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Method for extracting and separating high-purity dysprosium oxide and terbium oxide from terbium-dysprosium rare earth enrichment matters

A rare earth enrichment and terbium oxide technology, which is applied in the field of rare earth separation, can solve the problems of high commissioning cost, high acid-base consumption, and large amount of terbium element pressing, so as to reduce commissioning costs, save one-time investment, and reduce investment costs. Effect

Active Publication Date: 2014-10-08
GANZHOU ZHANHAI IND & TRADING +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current extraction and separation of high-purity terbium and dysprosium production lines mostly use multiple two-exit extraction processes to sequentially separate ~GdTbDy / / HoY~, ~GdTb / / Dy, ​​and ~Gd / / Tb for separation, because the produced terbium and dysprosium are both High-purity products have high acid-base consumption and large tanks; some use pre-grouping (fuzzy extraction) technology, but they are all finely divided into two on the element terbium (~GdTb / TbDyHoY~), and then enter the series (~ Gd / / Tb / / DyHoY~) separation process, separated into ~Gd, DyHoY~ two intermediate products and high-purity Tb products, and then connected to two outlets (Dy / / HoY~) process, separated into high-purity Dy and ( HoY~) Two products of holmium and yttrium heavy rare earth enrichment, this process can reduce the acid and alkali consumption by about 20% compared with the previous pure two-exit process, but the high price and small amount of terbium element has a large amount of groove, and it is one-time The investment is 1.5~2.0 times that of the two export processes. This is because terbium with high price and low quantity must form terbium-enriched full peak and pure terbium full peak in the pre-grouping and series separation processes respectively; and high-purity terbium and terbium The quality of dysprosium products is generally >99.95%, and it is difficult to improve to >99.99% of terbium and dysprosium products. This is because the small amount of terbium is divided into two, and it is difficult to control in time when the process or raw materials fluctuate. The quality of dysprosium is difficult to stabilize; at the same time, there is a long time for debugging and balancing, and the cost of debugging is high; moreover, when producing fluorescent grade terbium oxide, the pre-grouping and series separation processes must use high-grade pure hydrochloric acid to increase the cost of acid consumption, otherwise it will be very expensive. Rare earth impurities are difficult to pass and other shortcomings

Method used

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  • Method for extracting and separating high-purity dysprosium oxide and terbium oxide from terbium-dysprosium rare earth enrichment matters
  • Method for extracting and separating high-purity dysprosium oxide and terbium oxide from terbium-dysprosium rare earth enrichment matters
  • Method for extracting and separating high-purity dysprosium oxide and terbium oxide from terbium-dysprosium rare earth enrichment matters

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Implementation example 1: with raw materials Ⅰ As the feed solution of terbium-dysprosium enrichment, ① firstly pre-group in molar fraction of 0.55:0.45, extract part of the aqueous phase La~GdTbDy material to make rare earth soap, and then separate into two intermediate feed liquids, La~GdTbDy and DyHoY~; ② Middle The feed liquid directly enters the series separation process linkage, and after drawing out part of the aqueous phase La~GdTb material to make rare earth soap, it is then separated into: La~GdTb, HoY~ two pure enrichments and high-purity Dy products; ③ The separated intermediate products La~GdTb feed liquid, and then enter the La~Gd / / Tb two-outlet separation process to separate into La~Gd pure enrichment and high-purity Tb products. If the process uses high-grade pure hydrochloric acid as wash-back acid, the precipitant is purified Oxalic acid can produce fluorescent grade high-purity terbium oxide products (see the process flow figure 1 , figure 2 ).

...

Embodiment 2

[0028] Example 2: Using raw material II as the feed liquid of the terbium-dysprosium enrichment, 1. firstly pre-group by molar fraction of 0.6:0.4, draw out part of the aqueous phase ~SmEuGdDy material to make rare earth soap, and then separate it into ~SmEuGdTbDy and DyHo~LuY two The intermediate feed liquid; ②The intermediate feed liquid directly enters the series separation process linkage, and part of the water phase ~SmEuGdTb material is extracted to make rare earth soap, and then separated into: ~SmEuGdTb, HoY~ two pure enrichments and high-purity Dy products; ③Separation The intermediate product ~SmEuGdTb feed liquid, and then enter the ~SmEuGd / / Tb two-outlet separation process to separate into ~SmEuGd pure enrichment and high-purity Tb products. Refined oxalic acid can produce fluorescent-grade high-purity terbium oxide products (see the process flow figure 1 , figure 2 ).

[0029] The organic phase consists of extractant: bis(2-ethylhexyl)2-ethylhexylphosphoric aci...

Embodiment 3

[0035] Example 3: Using the raw material III as the feed liquid of the terbium-dysprosium enrichment, ① firstly pre-group by molar fraction of 0.5:0.5, and extract part of the aqueous phase La~GdDy materials to prepare rare earth soap, and then separate into La ~GdTbDy and DyHo~LuY two intermediate feed liquids; ②The intermediate feed liquid directly enters the series separation process, and part of the aqueous phase La~GdTb material is extracted to make rare earth soap, and then separated into: La~GdTb, Ho~LuY two pure rich Aggregates and high-purity Dy products; ③ separated intermediate products La ~GdTb feed liquid, and then enter the La~Gd / / Tb two-outlet separation process to separate into La~Gd pure concentrates and high-purity Tb products. If the process uses high-grade pure hydrochloric acid as the washing and reverse acid, the precipitating agent uses refined oxalic acid It can produce fluorescent grade high-purity terbium oxide products (see the process flow figure...

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Abstract

The invention relates to a rare earth separation method, and in particular relates to a method for extracting and separating high-purity dysprosium oxide and terbium oxide from various terbium-dysprosium rare earth enrichment materials. The invention aims to provide the method for extracting and separating high-purity dysprosium oxide and terbium oxide from various terbium-dysprosium rare earth enrichment matters which are easily-balanced in system, low in debugging cost, small in acid and alkali consumption, low in production cost as well as low in quantity of high-price terbium element pressing grooves, and saves one-time investment. The method for extracting and separating high-purity dysprosium oxide and terbium oxide from the terbium-dysprosium rare earth enrichment matters comprises the following steps: (1) a continuous saponification and continuous rare earth soap manufacturing process; (2) a pre-grouping process; (3) a tandem separation process; and (4) a two outlets-Gd / / Tb separation process. The method provided by the invention has the advantages that 1, the quality of high-price terbium element pressing grooves is less; 2, the method is easily-balanced in system, low in debugging cost, small in acid and alkali consumption and low in production cost, and saves the one-time investment.

Description

technical field [0001] The invention relates to a rare earth separation method, in particular to a method for extracting and separating high-purity dysprosium oxide and terbium oxide from various terbium-dysprosium rare-earth enrichment materials. Background technique [0002] Terbium-dysprosium rare earth enrichment materials are generally multi-element rare earth mixtures with terbium-dysprosium component as the main component. An intermediate rare earth product mainly composed of terbium and dysprosium, which is obtained from various rare earth raw materials after group separation, is used as a high-quality raw material for further separation of high-purity terbium and high-purity dysprosium. The current extraction and separation of high-purity terbium and dysprosium production lines mostly use multiple two-exit extraction processes to sequentially separate ~GdTbDy / / HoY~, ~GdTb / / Dy, ​​and ~Gd / / Tb for separation, because the produced terbium and dysprosium are both High-p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/26C22B59/00
CPCY02P10/20
Inventor 丁永权祝文才高亮任卫蔡伟
Owner GANZHOU ZHANHAI IND & TRADING
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