CN1260397C - Production method of high purity aluminium scandium alloy - Google Patents
Production method of high purity aluminium scandium alloy Download PDFInfo
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- CN1260397C CN1260397C CN 03153785 CN03153785A CN1260397C CN 1260397 C CN1260397 C CN 1260397C CN 03153785 CN03153785 CN 03153785 CN 03153785 A CN03153785 A CN 03153785A CN 1260397 C CN1260397 C CN 1260397C
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- scandium
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Abstract
The present invention provides a method for producing high-purity aluminium and scandium alloy, which relates to the method that an aluminium refining electrolytic tank for the existing three-layer liquid is used, scandium chloride or scandium fluoride is added in an electrolyte, and the high-purity aluminium and scandium alloy is produced by electrolysis. The present invention is characterized in that the scandium chloride or the scandium fluoride is added in the electrolyte electrolyzed by the three-layer liquid to directly electrolyze and produce the high-purity aluminium and scandium alloy, and the electrolyte adopts fluorine chlorides or pure fluorides. The present invention has operation and control parameters that electrolytic temperature is from 650 DEG C to 850 DEG C, the working voltage of the electrolytic tank is from 4.0V to 7.0V, and electrolyte thickness is from 4.0cm to 15.0cm. Because the present invention adopts the method that the scandium chloride or the scandium fluoride is directly added in the aluminium refining electrolytic tank for the three-layer liquid to electrolyze and separate out scandium and aluminium together and to directly produce the high-purity aluminium and scandium alloy, the quality of the aluminum and scandium alloy can be greatly improved, a metal recovery rate can be improved at the same time, and productive cost is reduced.
Description
Technical field
A kind of production method of rafifinal scandium alloy.Relate to the existing three layers of liquid aluminum refining electrolyzing cell of a kind of utilization, in ionogen, add Scium trichloride or scandium fluoride, the method for electrolysis production rafifinal scandium alloy.
Background technology
The production method of aluminum scandium alloy is many now joins method with melting, and is that the high pure metal scandium is cooperated with aluminium fusion under argon shield, and this method is not easy to operate, scaling loss serious and the production process complexity of pure metal scandium, and the metal yield is low, involves great expense.Also have fluorochemical vacuum thermit reduction in addition, the used scandium fluoride of this method is to be made by Scium trioxide after purifying repeatedly and hydrofluoric acid reaction, and long flow path and metal yield are low, the cost height.Existing aluminum scandium alloy uses the Raw Aluminium manufacturing, and foreign matter contents such as contained silicon, iron, potassium, sodium are higher in the primary aluminum, are difficult to satisfy the composition requirement of aerospace industry to alloy.
Summary of the invention
The production method that the three layers of liquid electrolytic process of a kind of usefulness that the objective of the invention is to develop at above deficiency are produced the rafifinal scandium alloy, be under the prerequisite that does not change existing rafifinal electrolytic producer apparatus and production technique substantially, in three layers of electrolytic ionogen of liquid, add Scium trichloride or scandium fluoride, electrolysis production rafifinal scandium alloy, ionogen can adopt fluorochloride, also can adopt pure fluorochemical.This method can significantly reduce the foreign matter content in the aluminum scandium alloy, reduces the production cost of alloy simultaneously, promotes the large-scale application of aluminum scandium alloy.
Method of the present invention is achieved through the following technical solutions.
A kind of method of electrolysis production rafifinal scandium alloy is characterized in that Scium trichloride or scandium fluoride are added direct electrolysis production rafifinal scandium alloy in three layers of electrolytic ionogen of liquid, and ionogen adopts fluorochloride or pure fluorochemical, controls electrolytical proportioning and is:
(1) adopt the electrolytical weight percent of fluorochloride to consist of: aluminum fluoride AlF
320%~30%, Sodium Fluoride NaF10%~15%, bariumchloride BaCl
250%~60%, sodium chloride nacl 5%~10% adds the Scium trichloride ScCl that accounts for ionogen gross weight 1%~20% in ionogen
3Carry out electrolysis;
(2) adopt the weight percent of pure electrolysis of fluorides matter to consist of: aluminum fluoride AlF
330%~50%, Sodium Fluoride NaF 15%~30%, Calcium Fluoride (Fluorspan) CaF
215%~20%, barium fluoride BaF
215%~40%, in ionogen, add the scandium fluoride ScF that accounts for ionogen gross weight 1%~20%
3Carry out electrolysis;
Its operation controlled variable is: electrolysis temperature: 650 ℃~850 ℃, and electric tank working voltage: 4.0v~7.0v, electrolyte thickness: 4.0cm~15.0cm;
The weight percent that adds the Scium trichloride in the ionogen in the electrolytic process consists of: Scium trichloride ScCl
3:>98.5%, igloss<1%, oxide compound summation<0.2%, other impurity summation<0.3%;
The weight percent that adds the scandium fluoride in the ionogen in the electrolytic process consists of: scandium fluoride ScF
3:>98.5%, igloss<1%, oxide compound summation<0.2%, other impurity summation<0.3%.
