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Cationic type macroporous chelate resin catalyst and preparation method thereof

A chelating resin and cationic technology, which is applied in the field of cationic macroporous chelating resin catalysts and their preparation, can solve the problems of difficulty in obtaining pure p-chlorotoluene, high content of intermediate sites in chlorinated liquids, and short catalyst life. The preparation method is simple, the dosage is low, and the effect of reducing the relative content

Inactive Publication Date: 2015-04-15
韩红淑
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the molecular sieve lattice is easily broken by the acid produced by the reaction, the catalyst life is short, and the proportion of p-chlorotoluene in the chlorination product is significantly reduced when it is reused after regeneration. Toluene

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In a four-neck flask, add 150ml of a saturated aqueous solution of nickel chloride, start stirring, raise the temperature to 60°C, and adjust the pH to 3 with hydrochloric acid; Acidic styrene-based cation-exchange resin, heated to 60°C for 2 hours; then filtered, rinsed twice with water and dried, the mother liquor can be applied mechanically. The dried solid is packed into a four-neck flask with a water separator, 150ml of toluene is added, heated and dehydrated, and the toluene is filtered off to obtain a cationic macroporous chelating resin catalyst.

Embodiment 2

[0027] In a four-neck flask, add 225ml of saturated nickel chloride aqueous solution, start stirring, raise the temperature to 50°C, adjust the pH to 2 with hydrochloric acid; then add 75ml of 0017 strong acidic styrene with a diameter of 0.5-1.5mm and a pore size of 0.6-1nm It is a cation exchange resin, heated to 50°C and kept for 3 hours; then filtered, the solid was rinsed twice with water and then dried, and the mother liquor can be applied mechanically. The dried solid is packed into a four-neck flask with a water separator, 150ml of toluene is added, heated and dehydrated, and the toluene is filtered off to obtain a cationic macroporous chelating resin catalyst.

Embodiment 3

[0029] In a four-necked flask, add 50ml of saturated nickel chloride aqueous solution, start stirring, raise the temperature to 50°C, adjust the pH to 3 with hydrochloric acid; then add 50ml of 0017 strong acid styrene with a diameter of 0.5-1.5mm and a pore size of 0.6-1nm It is a cation exchange resin, heated to 60°C and kept for 2 hours; then filtered, the solid was rinsed twice with water and dried, and the mother liquor can be used mechanically. The dried solid is packed into a four-neck flask with a water separator, 150ml of toluene is added, heated and dehydrated, and the toluene is filtered off to obtain a cationic macroporous chelating resin catalyst.

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Abstract

The invention relates to a catalyst of aromatic hydrocarbon cyclochlorination reaction, and especially relates to a cationic type macroporous chelate resin catalyst and a preparation method thereof. The cationic type macroporous chelate resin catalyst is formed by chelation of macroporous resin and a metal ion; according to the metal-ion resin chelate, macroporous resin is taken as a carrier, and the metal ion is in the channel of the macroporous resin; as the catalyst of aromatic hydrocarbon cyclochlorination reaction, an electrophilic reaction is mainly performed in the channel of resin; and because p-chloroaromatic hydrocarbons have the molecule dimension smaller than that of o-chloroaromatic hydrocarbons, the dispersing speed of p-chloroaromatic hydrocarbons in a channel with a certain dimension is larger than that of o-chloroaromatic hydrocarbons, thus more para-position products can be obtained in the electrophilic reaction, and therefore, the relative content of p-position substituted products is improved and the relative content of ortho-position substituted products is reduced.

Description

technical field [0001] The invention relates to a catalyst for ring chlorination of aromatic hydrocarbons, in particular to a cationic macroporous chelating resin catalyst and a preparation method thereof. Background technique [0002] For a long time, people have been trying to find a way to increase the ratio of para-products during the cyclic chlorination of aromatic hydrocarbons. The US patent (US4031144) reported that nickel chloride and sulfur dichloride were used as catalysts, and toluene and chlorine were cyclically chlorinated in the liquid phase. Chemical reaction, p-chlorotoluene:o-chlorotoluene=0.9~0.97:1 in the product. Toluene ring chlorination uses a Lewis acid catalyst, and simultaneously uses thianthrene or a derivative of thianthrene as a cocatalyst (US4069263, US4250122). In the monochlorination product, p-chlorotoluene: o-chlorotoluene=1.4:1, although this method obtains relatively High contrast ratio, but the reaction needs to be carried out at about 0°...

Claims

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Application Information

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IPC IPC(8): B01J31/30C07C17/12C07C25/02
Inventor 韩红淑
Owner 韩红淑
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