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A kind of co-production methyl benzoic acid, methyl benzonitrile and phthalonitrile method

A technology of methyl benzoic acid and methyl benzonitrile, which is applied in chemical instruments and methods, purification/separation of carboxylic acid nitrile, preparation of carboxylate, etc., can solve the problems of large amount of solid waste, single product structure, and target product. Low efficiency and other problems, to achieve the effect of reducing the amount of three wastes, diversifying product structure and low price

Active Publication Date: 2021-05-11
JIANGXI KEYUAN BIOPHARM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0020] The purpose of the present invention is to solve the problems in the prior art such as low yield of target product, large amount of solid waste, single product structure, etc., and provide a co-production methyl alcohol with simple process, low equipment investment, environmental protection and good comprehensive benefits. Methods for Benzoic Acid, Toluonitrile and Phthalonitrile

Method used

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  • A kind of co-production methyl benzoic acid, methyl benzonitrile and phthalonitrile method
  • A kind of co-production methyl benzoic acid, methyl benzonitrile and phthalonitrile method
  • A kind of co-production methyl benzoic acid, methyl benzonitrile and phthalonitrile method

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Experimental program
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Effect test

Embodiment 1

[0101] The catalyst that dissolves in the fresh p-xylene that adds in the oxidation reactor is cobalt naphthenate, metal phthalocyanine (R with general formula (IV) structure 1 =CH 3 CH 2 , R 2 =H, M=Mn), the metalloporphyrin (R 1 =R 2 = H, R 3 =CH 3 , M=Cu) mixture, the total concentration is 75ppm, the reaction temperature is 180°C, the reaction pressure is 2MPa, the oxygen-containing gas is the oxygen-enriched air of 24% oxygen concentration, the residence time of the reactants in the oxidation reactor is adjusted to make the The conversion rate of xylene was 42%, and the oxidation reaction solution was obtained. At this time, the mass percentage of each component in the reaction solution obtained by HPLC analysis is listed in Table 1. In the initial distillation tower, the boiling point in the oxidation reaction liquid is lower than all components of p-methylbenzyl alcohol for rectification separation, and when the p-methylbenzyl alcohol content reaches 0.06wt% in th...

Embodiment 2

[0104] The catalyst dissolved in fresh p-xylene fed to the oxidation reactor was MnO 2 And cobalt acetylacetonate, total concentration is 350ppm, and reaction temperature is 150 ℃, and reaction pressure is 1MPa, oxygen-containing gas concentration 21%, operation process is identical with embodiment 1, and difference is that the conversion rate control of p-xylene is 50% , the mass percent content of p-methylbenzyl alcohol in the initial distillation tower still liquid is controlled to be 0.07%. The mass percent composition of each component that HPLC analysis obtains in the reaction solution is listed in Table 1, and the quality, composition and the content of methylbenzoic acid in the first distillation column tower bottom liquid that obtains are listed in the table 2.

[0105] Add the liquid from the above-mentioned initial distillation tower to the rectification tower for rectification, and obtain 889.4 g of p-toluic acid product with a purity of 99.0% at the top of the to...

Embodiment 3

[0107] Add the catalyst dissolved in the fresh p-xylene in the oxidation reactor to be N-hydroxyphthalimide, cobalt isooctanoate, metal phthalocyanine (R with general formula (IV) structure 1 =OH,R 2 =H, M=Ru) and metalloporphyrins (R 1 =R 3 = H, R 2 =OH,M 1 = M 2 =Mn) mixture, the total concentration is 10000ppm, the reaction temperature is 116 ° C, the reaction pressure is 0.2MPa, the oxygen-containing gas is pure oxygen, the operation process is the same as in Example 1, and the difference is that the conversion rate of p-xylene is controlled as 60%, and the mass percent content of p-methylbenzyl alcohol in the initial distillation tower bottom liquid is controlled to be 0.10%. The mass percent composition of each component that HPLC analysis obtains in the reaction solution is listed in Table 1, and the quality, composition and the content of methylbenzoic acid in the first distillation column tower bottom liquid that obtains are listed in the table 2.

[0108] Add ...

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Abstract

The invention discloses a method for co-producing methylbenzoic acid, methylbenzonitrile and phthalonitrile, comprising: (1) continuously feeding xylene, a catalyst and an oxygen-containing gas into an oxidation reactor for reaction, Obtain the oxidation reaction liquid; (2) enter the oxidation reaction liquid into the initial distillation tower and carry out rectification separation, stop the rectification when the methyl benzyl alcohol content reaches 0.01~0.15wt% in the initial distillation tower bottom liquid, obtain low boiling point component and (3) enter the rectification tower with the initial distillation tower still liquid; (3) stop rectification when toluic acid content reaches 30~90wt% in the rectifying tower tower still liquid, obtain formosan (4) mixing the rectifying tower and tower liquid with ammonia to obtain a nitrile-containing reaction liquid; (5) carrying out rectification and separation of a nitrile-containing reaction liquid to obtain methylbenzene respectively Carbonitrile and phthalonitrile products. The invention has the advantages of simple process, less equipment investment, environmental protection and good comprehensive economic benefits.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a method for co-producing methylbenzoic acid, methylbenzonitrile and phthalonitrile. Background technique [0002] Tolunitrile includes m-methylbenzonitrile, p-methylbenzonitrile and o-methylbenzonitrile, all of which are widely used in medicine, pesticides, photosensitive materials and dye intermediates. The existing production of methyl benzonitrile mainly uses high-purity methyl benzoic acid as a raw material, and after preparing methyl benzonitrile through amination and dehydration reactions, the product is refined and purified by rectification. Due to the high boiling point of the product, more rectification residues will be produced in the rectification process, resulting in a large amount of solid waste residue in the rectification column and low product yield. Generally, the molar yield based on toluic acid is not more than 85%. Another production method of methy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/265C07C51/44C07C63/04C07C253/22C07C253/34C07C255/50C07C255/51
CPCC07C51/265C07C51/44C07C253/22C07C253/34C07C63/04C07C255/50C07C255/51
Inventor 王勤波熊振华宗匡曹金辉曾鹏
Owner JIANGXI KEYUAN BIOPHARM
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