Resin, preparation method thereof, and process for preparing ultra-high purity rare earth oxide by using resin

A technology of rare earth oxides and resins, which is applied in the field of preparation of ultra-high-purity rare earth oxides, can solve the problems of low separation coefficient and crossover of impurity removal rates, and achieve the effect of solving separation difficulties

Active Publication Date: 2019-12-17
TIANJIN BAOGANG RES INST OF RARE EARTHS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, the ultra-high purification of most ultra-high-purity rare earth compounds still has key links that are difficult to break through in technology. The resins used for ion exchange, such as the traditional P507 extraction resin, have low separation coefficients and poor impurity removal rates. Make ultra-high purity rare earth compounds in short supply in the market

Method used

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  • Resin, preparation method thereof, and process for preparing ultra-high purity rare earth oxide by using resin
  • Resin, preparation method thereof, and process for preparing ultra-high purity rare earth oxide by using resin
  • Resin, preparation method thereof, and process for preparing ultra-high purity rare earth oxide by using resin

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Effect test

preparation example Construction

[0051] The preparation method of above-mentioned resin is:

[0052] Take a certain amount of XAD-4 macroporous adsorption resin in a beaker, add enough absolute ethanol to completely submerge XAD-4 macroporous adsorption resin, soak for 12 hours, wait for the resin to fully swell, take out the resin with ultra-pure Rinse with water several times until the eluent is clear and free of floating impurities. Then soak in 4%-5% HCl aqueous solution for 4 hours, then wash with ultra-pure water until neutral, then soak with 4%-5% NaOH solution for 4 hours, wash with ultra-pure water until neutral, and remove the water on the surface of the resin as much as possible Then put it into a freeze-drying box to dry for later use. Take a certain amount of D2EHDGAA and dissolve it in 0.45-0.55mol / L kerosene, and then add a certain amount of pretreated XAD-4 resin into it. The volume ratio of resin to kerosene liquid is 1:1.7-1:2.0. Shake in a constant temperature shaker for 24 hours, and the...

Embodiment 1

[0060] A kind of resin, comprises each component of following weight part: extraction agent D 2 EHDGAA 50 parts, load resin XAD-4 100 parts.

[0061] The preparation method of above-mentioned resin is:

[0062] Take 1L XAD-4 macroporous adsorption resin in a beaker, add enough absolute ethanol to completely immerse XAD-4 macroporous adsorption resin, soak for 12 hours, wait for the resin to fully swell, take out the resin and rinse it with ultrapure water Several times until the eluent is clear and free of floating impurities. Then soak with 5wt% HCl aqueous solution for 4 hours, then wash with ultrapure water until neutral, then soak with 5wt% NaOH solution for 4 hours, then wash with ultrapure water until neutral, remove the water on the surface of the resin as much as possible and put it into a freeze-drying box Dry inside and set aside. Take 334g D2EHDGAA and dissolve it in 1.8L kerosene, then add 1LXAD-4 resin which has been pretreated in advance, shake it in a constan...

Embodiment 2

[0065] Preparation of ultra-high-purity ytterbium oxide: add ytterbium oxide with a relative purity of 99.9% and dilute hydrochloric acid to dissolve, and make 50g / L (REO) YbCl 3 Solution, adjust the pH to 2-3, add it to the material tank of the feeding area, adjust the flow rate to 75mL / h, add ultrapure water to the material tank in the washing area, adjust the flow rate to 300mL / h, add 1.5mol / h to the material tank of the pickling area 1 L of HCl solution, adjust the flow rate to 95mL / h, add 2.0mol / L HCl solution to the pickling zone 2 material tank, adjust the flow rate to 80mL / h, add 2.6mol / L HCl solution to the pickling zone 3 material tank, adjust The flow rate is 45mL / h, pure water is added to the material tank in the regeneration zone, and the flow rate is adjusted to 0.5L / h. The liquid in the high-purity product tank was collected, and the rare earth content was detected by titration method to be 31.2g / L, and the yield was 62.4%. The liquid is precipitated with oxali...

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Abstract

The invention provides resin, a preparation method thereof and a process for preparing an ultra-pure rare earth oxide by using the resin. The resin is prepared from the following components in parts by weight: 80-120 parts of loaded resin XAD-4 and 40-60 parts of an extracting agent D2EHDGAA. The resin disclosed by the invention is relatively high in separation coefficient of rare earth oxide andrelatively good in impurity removal rate.

Description

technical field [0001] The invention belongs to the technical field of preparation of ultra-high-purity rare earth oxides, and in particular relates to a resin and a preparation method thereof, and a process for preparing ultra-high-purity rare earth oxides using a continuous moving bed using the resin. Background technique [0002] Ultra-high-purity rare earth products have become an indispensable new material component for many high-end high-tech and devices today, and can be widely used in cast iron, alloy steel, non-ferrous metallurgy, petroleum catalytic cracking, thermal insulation materials, glass decolorization and coloring and radiation protection, Polishing powder, permanent magnet, fluorescent powder, magneto-optical material, laser material, magnetostrictive material, optical fiber, photoelectric material, piezoelectric material, hydrogen storage material, superconductor, atomic reactor control material and composite material, etc., so high-purity The added value...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/24B01J20/30B01D15/18C01F17/00
CPCB01J20/24B01D15/1871C01P2006/80
Inventor 张呈祥赵长玉温永清杨帆赵志钢郝先库张瑞祥张志宏王安丽马士精荣文娜
Owner TIANJIN BAOGANG RES INST OF RARE EARTHS
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