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Synthesis method of quaternary phosphonium type anion-exchange resin for catalyzing epoxyethane hydration

A technology of ethylene oxide hydration and ion exchange resin, which is applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc., can solve the problem of large skeleton damage and difficult preparation High-capacity quaternary phosphonium-type anion-exchange resins, difficult access to ω-halogenated olefins, etc.

Inactive Publication Date: 2003-12-10
JIANGSU POLYTECHNIC UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has a two-step heterogeneous reaction, and it is not easy to prepare a high-capacity quaternary phosphonium-type anion-exchange resin, and the distribution of functional groups is not uniform; the post-haloalkylation has great damage to the skeleton and is prone to internal stress; in addition, ω - Halogenated olefins are also not readily available

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] In the 500 milliliters of four-neck flasks that agitator, condenser and thermometer are equipped with, add dispersion agent 6 grams of gelatin, 300 milliliters of water, treat to add 72 grams of 4-bromobutyl styrene, 3.12 grams of divinylbenzene ( Content 50%) and initiator 0.4 grams of azobisisobutyronitrile mixed solution, stir, adjust the dispersed droplets to a suitable size, heat to 70 ° C for 40 minutes, heat up to 90 ° C for 18 hours, after the polymerization reaction is completed , washed with water, washed with ethanol, and dried to obtain 66.8 grams of light yellow transparent copolymerized beads.

[0018] In a 250 ml three-neck flask equipped with a stirrer, condenser, thermometer and nitrogen protection device, add 25 grams of the above-mentioned copolymerized beads, 80 ml of ethanol, add 10.4 grams of trimethylphosphine under nitrogen protection, and heat up to 40 ° C for reaction After 24 hours, the resin was filtered out and washed with ethanol to obtain ...

Embodiment 2

[0021] The steps are the same as in Example 1, except that the amount of divinylbenzene is changed to 7.8 grams, and the obtained quaternary phosphonium bromide anion exchange resin has an exchange capacity of 2.46 mmol / g dry resin. Replace the 5% sodium bicarbonate solution in Example 1 with 5% sodium formate solution to obtain a quaternary phosphonium-type anion exchange resin whose anion is formate, as a catalyst for hydration of ethylene oxide.

Embodiment 3

[0023] Add 6 grams of polyvinyl alcohol and 300 milliliters of deionized water into a 500 milliliter four-necked flask equipped with a stirrer, a condenser and a thermometer. After the polyvinyl alcohol is dissolved, add 54.3 grams of 4-chloropropyl styrene and 3.12 grams of di Vinylbenzene (content 50%), the mixed solution of porogen liquid paraffin 35 grams and 0.4 gram benzoyl peroxide, stir, adjust the dispersed liquid droplet to suitable size, be heated to 70 ℃ of reaction 1 hour, be warming up to 90 ℃ After reaction at ℃ for 18 hours, after the completion of the polymerization reaction, wash with water and ethanol, dry, extract with petroleum ether, and dry to obtain 49.2 g of copolymerized beads.

[0024] In a 250 ml three-necked flask equipped with a stirrer, condenser, thermometer and nitrogen protection device, add 19.2 grams of the above-mentioned copolymerized beads, 80 milliliters of n-butyl ether, add 30.3 grams of tributylphosphine under nitrogen protection, and ...

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Abstract

The synthesis method of quaternary phosphonium type ion exchange resin capable of being used as catalyst for catalyzing epoxyethare hydration reaction includes the following steps: using holoalkyl substituted styrene (halogen is chlorine and bromine) and divnylbenzene to make them implement suspension polymerization according to the conventional method to obtain the gel or macroporous structure copolymer bead body; making the obtained copolymer bead body and trialkylphosphine implement reaction with quaternary phosphonium in organic solvent to obtain the quaternary phosphonium type anion-exchange resin, then using bicarbonate radical, formic acid radical, bioxalate radical and citrate dihydroradical, etc. to exchange the halogen ion in the above-mentioned resin so as to obtain the invented product with high catalytic activity.

Description

Technical field [0001] The invention relates to a compound synthesis method, in particular to a synthesis method of a quaternary phosphonium ion exchange resin used for catalyzing the hydration of ethylene oxide. Its synthetic quaternary phosphonium type anion exchange resin has the following structural formula: [0002] Wherein n=3-4, R can independently be methyl, ethyl, propyl and butyl, X can independently be chlorine, bromine. [0003] The anion of the resin can be used to catalyze the hydration reaction of ethylene oxide after being exchanged by hydroxyl group, bicarbonate group, formate group, hydrogen oxalate group and dihydrogen citrate group. Background technique [0004] U.S. Patent No. 6,124,508 reports that the resin with the above structure is used to catalyze the hydrolysis reaction of ethylene oxide, and has the characteristics of high catalytic activity, good selectivity, and good heat resistance stability, but does not disclose its preparation method. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/08C07C29/10
Inventor 陈群何明阳王璠张卫红
Owner JIANGSU POLYTECHNIC UNIVERSITY
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