Application of a sulfur-containing polyimide resin as an adsorbent for rare earth elements

A technology of sulfur-containing polyimide resin and sulfur-containing polyimide resin, which is applied in the field of sulfur-containing polyimide resin, can solve problems such as resistance to organic solvents, difficult rare earth mining, time-consuming and energy-consuming problems, and achieve Strong hydrophilic performance, good adsorption and long service life

Active Publication Date: 2021-12-07
INSPECTION & QUARANTINE TECH CENT OF NINGBO ENTRY EXIT INSPECTION & QUARANTINE BUREAU +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Conventional rare earth extraction generally uses steps such as acid dissolution and solvent extraction, using a large amount of reagents, and the steps are complicated
For the concentration of rare earth elements in the solution, the method of solvent volatilization is generally used, which is time-consuming and energy-consuming.
There are few polymer adsorbents for the adsorption of rare earth elements, and broad-spectrum adsorption materials are often used for adsorption, which is poorly targeted and easily interfered by other elements
At the same time, ordinary organic adsorbents often have the disadvantages of being intolerant to organic solvents, strong acids, and high temperatures, and are difficult to be used in the mining of rare earth ores.

Method used

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  • Application of a sulfur-containing polyimide resin as an adsorbent for rare earth elements
  • Application of a sulfur-containing polyimide resin as an adsorbent for rare earth elements
  • Application of a sulfur-containing polyimide resin as an adsorbent for rare earth elements

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] The sulfur-containing diamine monomer 2,2'-bis(sulfonic acid)-4,4'-diaminodiphenyl ether (ODADS) and the sulfur-free diamine monomer 4,4'-diaminodiphenyl ether The molar ratio of (ODA) was set to 6:4 for the feeding reaction, and the reaction was carried out according to the preparation method of random sulfur-containing polyimide to obtain random sulfur-containing polyimide resin particles.

[0050] Add 2,2'-bis(sulfonic acid)-4,4'-diaminodiphenyl ether ODADS (0.6524g, 1.81mmol), triethylamine (0.5390g, 5.33mmol) and 8mL m-cresol, stirred to dissolve ODADS completely, then added 4,4'-diaminodiphenyl ether ODA (0.2417g, 1.21mmol), thioether naphthalene dianhydride SBNTA (1.2866g, 3.02mmol) and Benzoic acid (0.5522g, 4.53mmol). The mixture was stirred at room temperature for 30 minutes, then warmed to 80°C for 4h and 180°C for 18h. When the mixture was cooled to 80°C, it was poured into 500 mL of acetone to obtain a fibrous polymer. After washing once with acetone, ex...

Embodiment 2

[0059] Embodiment 2 Potassium, calcium, sodium, magnesium, aluminum, zinc, iron, tin, lead interference experiment

[0060] The molar ratio of the sulfur-containing diamine monomer and the sulfur-free diamine monomer is set to 6:4 for the feeding reaction, and the reaction is carried out according to the preparation method of the random sulfur-containing polyimide of Example 1 to obtain Random sulfur-containing polyimide resin particles.

[0061] Add potassium ions, calcium ions, sodium ions, magnesium ions, aluminum ions, zinc ions, iron ions, tin ions and lead at a concentration of 0.5 mg / L to the mixed solution with the contents of 16 rare earth elements at 0.2 mg / L. Ions, prepared as a multi-element interference mixed solution.

[0062] Take 1.0 g of the above-mentioned random sulfur-containing polyimide resin particles, add it to 50 mL of the above-mentioned multi-element interference mixed solution, put it in a shaker and shake it for 30 minutes, centrifuge to take the ...

Embodiment 3

[0066] The molar ratio of sulfur-containing diamine monomer and sulfur-free diamine monomer is set to 6:4 for feeding reaction, and the reaction is carried out according to the preparation method of block type sulfur-containing polyimide resin to obtain block type Sulfur-containing polyimide resin particles.

[0067] Add sulfonated diamine ODADS (0.6618g, 1.84mmol), triethylamine (0.4467g, 4.41mmol) and 8mL m-cresol into a No. Ether naphthalene dianhydride SBNTA (0.7640 g, 1.79 mmol) and benzoic acid (0.3274 g, 2.68 mmol). The mixture was stirred at room temperature for 30 minutes, then heated to 80° C. for 4 hours, and 180° C. for 18 hours to obtain an amine-terminated polyimide oligomer. Add the remaining naphthalene dianhydride SBNTA (0.5420g, 1.27mmol) and 8mL m-cresol into another No. 2 oblique three-neck flask protected by nitrogen, stir and dissolve, then add unsulfonated diamine ODA (0.2454g, 1.23mmol ), benzoic acid (0.2324g, 1.91mmol), reacted at 180°C for 18h. Wh...

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Abstract

The invention discloses the application of a sulfur-containing polyimide resin as an adsorbent for rare earth elements. The sulfur-containing polyimide resin is a random type sulfur-containing polyimide resin or a block type sulfur-containing polyimide resin. Amine resin, the structural formula of the random sulfur-containing polyimide resin is shown in formula I, and the structural formula of the block sulfur-containing polyimide resin is shown in formula II. The adsorbent provided by the invention has adsorption effect on 16 kinds of rare earth elements such as scandium, yttrium, lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and other 16 kinds of rare earth elements. Not interfered by potassium, calcium, sodium, magnesium, aluminum, zinc, iron, tin, lead and other elements. The adsorption process is simple and easy to operate. The adsorbent provided by the invention can be normally used in strong acid, high temperature and high pressure environments, and can regenerate resin materials through a simple desorption process, which is economical and environmentally friendly.

Description

technical field [0001] The invention relates to the application of a sulfur-containing polyimide resin as an adsorbent for 16 kinds of rare earth elements. Background technique [0002] Rare earth is composed of 14 natural elements and several synthetic elements. It is an important national strategic resource, and countries all over the world attach great importance to the reserve of rare earth. Although my country is one of the countries rich in rare earth resources in the world, it uses a large amount. With the increasing influence of rare earths on the national economy and people's livelihood, the country pays more and more attention to rare earth resources. As a non-renewable resource, the recycling, purification and concentration of rare earths have been extensively studied and concerned. [0003] In addition, with the increasing application of rare earths in military, metallurgy, petrochemical, glass ceramics, and agricultural fields, the pollution problems of rare ea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/10B01J20/26B01J20/30B01J20/34
CPCB01J20/262B01J20/3425B01J20/3475C08G73/1007C08G73/1042C08G73/105C08G73/1064C08G73/1071
Inventor 钟莺莺陈国飞蒋立佟岩王如坤顾佳丽曹丹
Owner INSPECTION & QUARANTINE TECH CENT OF NINGBO ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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