Benzocrown ether graft polymer with lithium isotopic separation effect and preparation method thereof

A technology of graft polymer and separation effect, which is applied in the separation of different isotopic elements, separation methods, and separation of dispersed particles, etc., can solve the problems of low isotope adsorption and desorption efficiency, weak lithium isotope separation ability, etc., and meet the operating conditions Mild, high immobilization capacity, efficient separation effect

Active Publication Date: 2012-11-21
TIANJIN POLYTECHNIC UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Chinese patent CN1186506A discloses a preparation method of a water-soluble polymer, which involves a water-soluble polymer grafted with 15-crown-5 ether on polyvinyl alcohol, but the material is not oriented to lithium isotope separation, and the side The hanging 15-crown 5 structure does not contain a benzene ring as a power supply group, and its lithium isotope separation ability is relatively weak
However, because the resin particle size is too small (50-100μm), the isotope adsorption and desorption efficiency is low

Method used

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  • Benzocrown ether graft polymer with lithium isotopic separation effect and preparation method thereof
  • Benzocrown ether graft polymer with lithium isotopic separation effect and preparation method thereof
  • Benzocrown ether graft polymer with lithium isotopic separation effect and preparation method thereof

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Embodiment 1

[0029] The method of grafting polyvinyl alcohol with 4-formylbenzo13crown4 is as follows: take 150mL of 6.7g / L polyvinyl alcohol aqueous solution, add 10g of 4-formyl Benzo-13-crown 4(5), add 1g of catalyst concentrated sulfuric acid according to the mass ratio of polymer to catalyst 1:1 and mix evenly, control the temperature at 70±5°C and react for 15h, then pour the reaction system into ethanol to precipitate, and obtain by suction filtration Precipitate. After being washed several times with ethanol and then dried, a 4-formylbenzo13crown4-grafted polyvinyl alcohol polymer was obtained, with a pendant group content of 3.0 mmol / g. Putting the polymer into lithium chloride aqueous solution and obtaining the single-stage separation factor of the polymer was 1.043 by means of solid-liquid extraction. Obtain polymer structure by embodiment 1 as follows:

[0030]

Embodiment 2

[0032] The method for grafting polyvinyl alcohol with 4-formylbenzo15crown5 is as follows: take 60mL of 85g / L polyvinyl alcohol aqueous solution, and drop 1g of 4-formylbenzene according to the mass ratio of polymer to benzocrown ether at 5:1 And 15 crown 5 (2), according to the mass ratio of polymer to catalyst 0.5:1, put 10g of catalyst concentrated hydrochloric acid and mix evenly, control the temperature at 80±5°C and react for 1h, then pour the reaction system into ethanol to precipitate. The precipitate was obtained by suction filtration. After being washed several times with ethanol and then dried, a crown ether grafted polymer material was obtained, with a pendant group content of 1.1 mmol / g. The polymer material was put into lithium chloride aqueous solution to obtain a single-stage separation factor of 1.033 for the polymer material by means of solid-liquid extraction.

Embodiment 3

[0034] The method for grafting polyvinyl alcohol with 4-formyl benzo 12 crown 4 is as follows: take 160 mL of 31.3 g / L polyvinyl alcohol aqueous solution, and add 1 g of 4-formyl For benzo12crown 4(1), 0.1 g of concentrated sulfuric acid was added and mixed uniformly according to the mass ratio of polymer to catalyst of 50:1, and the temperature was controlled at 80±5°C for 24 hours, and the reaction system was poured into n-butanol to precipitate. The precipitate was obtained by suction filtration, washed several times with acetone and then dried to obtain a crown ether graft polymer with a pendant group content of 0.7 mmol / g. Putting the crown ether graft polymer into the lithium chloride aqueous solution and obtaining the single-stage separation factor of the crown ether graft polymer by solid-liquid extraction was 1.043.

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Abstract

The invention provides a benzocrown ether graft polymer with a lithium isotopic separation effect and a preparation method thereof. As for the polymer, hydroxyl-contained polyvinyl alcohol or polyethylene-vinyl alcohol is adopted to serve as a main chain; benzocrown ether is adopted to serve as a side hung group; and the main chain and the side hung group are connected together through chemical bonds so as to form the benzocrown ether graft polymer. The preparation method comprises the following steps: dissolving the active hydroxyl-contained polyvinyl alcohol or the polyethylene-vinyl alcohol and the benzocrown ether with an active carboxyl functional group or an aldehyde group in a solvent; performing esterification or aldolization under the action of a catalyst at a certain temperature; completing the chemical grafting of the benzocrown ether with the polyvinyl alcohol or the polyethylene-vinyl alcohol; and finally adding a precipitating agent so as to obtain the graft polymer through precipitation. The graft polymer provided by the invention, which contains the benzocrown ether group, has a good lithium isotopic separation effect. Moreover, through adjusting the size of the crown ether ring, the graft polymer can be used for recognition and separation of heavy metal ions, and has an extensive application prospect.

Description

technical field [0001] The invention belongs to the field of lithium isotope separation, in particular to a graft polymer with lithium isotope separation effect and a preparation method thereof, specifically a benzocrown ether grafted polyvinyl alcohol or crown ether graft with lithium isotope separation effect Polyethylene-vinyl alcohol graft polymer and its preparation method. Background technique [0002] Natural Lithium consists of 6 Li and 7 Li two isotopic compositions, their abundances are 7.52% and 92.48%, respectively. isotope 6 Li has a strong ability to capture low-speed neutrons, and the neutron bombardment is caused by isotopes 6 When lithium deuteride, a compound synthesized by Li and deuterium, produces a strong thermonuclear reaction, accompanied by a large amount of energy. isotope 7 Due to its extremely small thermal neutron absorption cross section (0.037b), Li can be used as a core coolant and a heat transfer agent for nuclear fusion reactors. Thus...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F116/06C08F216/06C08F210/02C08F8/08B01J20/26B01D59/26
Inventor 李建新严峰何本桥袁威津崔振宇
Owner TIANJIN POLYTECHNIC UNIV
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