The weight percent chemical constitution of the rafifinal scandium alloy of producing with method of the present invention is: Sc0.1%~2.0%, all the other are aluminium Al and unavoidable impurities, iron Fe<0.01% wherein, silicon Si<0.01%, other impurity summation<0.02%.
The present invention adopts and directly add Scium trichloride or scandium fluoride in three layers of liquid aluminum refining electrolyzing cell, the method that the common electrolysis of scandium and aluminium is separated out, direct production rafifinal scandium alloy can significantly improve the aluminum scandium alloy quality, simultaneously can improve metal recovery rate, reduce production costs.
Embodiment
A kind of method of electrolysis production aluminum scandium alloy is characterized in that Scium trichloride or scandium fluoride are added direct electrolysis production rafifinal scandium alloy in three layers of electrolytic ionogen of liquid, and ionogen can adopt fluorochloride, also can adopt pure fluorochemical.Processing condition are: controlling electrolytical proportioning is:
(1) adopts the fluorochloride ionogen: aluminum fluoride AlF
320%~30%, Sodium Fluoride NaF 10%~15%, bariumchloride BaCl
250%~60%, sodium chloride nacl 5%~10% adds 1%~20% scandium fluoride ScCl in ionogen
3Carry out electrolysis.
(2) adopt pure electrolysis of fluorides matter: aluminum fluoride AlF
330%~50%, Sodium Fluoride NaF 15%~30%, Calcium Fluoride (Fluorspan) CaF
215%~20%, barium fluoride BaF
215%~40%, in ionogen, add 1%~20% scandium fluoride ScF
3Carry out electrolysis.
Its operation controlled variable is: electrolysis temperature: 650 ℃-850 ℃, and electric tank working voltage: 4.0~7.0v, electrolyte thickness: 4.0~15.0cm.
The Scium trichloride in the electrolytic process in the adding ionogen or the chemical ingredients of scandium fluoride require to be respectively: the chemical ingredients of Scium trichloride requires: Scium trichloride ScCl
3:>98.5%, igloss<1%, oxide compound summation<0.2%, other impurity summation<0.3%; The chemical ingredients of scandium fluoride requires: scandium fluoride ScF
3:>98.5%, igloss<1%, oxide compound summation<0.2%, other impurity summation<0.3%.
The weight percent chemical constitution of the rafifinal scandium alloy of producing with method of the present invention is: scandium Sc0.1%~2.0%, all the other are aluminium Al and unavoidable impurities, iron Fe<0.01% wherein, silicon Si<0.01%, other impurity summation<0.02%.
Embodiment 1
Controlling electrolytical proportioning is: aluminum fluoride AlF
325%, Sodium Fluoride NaF 13%, bariumchloride BaCl
257%, sodium chloride nacl 5%, the Scium trichloride ScCl of adding 15% in ionogen
3Its operation controlled variable is: electrolysis temperature: 720 ℃, and electric tank working voltage: 4.5v, electrolyte thickness: 7.0cm.The chemical ingredients that adds the Scium trichloride in the ionogen in the electrolytic process requires: Scium trichloride ScCl
3:>98.5%, igloss<1%, oxide compound summation<0.2%, other impurity summation<0.3%.The weight percent chemical constitution of the rafifinal scandium alloy of producing with method of the present invention is: scandium Sc2.0%, all the other are aluminium Al and unavoidable impurities, iron Fe<0.01% wherein, silicon Si<0.01%, other impurity summation<0.02%.
Embodiment 2
Controlling electrolytical proportioning is: aluminum fluoride AlF
322%, Sodium Fluoride NaF 15%, bariumchloride BaCl
255%, sodium chloride nacl 8%, the Scium trichloride ScCl of adding 1% in ionogen
3Its operation controlled variable is: electrolysis temperature: 700 ℃, and electric tank working voltage: 5.0v, electrolyte thickness: 6.0cm.The chemical ingredients that adds the Scium trichloride in the ionogen in the electrolytic process requires: Scium trichloride ScCl
3:>98.5%, igloss<1%, oxide compound summation<0.2%, other impurity summation<0.3%.The weight percent chemical constitution of the rafifinal scandium alloy of producing with method of the present invention is: scandium Sc0.1%, all the other are aluminium Al and unavoidable impurities, iron Fe<0.01% wherein, silicon Si<0.01%, other impurity summation<0.02%.
Embodiment 3
Controlling electrolytical proportioning is: aluminum fluoride AlF
327%, Sodium Fluoride NaF 15%, bariumchloride BaCl
250%, sodium chloride nacl 8%, the Scium trichloride ScCl of adding 10% in ionogen
3Its operation controlled variable is: electrolysis temperature: 750 ℃, and electric tank working voltage: 6.0v, electrolyte thickness: 13cm.The chemical ingredients that adds the Scium trichloride in the ionogen in the electrolytic process requires: Scium trichloride ScCl
3:>98.5%, igloss<1%, oxide compound summation<0.2%, other impurity summation<0.3%.The weight percent chemical constitution of the rafifinal scandium alloy of producing with method of the present invention is: scandium Scl.0%, all the other are aluminium Al and unavoidable impurities, iron Fe<0.01% wherein, silicon Si<0.01%, other impurity summation<0.02%.
Embodiment 4
Controlling electrolytical proportioning is: aluminum fluoride AlF
327%, Sodium Fluoride NaF 15%, bariumchloride BaCl
252%, sodium chloride nacl 6%, the Scium trichloride ScCl of adding 5% in ionogen
3Its operation controlled variable is: electrolysis temperature: 800 ℃, and electric tank working voltage: 6.0v, electrolyte thickness: 13cm.The chemical ingredients that adds the Scium trichloride in the ionogen in the electrolytic process requires: Scium trichloride ScCl
3:>98.5%, igloss<1%, oxide compound summation<0.2%, other impurity summation<0.3%.The weight percent chemical constitution of the rafifinal scandium alloy of producing with method of the present invention is: scandium Sc0.5%, all the other are aluminium Al and unavoidable impurities, iron Fe<0.01% wherein, silicon Si<0.01%, other impurity summation<0.02%.
Embodiment 5
Controlling electrolytical proportioning is: aluminum fluoride AlF
340%, Sodium Fluoride NaF 25%, Calcium Fluoride (Fluorspan) CaF
216%, barium fluoride BaF
219%, the Scium trichloride ScF of adding 18% in ionogen
3Its operation controlled variable is: electrolysis temperature: 820 ℃, and electric tank working voltage: 6.0v, electrolyte thickness: 13cm.The chemical ingredients that adds the scandium fluoride in the ionogen in the electrolytic process requires: scandium fluoride ScF
3:>98.5%, igloss<1%, oxide compound summation<0.2%, other impurity summation<0.3%.The weight percent chemical constitution of the rafifinal scandium alloy of producing with method of the present invention is: scandium Sc1.5%, all the other are aluminium Al and unavoidable impurities, iron Fe<0.01% wherein, silicon Si<0.01%, other impurity summation<0.02%.
Embodiment 6
Controlling electrolytical proportioning is: aluminum fluoride AlF
345%, Sodium Fluoride NaF 23%, Calcium Fluoride (Fluorspan) CaF
216%, barium fluoride BaF
216%, the Scium trichloride ScF of adding 1% in ionogen
3Its operation controlled variable is: electrolysis temperature: 800 ℃, and electric tank working voltage: 5.0v, electrolyte thickness: 15cm.The chemical ingredients that adds the scandium fluoride in the ionogen in the electrolytic process requires: scandium fluoride ScF
3:>98.5%, igloss<1%, oxide compound summation<0.2%, other impurity summation<0.3%.The weight percent chemical constitution of the rafifinal scandium alloy of producing with method of the present invention is: scandium Sc0.2%, all the other are aluminium Al and unavoidable impurities, iron Fe<0.01% wherein, silicon Si<0.01%, other impurity summation<0.02%.
Embodiment 7
Controlling electrolytical proportioning is: aluminum fluoride AlF
335%, Sodium Fluoride NaF 26%, Calcium Fluoride (Fluorspan) CaF
215%, barium fluoride BaF
224%, the Scium trichloride ScF of adding 10% in ionogen
3Its operation controlled variable is: electrolysis temperature: 750 ℃, and electric tank working voltage: 6.5v, electrolyte thickness: 10cm.The chemical ingredients that adds the scandium fluoride in the ionogen in the electrolytic process requires: scandium fluoride ScF
3:>98.5%, igloss<1%, oxide compound summation<0.2%, other impurity summation<0.3%.The weight percent chemical constitution of the rafifinal scandium alloy of producing with method of the present invention is: scandium Sc1.0%, all the other are aluminium Al and unavoidable impurities, iron Fe<0.01% wherein, silicon Si<0.01%, other impurity summation<0.02%.
Embodiment 8
Controlling electrolytical proportioning is: aluminum fluoride AlF
335%, Sodium Fluoride NaF 20%, Calcium Fluoride (Fluorspan) CaF
217%, barium fluoride BaF
228%, the Scium trichloride ScF of adding 15% in ionogen
3Its operation controlled variable is: electrolysis temperature: 780 ℃, and electric tank working voltage: 6.5v, electrolyte thickness: 12cm.The chemical ingredients that adds the scandium fluoride in the ionogen in the electrolytic process requires: scandium fluoride ScF
3:>98.5%, igloss<1%, oxide compound summation<0.2%, other impurity summation<0.3%.The weight percent chemical constitution of the rafifinal scandium alloy of producing with method of the present invention is: scandium Sc1.5%, all the other are aluminium Al and unavoidable impurities, iron Fe<0.01% wherein, silicon Si<0.01%, other impurity summation<0.02%.
Claims (2)
1. the method for an electrolysis production rafifinal scandium alloy is characterized in that Scium trichloride or scandium fluoride are added direct electrolysis production rafifinal scandium alloy in three layers of electrolytic ionogen of liquid, and ionogen adopts fluorochloride or pure fluorochemical, controls electrolytical proportioning and is:
(1) adopt the electrolytical weight percent of fluorochloride to consist of: aluminum fluoride AlF
320%~30%, Sodium Fluoride NaF10%~15%, bariumchloride BaCl
250%~60%, sodium chloride nacl 5%~10% adds the Scium trichloride ScCl that accounts for ionogen gross weight 1%~20% in ionogen
3Carry out electrolysis;
(2) adopt the weight percent of pure electrolysis of fluorides matter to consist of: aluminum fluoride AlF
330%~50%, Sodium Fluoride NaF15%~30%, Calcium Fluoride (Fluorspan) CaF
215%~20%, barium fluoride BaF
215%~40%, in ionogen, add the scandium fluoride ScF that accounts for ionogen gross weight 1%~20%
3Carry out electrolysis;
Its operation controlled variable is: electrolysis temperature: 650 ℃~850 ℃, and electric tank working voltage: 4.0v~7.0v, electrolyte thickness: 4.0cm~15.0cm;
The weight percent that adds the Scium trichloride in the ionogen in the electrolytic process consists of: Scium trichloride ScCl
3:>98.5%, igloss<1%, oxide compound summation<0.2%, other impurity summation<0.3%;
The weight percent that adds the scandium fluoride in the ionogen in the electrolytic process consists of: scandium fluoride ScF
3:>98.5%, igloss<1%, oxide compound summation<0.2%, other impurity summation<0.3%.
2. the method for a kind of electrolysis production rafifinal scandium alloy according to claim 1, it is characterized in that the aluminum scandium alloy weight percent of producing consists of: scandium Sc0.1%~2.0%, all the other are aluminium Al and unavoidable impurities, iron Fe<0.01% wherein, silicon Si<0.01%, other impurity summation<0.02%.
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Cited By (1)
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US9567381B2 (en) | 2012-03-09 | 2017-02-14 | Vestaron Corporation | Toxic peptide production, peptide expression in plants and combinations of cysteine rich peptides |
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CN104694975A (en) * | 2015-03-26 | 2015-06-10 | 中南大学 | Electrolyte for preparing aluminum-scandium intermediate alloy |
CN104746106B (en) * | 2015-04-21 | 2017-02-22 | 中南大学 | Molten salt electrolysis method for preparing aluminum-scandium intermediate alloy |
US11186897B2 (en) * | 2015-04-22 | 2021-11-30 | United Company RUSAL Engineering and Technology Centre LLC | Method for producing aluminum-scandium alloy and reactor for implementing the method |
EP3612654B1 (en) * | 2017-03-20 | 2021-09-08 | Minertek Mineral Teknolojileri Madencilik Sanayi Ve Ticaret Anonim Sirketi | Production method for scandium metal and al-sc alloys via electrolysis of fluorinated scandium salts obtained by the calcination of scandium compound in the form of (nh4)2nascf6 |
CN107130264B (en) * | 2017-05-19 | 2018-12-18 | 东北大学 | A kind of method of nearly room temperature electrolytic preparation aluminium-based rare-earth alloy |
CN107630234B (en) * | 2017-09-18 | 2019-09-17 | 江西理工大学 | A method of scandium bearing master alloy is prepared using villaumite oxide system molten-salt electrolysis |
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US9567381B2 (en) | 2012-03-09 | 2017-02-14 | Vestaron Corporation | Toxic peptide production, peptide expression in plants and combinations of cysteine rich peptides |
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