A method for co-producing methylbenzoic acid, methylbenzoyl chloride and phthaloyl chloride

A technology of toluoyl chloride, phthaloyl chloride, and toluic acid is applied in chemical instruments and methods, separation/purification of carboxylic acid compounds, preparation of carboxylate salts, etc., and can solve the problem of low yield of target products, Problems such as large amount of solid waste and single product structure

Active Publication Date: 2020-10-20
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 of low yield of target product, large amount of solid waste, and single product structure in the prior art, and provide a co-production methyl alcohol with simple process, low equipment investment, environmental protection and good comprehensive benefits. Methods for Benzoic Acid, Toluoyl Chloride, and Phthaloyl Chloride

Method used

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  • A method for co-producing methylbenzoic acid, methylbenzoyl chloride and phthaloyl chloride
  • A method for co-producing methylbenzoic acid, methylbenzoyl chloride and phthaloyl chloride
  • A method for co-producing methylbenzoic acid, methylbenzoyl chloride and phthaloyl chloride

Examples

Experimental program
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Effect test

Embodiment 1

[0100] 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

[0103] 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.

[0104] The liquid in the first distillation tower was rectified to obtain 889.4 g of p-toluic acid product with a purity of 99.0% at the top of the tower, and 1226.0 g of a high-boiling liquid in the bottom ...

Embodiment 3

[0106] 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 bottom liquid of the primary distillation tower 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.

[01...

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Abstract

The invention discloses a method of co-producing methyl benzoic acid, methylbenzoyl chloride and phthaloyl dichloride. The method comprises the following steps: (1) continuously introducing xylene, acatalyst and oxygen-containing gas into an oxidizing reactor to react to obtain an oxidized reaction solution; (2) rectifying and separating the oxidized reaction solution to obtain a low-boiling-point component and an initial evaporative tower bottom; (3) rectifying the initial evaporative tower bottom to obtain a methyl benzoic acid product and a tower bottom; (4) carrying out an acylating chlorination reaction on the tower bottom and an acylating chlorination reagent to obtain an acyl chloride reaction solution; and (5) rectifying and separating the acyl chloride reaction solution to separately obtain methylbenzoyl chloride and phthaloyl dichloride products. The method provided by the invention has the advantages of being simple in process, small in equipment investment, green and environment-friendly and good in comprehensive economical benefit.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a method for co-producing toluic acid, toluyl chloride and phthaloyl chloride. Background technique [0002] Toluoyl chloride includes m-toluoyl chloride, p-toluoyl chloride and o-toluoyl chloride, which are widely used in medicine, pesticides, photosensitive materials and dye intermediates, such as DEET, fluorescent whitening Agent OB-1 etc. The production of existing toluoyl chloride all takes high-purity toluic acid as raw material, and after preparing toluoyl chloride by acid chloride reaction, 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%. [0003] Phthaloyl chloride inc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/265C07C51/44C07C63/04C07C51/60C07C51/64C07C63/24C07C63/15
CPCC07C51/265C07C51/44C07C51/60C07C51/64C07C63/04C07C63/24C07C63/15
Inventor 王勤波熊振华宗匡曹金辉曾鹏
Owner JIANGXI KEYUAN BIOPHARM
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