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Method for preparing phthalide through catalytic liquid phase selective oxidation

A technology of phase selection and oxidation, which is applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of difficult control of phthalide selectivity, complicated post-treatment, high reaction temperature, etc. The effect of high conversion rate and product selectivity, recyclable catalyst and mild reaction conditions

Active Publication Date: 2021-05-11
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] This application aims at the high cost of raw materials for the production of phthalide from o-cyanobenzyl chloride in the prior art, serious equipment corrosion, a large amount of acidic waste water, and complicated post-treatment; the selectivity of phthalide produced by catalytic hydrogenation of phthalic anhydride is difficult to control, and the main It is produced by gas-phase oxidation of ortho-xylene. The reaction temperature is high, the safety is poor, it is prone to over-oxidation, the consumption of raw materials is large, and the product selectivity is low. A kind of catalytic liquid-phase selective oxidation of ortho-xylene to prepare phthalide is proposed. The method has the advantages of mild reaction conditions, high conversion rate of raw materials and high product selectivity, and recyclable catalyst.

Method used

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  • Method for preparing phthalide through catalytic liquid phase selective oxidation
  • Method for preparing phthalide through catalytic liquid phase selective oxidation
  • Method for preparing phthalide through catalytic liquid phase selective oxidation

Examples

Experimental program
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Embodiment 1

[0037] Dissolve 1g of cobalt acetate tetrahydrate and 1g of manganese chloride tetrahydrate in 150ml of methanol, and add to 150ml of methanol with 4g of benzotriazole dissolved in it under stirring, continue to stir for 2h, filter, and wash the obtained solid with methanol, dry it in the air, and blow it under nitrogen. After roasting at 700°C for 4h under protection, soak in 10wt% dilute hydrochloric acid for 8h, filter and wash to neutrality, and vacuum-dry the resulting solid at 80°C for 8h to obtain 2g of nitrogen-doped carbon-supported cobalt-manganese bimetallic catalyst (Co-Mn / N-C).

[0038] Take 0.5g of Co-Mn / N-C catalyst and put it into a high-pressure reactor equipped with 50g of o-xylene, stir, raise the temperature to 150°C, fill in oxygen to a pressure of 1.0MPa, and react for 2h. The qualitative and quantitative analysis of the product shows that the conversion rate of o-xylene is 41%, and the selectivity of phthalide is 95%.

Embodiment 2～6

[0040] Examples 2-6 studied the influence of metal components in nitrogen-doped carbon-supported catalysts on the reaction. The specific method is similar to that of Example 1, except that different metal salt compounds and different multi-dentate nitrogen-containing compounds are used to prepare Catalyst, other conditions are identical with embodiment 1, and result is as shown in table 1.

Embodiment 2

[0041] The catalyst preparation process of Example 2 is different from that of Example 1 in that: the metal salt is 3g of copper sulfate pentahydrate and 1g of manganese sulfate tetrahydrate; the multidentate nitrogen-containing compound is 12g of benzotriazole; roasting at 600°C for 5h; finally A nitrogen-doped carbon-supported ruthenium catalyst (Cu-Mn / N-C) was prepared.

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Abstract

The invention discloses a method for preparing phthalide through catalytic liquid phase selective oxidation. The method comprises the following steps of: contacting and reacting a raw material containing o-xylene with a catalyst in the presence of an oxygen source to obtain phthalide, wherein air or oxygen is used as the oxygen source, and nitrogen-doped carbon-loaded bimetal is used as the catalyst. The method has the advantages of mild reaction conditions, high raw material conversion rate, high product selectivity, recyclability of the catalyst and the like.

Description

technical field [0001] The application relates to a method for preparing phthalide by catalytic liquid-phase selective oxidation, which belongs to the technical field of organic chemical industry. Background technique [0002] Phthalide, also known as o-hydroxymethylbenzoic acid lactone, is an important fine chemical intermediate, mainly used in the production of dye intermediates 1,4-dichloroanthraquinone, 1-chloroanthraquinone, anticoagulant phenyl Indandione, fungicide tetrachlorophthalide, phenoxystrobin, anti-anxiety drug doxepin, dye vat brown BR and other chemicals. [0003] The traditional preparation method of phthalide has the following problems: (1) o-cyanobenzyl chloride can prepare phthalide under the action of sulfuric acid. This method has high cost of raw materials, serious corrosion of equipment, large amount of acid waste water, and complex post-treatment. (2) Phthalide can be obtained by reducing phthalic anhydride with zinc-hydrochloric acid. This meth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/88B01J27/24B01J37/08
CPCC07D307/88B01J27/24B01J37/086Y02P20/584
Inventor 黄义争高进徐杰孙颖苗虹车鹏华石松马继平
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI