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Method for recycling Al resources in Friedel-Crafts reaction

A Friedel-Crafts reaction and resource technology, which is applied in chemical instruments and methods, preparation of organic compounds, compounds of group 5/15 elements of the periodic table, etc., can solve the problems of cumbersome post-processing and inconvenient recycling of aluminum-containing resources, etc. Achieve the effect of simple post-treatment, reduce the generation of acid gas, and avoid secondary pollution

Active Publication Date: 2015-07-29
HONGHU YITAI TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This treatment method will produce a large amount of acid wastewater and acid gas, resulting in rather cumbersome post-treatment, and the aluminum-containing resources are not easy to recycle.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] This example involves the recovery and utilization of aluminum trichloride in the system after the preparation of the pharmaceutical intermediate p-acetamidobutyrophenone by Friedel-Crafts reaction. P-acetamidobutyrophenone is obtained by the Friedel-Crafts reaction of acetanilide and n-butyryl chloride. The Friedel-Crafts reaction uses aluminum trichloride as a catalyst and carbon disulfide as a solvent. After the reaction is completed, it is processed to realize the extraction of the product and the recovery of aluminum at the same time. The processing method is as follows.

[0027] (1), through in-situ distillation, the system after the reaction is concentrated, reclaims carbon disulfide, and in the later stage of distillation (volume is concentrated to about 30% of the original volume), add the mixture of ethyl acetate and chlorobenzene in the reaction kettle, continue Distill until carbon disulfide is completely removed, and the feeding amount of the mixture of et...

Embodiment 2

[0030] This example involves the recovery and utilization of aluminum in the residue (containing aluminum chloride, sodium chloride, and a small amount of phosphine) after dissociation in the production process of the pharmaceutical intermediate phenyl dichlorophosphine. details as follows:

[0031] The residue after the dissociation is stirred and dispersed with chlorobenzene (the amount of chlorobenzene is 5 times of the volume of the residue), filtered to obtain the filtrate, and the filtrate is recovered by distillation to obtain part of the phosphine product; after the obtained filter cake is dried, the It is dispersed in an ethanol-water mixed solution (the volume ratio of ethanol to water is 7:1), and the mixture is filtered to obtain a filter cake and a filtrate, wherein the filter cake is sodium chloride, and the filtrate is ethanol containing aluminum trichloride hexahydrate. Aqueous solution, the filtrate is concentrated, crystallized and filtered to obtain aluminum...

Embodiment 3

[0033] This example involves the recycling of aluminum in the Friedel-Crafts reaction system for the production of 1,3,5-triethylbenzene, wherein the Friedel-Crafts reaction uses aluminum trichloride as a catalyst and ethyl bromide as a solvent. The recycling method is as follows:

[0034] (1), through in-situ distillation, the system after the reaction is concentrated, reclaims ethyl bromide, adds chlorobenzene in the reaction kettle in the late stage of distillation (volume is concentrated to about 20% of original volume), continues distillation, until removing Complete bromoethane, the feeding capacity of chlorobenzene is 3 times of concentrate volume.

[0035] (2) Cool down the system after step (1) to 20°C, add water with a molar mass 6 times the molar mass of aluminum trichloride, stir well, make the system evenly mixed, filter to obtain a filter cake, and dry to obtain Aluminum trichloride hexahydrate, the filtrate is concentrated to obtain the product 1,3,5-triethylbe...

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Abstract

The invention relates to a method for recycling Al resources in a Friedel-Crafts reaction. The method comprises steps performed after the Friedel-Crafts reaction as follows: (1), a reaction system is concentrated, a reaction solvent is recovered, a replacement solvent is added to disperse concentrated residues when the size of the reaction system is concentrated to 20%-50% of the original size, and concentration is continued until the reaction solvent is completely eliminated; (2), the temperature of the system obtained after the step (1) is controlled to range from subzero 20 DEG C to 100 DEG C, water is added to the system, the mixture is sufficiently mixed and filtered, the replacement solvent is recovered after filtrate is concentrated, meanwhile, a product of the Friedel-Crafts reaction is obtained, aluminum(III) chloride hexahydrate is obtained after a filter cake is dried, and the mole ratio of the added water to aluminum (III) chloride is (1-10):1. According to the method, no wastewater or acid gas is produced, the operation is simple, and environmental protection is facilitated.

Description

technical field [0001] The invention relates to a method for recovering Al resources from a Friedel-Crafts reaction system. Background technique [0002] Friedel-Crafts reaction (Friedel-Crafts reaction), referred to as Friedel-Crafts reaction, is an important class of organic reactions that can be used for dyes (such as triphenylmethane and xanthene, etc.), pesticide intermediates (alkylbenzene Synthesis of fine chemicals such as pharmaceutical intermediates (aryl ketones, phenylphosphine chloride, etc.) and other natural products. The most commonly used catalysts in the Friedel-Crafts reaction are aluminum-containing catalysts, among which anhydrous aluminum trichloride and sodium tetrachloroaluminate are used more. In the large-scale production process of these fine chemicals, the demand and dosage of anhydrous aluminum trichloride are also increasing, especially in the Friedel-Crafts acylation reaction. The post-treatment method of the Friedel-Crafts reaction is usuall...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/33C07C231/12C07F9/52C01F7/56
Inventor 郑智慧吴芳敏吕从高颜新天赵根根蔡华胜孙素丽成贞辉
Owner HONGHU YITAI TECH CO LTD
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