Rare earth fluoride molten salt electrolysis slag treatment method

A technology of molten salt electrolysis and rare earth fluorination, which is applied in the field of rare earth, iron recovery, and fluorine recycling in rare earth fluoride molten salt slag, to achieve the effects of recovery, easy operation, and simple process

Inactive Publication Date: 2019-03-19
JIANGXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide an environmentally friendly and economical method for treating fluoride rare earth molten salt electrolytic slag. Aiming at many problems faced by defluorination and extraction of rare earth from rare earth molten salt electrolytic slag, a magnetic separation-sulfuric acid aging-water immersion method is proposed. The method of ra

Method used

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  • Rare earth fluoride molten salt electrolysis slag treatment method
  • Rare earth fluoride molten salt electrolysis slag treatment method
  • Rare earth fluoride molten salt electrolysis slag treatment method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The mixed rare earth fluoride molten salt electrolytic slag is used as the raw material, and its composition is as follows.

[0034] element

Nd

Pr

Dy

F

Fe

Mn

Co

Ba

content

31.9

3.76

3.04

21.46

21.49

0.066

<0.010

<0.010

element

Li

Si

Ca

Na

Mg

S

Al

C

content

2.95

0.60

0.34

0.20

0.0077

0.10

<0.010

1.7

[0035] First, grind the electrolytic slag finely with a sample mill, then sieve the slag with a particle size of 58-75 μm through a vibrating screen, take 250 g and put it in water according to the liquid-solid ratio of 20:1 and stir it thoroughly, and then use the SLon-100 magnetic separator Carry out magnetic separation, set the magnetic separation conditions as current 400 A, voltage 5.8 V, power 2.3 Kw, field strength 0.668 T, the magnetic separation tailings obtained carry out suction filtration, drying; Magnetic separation tailin...

Embodiment 2

[0038] A single fluoride rare earth molten salt electrolytic slag is used as a raw material, and its composition is as follows.

[0039] element

Nd

F

Fe

C

Ca

Mn

Co

content

38.57

20.87

24.36

1.92

0.34

<0.010

<0.010

element

Li

Si

Mg

Na

S

Al

Ba

content

3.73

1.20

<0.010

0.14

0.05

<0.010

<0.010

[0040] Firstly, the electrolytic slag was ground with a sample mill, and then the slag with a particle size of 58-75 μm was sieved through a vibrating screen. 250 g of it was placed in water according to the liquid-solid ratio of 20:1 and fully stirred, and then the SLon-100 magnetic separator was used. Perform magnetic separation, set the magnetic separation conditions as current 400 A, voltage 5.8 V, power 2.3 Kw, and field strength 0.668 T, and the obtained magnetic separation tailings are subjected to suction filtration and drying; the magnetic separation tail...

Embodiment 3

[0043] Using the molten salt electrolytic slag after ball milling in Example 1 as the raw material, the slag with a particle size of 30-50 μm was sieved through a vibrating screen, and 250 g of slag was placed in water according to a liquid-solid ratio of 20:1 and fully stirred, and then SLon- 100 magnetic separator for magnetic separation, set the magnetic separation conditions as current 400 A, voltage 5.8 V, power 2.3 Kw, field strength 0.668 T, and the obtained magnetic separation tailings were subjected to suction filtration and drying; the magnetic separation tailings were mixed with 60 % concentrated sulfuric acid is placed in a polytetrafluoroethylene beaker at a liquid-solid ratio of 5:1, and then placed in a constant temperature water bath. 140 ℃, the aging reaction is 5 h, and the stirring speed is 300 r min -1 Under the same conditions, the removal rate of F reaches 94.11%, the transformation rate of Nd reaches 94.72%, the transformation rate of Pr reaches 95.02%, ...

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Abstract

The invention discloses a rare earth fluoride molten salt electrolysis slag treatment method. The rare earth fluoride molten salt electrolysis slag treatment method comprises the following steps thatball milling is carried out on rare earth molten salt electrolytic slag to a certain particle size; the electrolytic slag obtained after ball milling is subjected to magnetic separation, and magneticseparation tailings and magnetic separation concentrates are obtained; the magnetic separation tailings and concentrated sulfuric acid are mixed to make a heating reaction, and curing residues and HFgas (preparing an HF solution with water absorption) are obtained; the sulfuric acid curing residues are leached with water, and water leaching liquid is obtained; and the water leaching liquid obtained in the fourth step is subjected to fluoride precipitation with the HF solution obtained in the step three, and a rare earth fluoride product is obtained after liquid-solid separation is carried. The rare earth fluoride molten salt electrolysis slag treatment method is environment-friendly and economical, and solves the problem about separation of molten salt electrolysis slag rare earth and fluorine; meanwhile, the fluorine is finally recycled into a reaction system to react with rare earth to form precipitate, and green production and high-efficiency recovery of rare earth and iron from rare earth molten salt electrolysis slag are realized.

Description

technical field [0001] The invention relates to a comprehensive recovery and utilization treatment technology of rare earth waste residue in the rare earth smelting industry. More specifically, the present invention relates to the recycling of fluorine in rare earth fluoride molten salt slag and the recovery method of rare earth and iron. Background technique [0002] At present, the equipment for the production of rare earth metals or alloys in my country is a 3000 A electrolytic cell mainly operated by hand. Therefore, during the production operations of rare earth metals out of the furnace, replacement of anodes, regular furnace cleaning, and furnace dismantling, there are many non-rare earth impurities. Accumulated in the rare earth molten salt, the generation of waste rare earth molten salt is unavoidable. There are many types of these waste rare earth molten salts, and the degree of contamination by impurities is also quite different. During the molten salt electrolys...

Claims

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Application Information

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IPC IPC(8): C22B7/04C22B1/00C22B59/00C01B7/19
CPCC01B7/191C22B1/005C22B7/006C22B7/04C22B59/00Y02P10/20
Inventor 田磊徐志峰李玉虎严康陈丽杰
Owner JIANGXI UNIV OF SCI & TECH
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