CN1514042A - Production method of high purity aluminium scandium alloy - Google Patents

Production method of high purity aluminium scandium alloy Download PDF

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CN1514042A
CN1514042A CNA031537855A CN03153785A CN1514042A CN 1514042 A CN1514042 A CN 1514042A CN A031537855 A CNA031537855 A CN A031537855A CN 03153785 A CN03153785 A CN 03153785A CN 1514042 A CN1514042 A CN 1514042A
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fluoride
scandium
ionogen
electrolysis
weight percent
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CN1260397C (en
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N 杨
杨昇
顾松青
刘凤琴
李强
罗丽芬
赵淋
徐建华
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Aluminum Corp of China Ltd
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Aluminum Corp of China Ltd
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Abstract

A technology for preparing high-purity Al-Sc alloy by use of three-layer molten aluminium refining electrolyzer features that the scandium chloride (or fluoride) is added to electrolyte (fluorochloride or fluoride), and then directly electrolyzed at 650-850 deg.C and under 4-7 V of working voltage. Its advantages are high quality and low cost.

Description

A kind of production method of rafifinal scandium alloy
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 NaF15%～30%, Calcium Fluoride (Fluorspan) CaF 215%～20%, barium fluoride BaF 215%～40%, in ionogen, go into to account for the scandium fluoride ScF of 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 NaF10%～15%, bariumchloride (BaCl 250%～60%, sodium chloride nacl 5%～10% adds 1%～20% scandium fluoride (ScCl in ionogen 3) carry out electrolysis.
(2) adopt pure electrolysis of fluorides matter: aluminum fluoride AlF 330%～50%, Sodium Fluoride NaF15%～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 NaF13%, 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 NaF15%, 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 NaF15%, 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 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 4
Controlling electrolytical proportioning is: aluminum fluoride AlF 327%, Sodium Fluoride NaF15%, 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 NaF25%, 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 NaF23%, 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 NaF26%, 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 NaF20%, 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. 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 NaF15%～30%, Calcium Fluoride (Fluorspan) CaF 215%～20%, barium fluoride BaF 215%～40%, in ionogen, go into to account for the scandium fluoride ScF of 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. 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%.
CN 03153785 2003-08-21 2003-08-21 Production method of high purity aluminium scandium alloy Expired - Lifetime CN1260397C (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104694975A (en) * 2015-03-26 2015-06-10 中南大学 Electrolyte for preparing aluminum-scandium intermediate alloy
CN104746106A (en) * 2015-04-21 2015-07-01 中南大学 Molten salt electrolysis method for preparing aluminum-scandium intermediate alloy
CN107130264A (en) * 2017-05-19 2017-09-05 东北大学 A kind of method of nearly room temperature electrolytic preparation aluminium-based rare-earth alloy
CN107532317A (en) * 2015-04-22 2018-01-02 俄铝工程技术中心有限责任公司 Produce the method for aluminium-scandium alloy and implement the reactor of this method
CN107630234A (en) * 2017-09-18 2018-01-26 江西理工大学 A kind of method for preparing scandium bearing master alloy using villaumite oxide system molten-salt electrolysis
WO2019040016A3 (en) * 2017-03-20 2019-04-25 Mi̇nertek Mi̇neral Teknoloji̇leri̇ Madenci̇li̇k Sanayi̇ Ve Ti̇caret Anoni̇m Şi̇rketi̇ 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 (nh 4)2nascf6

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WO2013134734A2 (en) 2012-03-09 2013-09-12 Vestaron Corporation Toxic peptide production, peptide expression in plants and combinations of cysteine rich peptides

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104694975A (en) * 2015-03-26 2015-06-10 中南大学 Electrolyte for preparing aluminum-scandium intermediate alloy
CN104746106A (en) * 2015-04-21 2015-07-01 中南大学 Molten salt electrolysis method 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
CN107532317A (en) * 2015-04-22 2018-01-02 俄铝工程技术中心有限责任公司 Produce the method for aluminium-scandium alloy and implement the reactor of this method
WO2019040016A3 (en) * 2017-03-20 2019-04-25 Mi̇nertek Mi̇neral Teknoloji̇leri̇ Madenci̇li̇k Sanayi̇ Ve Ti̇caret Anoni̇m Şi̇rketi̇ 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 (nh 4)2nascf6
CN107130264A (en) * 2017-05-19 2017-09-05 东北大学 A kind of method of nearly room temperature electrolytic preparation aluminium-based rare-earth alloy
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
CN107630234A (en) * 2017-09-18 2018-01-26 江西理工大学 A kind of method for preparing scandium bearing master alloy using villaumite oxide system molten-salt electrolysis
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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