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A kind of method for preparing o-benzoylbenzoic acid by acylation reaction of benzene and phthalic anhydride

A technology of benzoylbenzoic acid and phthalic anhydride, which is applied in the field of preparation of o-benzoylbenzoic acid by the acylation reaction of benzene and phthalic anhydride catalyzed by chloroaluminate ionic liquid, which can solve the problem of corrosion of equipment, pollution of the environment, failure of catalyst to be recycled, etc. problems, to achieve the effect of low vapor pressure, high catalytic activity, and good industrial application prospects

Inactive Publication Date: 2015-08-05
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide recyclable chlorine for the problems that existing catalysts in the process of preparing o-benzoylbenzoic acid through the acylation reaction of benzene and phthalic anhydride catalyzed by aluminum trichloride cannot be recycled, corroded equipment, and polluted the environment. Preparation of o-benzoylbenzoic acid by the acylation reaction of benzene and phthalic anhydride catalyzed by aluminate ionic liquid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Under the protection of nitrogen, the reaction of benzene and phthalic anhydride to synthesize o-benzoylbenzoic acid: add 0.20mol benzene, 0.02mol phthalic anhydride, 0.04mol[Pmim]Br-2AlCl to a 100ml three-necked flask 3 The ionic liquid was reacted at 40°C for 5h under stirring and reflux conditions. After the reaction, the reaction solution was left to stand, and the remaining benzene in the upper layer was removed, and then used in the reaction process of synthesizing o-benzoylbenzoic acid; According to the volume ratio of 1:1, the extractant obtained by mixing it is extracted and separated, and each time 45ml of extractant is used for two-stage extraction operation. liquid phase, the upper layer is the upper extractant phase), and the product is extracted into the extractant phase. The extracted ionic liquid phase is vacuum-dried to remove residual extractant to obtain recovered ionic liquid. Extractant phase is that temperature is 50 ℃, and vacuum is 0.09MPa cond...

Embodiment 2

[0030] Under the protection of nitrogen, the reaction of benzene and phthalic anhydride to synthesize o-benzoylbenzoic acid: add 0.06mol benzene, 0.02mol phthalic anhydride, 0.06mol [Emim]Cl-2.5AlCl into a 100ml three-necked flask 3The ionic liquid was reacted at 50° C. for 4 hours under the conditions of stirring and reflux, and the reaction was completed. After the reaction solution was allowed to stand, the remaining benzene was removed, and then the ionic liquid phase containing the product was transferred into a separatory funnel, and extracted and separated using an extractant obtained by mixing n-heptane and ethyl acetate at a volume ratio of 2:1. Use 10ml of extractant each time to carry out a three-stage extraction operation, and extract the product into the extractant phase. The extracted ionic liquid phase is vacuum-dried to remove residual extractant to obtain recovered ionic liquid. The extractant phase was distilled under reduced pressure at a temperature of 60°...

Embodiment 3

[0032] Under the protection of nitrogen, the reaction of benzene and phthalic anhydride to synthesize o-benzoylbenzoic acid: add 0.40mol benzene, 0.02mol phthalic anhydride, 0.02mol[Bmim]Br-3AlCl to a 100ml three-necked flask 3 The ionic liquid was reacted at 30° C. for 9 hours under stirring and reflux conditions, and the reaction was completed. After the reaction solution was allowed to stand, the remaining benzene was removed, and then the ionic liquid phase containing the product was transferred into a separatory funnel, and extracted and separated using an extractant obtained by mixing n-octane and ethyl acetate at a volume ratio of 3:1. Use 40ml of extractant each time to carry out two-stage extraction operation, and extract the product into the extractant phase. The extracted ionic liquid phase is vacuum-dried to remove residual extractant to obtain recovered ionic liquid. Extractant phase is that temperature is 70 ℃, and vacuum is 0.07MPa condition under reduced press...

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Abstract

The invention discloses a technological method of preparing o-benzoylbenzoic acid by acylation reaction of benzene and phthalic anhydride. The method comprises the following steps: catalyzing acylation reaction of benzene and phthalic anhydride by adopting a chloroaluminate ionic liquid with high activity; and extracting a product from the ionic liquid catalyst by an extracting agent to separate the product from the catalyst. The ionic liquid catalyst used in the method disclosed by the invention can be efficiently and repeatedly used to avoid pressure of a conventional catalyst aluminum chloride anhydrous on three waste treatment, so that the requirements on green environmental protection is satisfied. The ionic liquid catalyst is adjustable in acidity, good in dissolving property, low in steam pressure and high in thermal stability and chemical stability, and can be repeatedly used. The method not only can overcome the defects that the post-treatment is tedious and the three waste treatment cost is high and the like after the conventional catalyst aluminum chloride anhydrous reacts, but also can overcome the defect that the catalyst aluminum chloride anhydrous cannot be repeatedly used.

Description

technical field [0001] The invention belongs to the technical field of green chemical industry, and specifically relates to a process method for preparing o-benzoylbenzoic acid through the acylation reaction of benzene and phthalic anhydride catalyzed by a recyclable chloroaluminate ionic liquid. Background technique [0002] Phthaloylbenzoic acid (BBA) is an important dye and pharmaceutical intermediate, especially it is an intermediate in the synthesis of anthraquinone by phthalic anhydride. The process of synthesizing anthraquinone from benzene and phthalic anhydride is divided into two steps. First, the Friedel-Crafts acylation reaction of benzene and phthalic anhydride produces BBA, and then BBA is decomposed to obtain anthraquinone. At present, the industrial acylation reaction of benzene and phthalic anhydride uses anhydrous aluminum trichloride as a catalyst. This process needs to consume a large amount of aluminum trichloride, and the aluminum trichloride cannot be ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/083C07C51/48C07C65/34
CPCC07C51/083C07C65/34
Inventor 王桂荣李济深赵新强王延吉
Owner HEBEI UNIV OF TECH
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