parts, Na3A1F66 parts, Na2SiF64 parts, 0.4 part of FNd, F30.8 part of La；
The preparation method of aluminium alloy high-efficiency refining agent comprising above raw material and component, comprises the following steps：
S1：By La2O3It is dissolved in hydrochloric acid and is diluted to 130g/L, heated solution adds 48% hydrofluoric acid to 75 DEG C, Stirring, obtains sediment, then sediment is washed, filtered, dries to water content≤2%, be crushed to granularity≤2mm, in vacuum To be dehydrated to obtain F under conditions of 0.5MPa3La powder；
S2：By Nd2O3It is dissolved in hydrochloric acid and is diluted to 130g/L, heated solution adds 48% hydrofluoric acid to 75 DEG C, Stirring, obtains sediment, then sediment is washed, filtered, dries to water content≤2%, be crushed to granularity≤2mm, in vacuum To carry out being dehydrated obtained FNd powder under conditions of 0.5MPa；
S3：By KCl, NaCl, KNO3、A1F3、MgF2、Na3A1F6、Na2SiF6Powder is put into mixer and is stirred, mixing Uniformly, 10 mesh sieves are crossed；
S4：It is to be dried in 250 DEG C of drying oven that the powder being well mixed in step S3 is placed on into temperature, is dried to containing Water≤2%, cooled down after being incubated 30min, after 10 mesh sieves, produce aluminium alloy high-efficiency refining agent.
Comparative example 1
Refining agent component and preparation method are substantially the same manner as Example 1, difference do not contained in component FNd, F3La。
Comparative example 2
Refining agent component and preparation method are substantially the same manner as Example 1, and difference is not containing A1F in component3、 MgF2、Na3A1F6、Na2SiF6。
Comparative example 3
Refining agent component and preparation method are substantially the same manner as Example 1, difference do not contained in component FNd, F3La、A1F3、MgF2、Na3A1F6、Na2SiF6。
Embodiment according to above-described embodiment 1-5 and comparative example 1-3 is tested, and measures hydrogen content in aluminium alloy melt And dregginess, it the results are shown in Table 1.
Hydrogen content and slag inclusion scale in the aluminium alloy melt of table 1
From upper table embodiment 1-5, the dehydrogenation slagging-off effect of purifying aluminium alloy melt method of the present invention is good, utilizes this essence Hydrogen content is less than 0.082ml/100gAl in melt after refining agent dehydrogenation, and hydrogen addition rate is more than 67.18%；Dregginess in melt after slagging-off Less than 0.0035, slagging-off rate is more than 90%, more than requirements of the national standard, meets the requirement of aluminium alloy crudy.From comparative example 1-3 Understand, at least part of component is lacked in refining agent component by the effect to reducing its dehydrogenation slagging-off, it is seen that each group of the present invention divides it Between mutually promote.
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to is assert The specific implementation of the present invention is confined to these explanations, for person of an ordinary skill in the technical field, is not departing from On the premise of present inventive concept, some simple deduction or replace can also be made, should all be considered as belonging to the present invention by being submitted Claims determine scope of patent protection.

Claims (9)

  1. A kind of 1. aluminium alloy high-efficiency refining agent, it is characterised in that in units of parts by weight, including following component：KCl 30-40 Part, NaCl 20-30 parts, KNO330-40 parts, A1F36-11 parts, MgF23-8 parts, Na3A1F64-10 parts, Na2SiF6 2-7 Part, FNd 0.2-0.6 parts, F3La 0.5-1.1 parts.
  2. 2. aluminium alloy high-efficiency refining agent according to claim 1, it is characterised in that the refining agent is using parts by weight to be single Position, including following component：KCl 33-38 parts, NaCl 24-27 parts, KNO332-35 parts, A1F37-10 parts, MgF24-6 parts, Na3A1F65-7 parts, Na2SiF63-5 parts, FNd 0.3-0.5 parts, F3La 0.7-0.9 parts.
  3. 3. aluminium alloy high-efficiency refining agent according to claim 2, it is characterised in that the refining agent is using parts by weight to be single Position, including following component：35 parts of KCl, 26 parts of NaCl, KNO333 parts, A1F38 parts, MgF25 parts, Na3A1F66 parts, Na2SiF64 parts, 0.4 part of FNd, F30.8 part of La.
  4. A kind of 4. preparation method of aluminium alloy high-efficiency refining agent according to claim any one of 1-3, it is characterised in that Comprise the following steps：
    S1：By La2O3It is dissolved in hydrochloric acid and is diluted to 120-130g/L, heated solution adds 48% hydrogen fluorine to 72-75 DEG C Acid, stirring, obtain sediment, then sediment is washed, filtered, is dried, is crushed, vacuum dehydration obtains F3La powder；
    S2：By Nd2O3It is dissolved in hydrochloric acid and is diluted to 120-130g/L, heated solution adds 48% hydrogen fluorine to 72-75 DEG C Acid, stirring, obtains sediment, then sediment is washed, filtered, is dried, is crushed, the obtained FNd powder of vacuum dehydration；
    S3：By KCl, NaCl, KNO3、A1F3、MgF2、Na3A1F6、Na2SiF6Powder is put into mixer and is stirred, and is well mixed, Sieving；
    S4：The powder being well mixed in step S3 is placed in drying oven and dried, is cooled down after being incubated 30min, sieves, produces Aluminium alloy high-efficiency refining agent.
  5. 5. the preparation method of aluminium alloy high-efficiency refining agent according to claim 4, it is characterised in that the step S1 and Dehydration in S2 is carried out under conditions of vacuum is 0.5-0.8MPa.
  6. 6. the preparation method of aluminium alloy high-efficiency refining agent according to claim 4, it is characterised in that the step S1 and F in S23La powder and FNd dried bean noodles are dry to water content≤2%, are crushed to granularity≤2mm.
  7. 7. the preparation method of aluminium alloy high-efficiency refining agent according to claim 4, it is characterised in that in the step S3 Powder crosses 10-20 mesh sieves.
  8. 8. the preparation method of aluminium alloy high-efficiency refining agent according to claim 4, it is characterised in that in the step S4 Powder is dried under 200-260 DEG C of temperature conditionss, is dried to water content≤2%, after 10-20 mesh sieves.
  9. 9. the preparation method of aluminium alloy high-efficiency refining agent according to claim 8, it is characterised in that powder is at 250 DEG C Temperature conditionss under dry.
CN201710835564.0A 2017-09-15 2017-09-15 A kind of aluminium alloy high-efficiency refining agent and preparation method thereof Pending CN107779633A (en)

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CN112458312A (en) * 2020-11-25 2021-03-09 中国恩菲工程技术有限公司 Refining agent for smelting aluminum or aluminum alloy and application thereof

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CN102226239A (en) * 2011-06-14 2011-10-26 华南理工大学 Refining flux used for purifying and processing aluminum or aluminum alloy melt, and its preparation method

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CN112458312A (en) * 2020-11-25 2021-03-09 中国恩菲工程技术有限公司 Refining agent for smelting aluminum or aluminum alloy and application thereof

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Application publication date: 20180309