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Macroporous chelate resin catalyst as well as preparation method and applications thereof

The technology of a chelating resin and a macroporous resin is applied in the field of macroporous chelating resin catalyst and its preparation, which can solve the problems such as difficulty in obtaining pure p-chlorotoluene, high meso-content in chlorinated liquid, short catalyst life, etc. The method is simple, the dosage is low, and the effect of reducing the relative content

Active Publication Date: 2014-06-11
江苏超跃化学有限公司
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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

[0031] In a four-neck flask, add 150ml of 10% ferric chloride aqueous solution, start stirring, raise the temperature to 60°C, and adjust the pH to 3 with hydrochloric acid; then add 75ml with a particle size of 0.5-1.5 mm and a pore size of 0.6-1 nm D418 styrene cation exchange resin, heated to 60 ° C for 2 hours; then filtered, the solid was rinsed twice with water and dried, and the mother liquor could be used mechanically. The dried solid is packed into a four-necked flask with a water separator, 150ml of toluene is added, heated and dehydrated, and the toluene is filtered to obtain a macroporous chelating resin catalyst.

Embodiment 2

[0033] In a four-neck flask, add 150ml of 5% copper sulfate aqueous solution, start stirring, raise the temperature to 80°C, adjust the pH to 4 with sulfuric acid; then add 75ml of D418 styrene with a diameter of 0.5-1.5mm and a pore size of 0.6-1nm For the cation exchange resin, heat it to 80°C and keep it warm for 3 hours; then filter it, rinse the solid with clean water twice and dry it, the mother liquor can be applied mechanically. The dried solid is packed into a four-necked flask with a water separator, 150ml of toluene is added, heated and dehydrated, and the toluene is filtered to obtain a macroporous chelating resin catalyst.

Embodiment 3

[0035] In a four-neck flask, add 150ml of 15% antimony nitrate aqueous solution, start stirring, raise the temperature to 50°C, adjust the pH to 3 with nitric acid; then add 50ml of D418 styrene with a diameter of 0.5-1.5mm and a pore size of 0.6-1nm For cation exchange resin, heat it to 50°C and keep it warm for 2 hours; then filter it, rinse the solid with clean water twice and dry it, and the mother liquor can be applied mechanically. The dried solid is packed into a four-necked flask with a water separator, 150ml of toluene is added, heated and dehydrated, and the toluene is filtered to obtain a macroporous chelating resin catalyst.

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Abstract

The invention relates to a catalyst for polycyclic aromatic hydrocarbon chlorination reaction, and in particular relates to a macroporous chelate resin catalyst as well as a preparation method and applications thereof. The catalyst is formed by chelating a specific proportion of metal saline solution and D418 styrene cation exchange resin with specific aperture at the constant temperature of 60-80 DEG C. Metal ions are positioned in a macroporous resin pore duct; when the catalyst serves as a catalyst of the polycyclic aromatic hydrocarbon chlorination reaction, electrophilic reaction is performed mainly in a resin pore duct; and the dimension of parachlorotoluene molecules is smaller than that of orthochlorotoluene molecules, the dispersion speed in the pore duct of certain dimension is faster than that of the orthochlorotoluene, and therefore more para-position products can be obtained in the electrophilic reaction, thereby improving the relative content of para-orientation products, and reducing the relative content of ortho-orientation products.

Description

technical field [0001] The invention relates to a catalyst for ring chlorination of aromatic hydrocarbons, in particular to a macroporous chelating resin catalyst and a preparation method and application thereof. Background technique [0002] Aromatic hydrocarbons such as toluene react with chlorine gas in the liquid phase under the action of Lewis acid catalysts such as iron trichloride, antimony trichloride, and aluminum trichloride, and the mono-substituted products of aromatic hydrocarbon rings produced are o-chlorotoluene and p-chlorotoluene. mixture of toluene. If ferric chloride is used as catalyst, the ratio of p-chlorotoluene to o-chlorotoluene in the monochlorotoluene mixture is about 0.5-0.55:1. [0003] Among the cyclic chlorination products of aromatic hydrocarbons, the para-substituted products are widely used. For example, in the cyclic chlorination products of toluene, p-chlorotoluene is an important intermediate in the production of fine chemical products s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/08C07C17/12C07C25/02
Inventor 殷云武任坚跃薛保安
Owner 江苏超跃化学有限公司
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