Monoazabenzo crown ether graft polymer material with lithium isotope separation effect and preparation method thereof

A graft polymer, separation effect technology, applied in the separation of different isotopic elements, separation methods, dispersed particle separation and other directions, can solve the problems of difficult lithium isotope, low single-stage separation factor of lithium isotope, etc. Mild operating conditions and high solid loading effect

Inactive Publication Date: 2018-11-02
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, using column chromatography to separate lithium isotopes, the lithium isotopes adsorbed in the resin are difficult to elute. In addition, crown ether and cryptate resins with lithium isotope separation capabilities are filled in the separation tower. Due to the gaps between the resin particles, lithium isotopes low single-stage separation factor

Method used

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  • Monoazabenzo crown ether graft polymer material with lithium isotope separation effect and preparation method thereof
  • Monoazabenzo crown ether graft polymer material with lithium isotope separation effect and preparation method thereof
  • Monoazabenzo crown ether graft polymer material with lithium isotope separation effect and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022]The preparation method of benzomonaazepine-15-crown-5 grafted polysulfone polymer material is as follows: Weigh dry 18g polysulfone and place it in a three-necked flask, add chloroform to dissolve it completely, cool to 10 Below ℃, then add 63ml of trimethylchlorosilane, 15g of paraformaldehyde and 0.6ml of tin tetrachloride, stabilize for 15 minutes and react at 50℃ for 11 hours, then precipitate it in methanol, Dry in a vacuum drying oven to obtain chloromethylated polysulfone with a substitution degree of about 0.4. Weigh 1.5 g of chloromethylated polysulfone and dissolve it in 12 mL of DMF, add 0.86 g of benzodiazepine-15-crown-5, control the temperature at 60±5°C for 6 hours, pour the reaction system into ethanol for precipitation, pump The precipitate was obtained by filtration, washed several times with ethanol and then dried to obtain a crown ether grafted polysulfone polymer material with a crown ether immobilization capacity of 0.58 mmol / g. The single-stage se...

Embodiment 2

[0025] The preparation method of 4-hydroxybenzo15crown5-grafted polysulfone polymer is as follows: use the same method as above to prepare chloromethylated polysulfone with a degree of substitution of about 1.5, and then weigh 1g of chloromethylated polysulfone Dissolve the polysulfone in 10mL DMF, add 1g of 4-hydroxybenzo15crown 5 and 0.488g of anhydrous potassium carbonate and mix evenly, control the temperature at 80±5°C for 24h, pour the reaction system into methanol to precipitate, and filter with suction to obtain The precipitate was washed several times with methanol and then dried to obtain a grafted polymer material with a crown ether immobilization capacity of 2.0 mmol / g. The single-stage separation factor of the grafted polymer material for lithium isotopes obtained by liquid-solid extraction was 1.068.

Embodiment 3

[0027] The method for grafting polysulfone polymer materials with 4-aminobenzo12crown4 is as follows: the same method is used to prepare chloromethylated polysulfone with a degree of substitution of about 1.0, and accurately weigh 1g of chloromethylated polysulfone Dissolve sulfone in 20mL of DMAA, add 0.4g of 4-aminobenzo12crown 4 and 0.30g of triethylamine and mix evenly, control the temperature at 60±5°C for 12h, pour the reaction system into ethanol to precipitate, and filter to obtain the precipitate. After being washed several times with ethanol and then dried, a benzocrown ether grafted polysulfone polymer material with a crown ether immobilization amount of 1.0 mmol / g was obtained. The single-stage separation factor of polymer material to lithium isotope was 1.043 by liquid-solid extraction.

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Abstract

The invention discloses a monoazabenzo crown ether graft polymer material with a lithium isotope separation effect and a preparation method thereof. According to the polymer, polysulfone, polyether sulfone or polyether ether ketone containing chloromethyl groups are utilized as matrix, monoazabenzo crown ether is utilized as a side hanging group, and the monoazabenzo crown ether graft polymer is prepared by chemical bone connection. A preparation process comprises the steps: polysulfone, polyether sulfone or polyether ether ketone and a chloromethylation reagent can generate electrophilic substitution reaction under the catalytic action of the lewis acid, polymer with an active functional group of a chloromethyl group is prepared, the polymer containing the active chloromethyl group and the monoazabenzo crown ether containing an active functional group of hydroxyl or amino are dissolved in a certain solvent to generate unimolecular nucleophilic substitution reaction to finish chemicalgrafting, and finally, a precipitator is added to obtain polymer through precipitation. The monoazabenzo crown ether graft polymer disclosed by the invention contains a crown ether group, so that themonoazabenzo crown ether graft polymer has a good lithium isotope separation characteristic.

Description

technical field [0001] The invention belongs to the field of lithium isotope separation, and relates to a graft polymer with lithium isotope separation effect and a preparation method thereof, specifically a benzomonazacrown ether grafted polysulfone and benzene with lithium isotope separation effect. Monoaza crown ether grafted polyether sulfone or benzo monoaza crown ether grafted polyether ether ketone graft polymer material and its preparation method. Background technique [0002] Lithium (Li) is the lightest metal, and there are abundant lithium resources in the world, among which my country is the third largest producer of lithium resources, and the stable isotope of lithium is derived from 6 Li and 7 Li is composed of two kinds, and its abundance is about 7.5% and 92.5%, respectively. 6 Li and 7 Li differs in nuclear properties, 6 After Li is bombarded by neutrons, tritium and helium are generated, so that tritium in the fusion reactor can continue to proliferate,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/20C08G75/23C08G8/02B01D59/26
CPCC08G75/20B01D59/26C08G8/02C08G75/23
Inventor 杨博然严峰裴洪昌
Owner TIANJIN POLYTECHNIC UNIV
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