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Method for preparing strong alkali anion exchange resin with long spacer arm

An exchange resin, spacer arm technology, applied in anion exchange, ion exchange, chemical instruments and methods, etc., can solve the problems of cumbersome process, difficult to control, difficult operation, etc., and achieve broad application prospects, cost saving, and simple process. Effect

Active Publication Date: 2010-12-08
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process is cumbersome, the operation is difficult, it is not easy to control, the manufacturing cost is also high, and it is difficult to realize industrialization

Method used

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  • Method for preparing strong alkali anion exchange resin with long spacer arm
  • Method for preparing strong alkali anion exchange resin with long spacer arm
  • Method for preparing strong alkali anion exchange resin with long spacer arm

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] In a 250mL four-neck flask equipped with a stirrer, condenser and thermometer, add 15.9g (0.119mol) of triethylamine hydrochloride and 31.8g (0.238mol) of aluminum trichloride under nitrogen protection, and stir at 80°C for 2h , add 3g macroporous white spherical beads and 20ml nitrobenzene that have been swelled in nitrobenzene for 6h, then gradually add 12g (0.119mol) of 1,3-oxazin 2-ketone (a kind of cyclic carbamate), After reacting at 95°C for 24 hours, the aminopropylated white spherical beads were separated and extracted with ethanol for 2 hours to obtain aminopropylated copolymerized beads with a weak base exchange capacity of 2.21meq / g dry resin.

[0018] Weigh 3 g of the above-mentioned amine-propylated copolymerized beads, 10 mL of formaldehyde, and 15 mL of formic acid, react at 50° C. for 5 h, filter, extract, wash, and dry to obtain 3.6 g of tertiary-aminated copolymerized beads.

[0019] Add the copolymerized beads after tertiary amination and 10ml bromoe...

Embodiment 2

[0022] In a 250mL four-neck flask equipped with a stirrer, a condenser and a thermometer, add 100mL of nitrobenzene and 15.8g (0.119mol) of aluminum trichloride under nitrogen protection, start stirring, and after the aluminum trichloride is dissolved, add Swell 3g of gel beads in nitrobenzene for 6h, then gradually add 12g (0.119mol) of 1,3-oxazin-2-one, react at 80°C for 36h, and separate the aminopropylated white balls The beads were extracted with ethanol for 2 hours to obtain aminopropylated copolymerized beads with a weak base exchange capacity of 1.86meq / g dry resin.

[0023] The tertiary amination and quaternization of Example 1 were used to obtain bromide quaternary ammonium anion exchange resins with an exchange capacity of 1.55meq / g. The structure is as follows:

[0024]

Embodiment 3

[0026] In a 250mL four-neck flask equipped with a stirrer, condenser and thermometer, add 31.3g (0.228mol) of triethylamine hydrochloride and 60.7g (0.455mol) of aluminum trichloride under nitrogen protection, and stir at 80°C for 2h , add 3g of macroporous white spherical beads swelled in fluorobenzene for 6h and 20ml of fluorobenzene, then gradually add 8g (0.091mol) of 2-oxazolidinone (a cyclic carbamate) and react at 120°C After 24 hours, the amine-ethylated white spherical beads were separated and extracted with ethanol for 2 hours to obtain amine-ethylated copolymerized beads, with a weak base exchange capacity of 1.96meq / g dry resin.

[0027] Tertiary amination and quaternization with Example 1 to obtain quaternary ammonium bromide strong base anion exchange resin with an exchange capacity of 1.75meq / g. The structure is as follows:

[0028]

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PUM

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Abstract

The invention relates to a method for preparing a strong anion exchange resin with long spacer arms, belonging to the field of the synthesis of ion exchange resins. The method enables macropore or hydrogel polystyrene resin swollen by inert solvent such as nitrobenzene to have amine-alkylation reaction by taking cyclic carbamate as alkylation reagent and Lewis acid or ionic liquid as catalyzer, thus producing polystyrene resin with long spacer arms primary amines; the polystyrene resin with long spacer-arm primary amines reacts with formic acid and formaldehyde to get tert-aminated polystyrene resin which then reacts with ethyl bromide to get strong anion exchange resin with long spacer arms. Directly introducing primary amine groups into white beads through amine-alkylation, the method disclosed by the invention simplifies process, saves cost and is simple in process; therefore, the method is of wide application prospect.

Description

technical field [0001] The invention relates to a preparation method of a strong base anion exchange resin with long spacer arms, and belongs to the field of synthesis of ion exchange resins. Background technique [0002] Ion exchange resins are used in many industrial production and scientific and technological fields. High temperature resistant strong base anion exchange resins have high chemical stability at high temperatures, which improves the durability of the resins at high temperatures, thus enabling The resin can be used in high temperature processes where previously ion exchange resins could not. [0003] Commercially available strong base anion exchange resins are poorly thermally stable because their benzylic carbon atoms are directly attached to the nitrogen atoms resulting in increased activity of the carbon atoms (reduced thermal stability). JP10045830, JP10137752, JP11012206, JP10053550, EP0776911, US5814672 once reported to improve the thermostability of re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F8/00C08F8/44C08F12/08B01J41/14
Inventor 陈群何明阳刘迎春高山
Owner CHANGZHOU UNIV
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