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Preparation method of p-methylsulfonylbenzoic acid

A technology of methylsulfonyl benzoic acid and p-methylsulfonyl benzoic acid is applied in the field of preparation of p-methylsulfonyl benzoic acid, and can solve the problems of low selectivity, low conversion rate and yield, difficult control of reaction degree, difficulty in separation and purification, and the like, To achieve the effect of simple preparation method, convenient large-scale industrialization and reasonable process

Inactive Publication Date: 2015-04-01
扬州德耀电气有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] (1) The degree of reaction is not easy to control, and the selectivity, conversion rate and yield of the process are low
[0007] (2) The reaction product is complex, difficult to separate and refine, and the product quality is low;
[0008] (3) poor safety and reliability, serious pollution

Method used

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  • Preparation method of p-methylsulfonylbenzoic acid
  • Preparation method of p-methylsulfonylbenzoic acid
  • Preparation method of p-methylsulfonylbenzoic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Main process equipment: stirred tank reactor, flat plate electrochemical reactor, sedimentation solid-liquid separator, melting equipment, preheating equipment, washing equipment, crystallization equipment, drying equipment, etc.

[0051] Such as figure 1 Shown, a kind of preparation method of thiamphenicol benzoic acid is to carry out selective oxidation to prepare the method for thiamphenicol benzoic acid with p-thiamphenicol toluene as raw material, and its steps are as follows:

[0052] (1) Melting: in a stirred tank, p-thiamphenicol toluene is heated up to 90° C., and the p-thiamphenicol toluene that is solid at room temperature is melted into a liquid material;

[0053] (2) Preheating: In the stirred tank, add sulfuric acid aqueous solution and oxidant potassium dichromate, heat up to 90°C, the concentration of potassium dichromate in the system is 0.5mol / L, the concentration of sulfuric acid is 0.1mol / L, The system is in a liquid state when the material is mixed...

Embodiment 2

[0066] Main process equipment: static mixing reactor, three-dimensional electrochemical reactor, filter solid-liquid separator, melting equipment, preheating equipment, washing equipment, crystallization equipment, drying equipment, etc.

[0067] Proceed as follows:

[0068] (1) Melting: In the falling film melting equipment, p-thiamphenicol is heated up to 150° C., so that the solid p-thiamphenicol at room temperature is melted into a liquid material;

[0069] (2) Preheating: In the stirred tank, add sulfuric acid aqueous solution and oxidant potassium dichromate, heat up to 120°C, the concentration of potassium dichromate in the system is 3.0mol / L, the concentration of sulfuric acid is 8.0mol / L, The system is in a liquid state when the material is mixed with the raw material p-thiamphenicol by heating the temperature;

[0070] (3) Chemical oxidation: In the static mixing reactor, the sulfuric acid aqueous solution of potassium dichromate preheated in the previous step is mi...

Embodiment 3

[0082] Main process equipment: static mixing reactor, flat plate electrochemical reactor, centrifugal solid-liquid separator, melting equipment, preheating equipment, washing equipment, crystallization equipment, drying equipment, etc.

[0083] Proceed as follows:

[0084] (1) Melting: in a stirred tank, p-thiamphenicol toluene is heated up to 120° C., and the p-thiamphenicol toluene that is solid at room temperature is melted into a liquid material;

[0085] (2) Preheating: In the stirred tank, add sulfuric acid aqueous solution and oxidant potassium dichromate, heat up to 100°C, the concentration of potassium dichromate in the system is 2.0mol / L, the concentration of sulfuric acid is 4.0mol / L, The system is in a liquid state when the material is mixed with the raw material p-thiamphenicol by heating the temperature;

[0086] (3) Chemical oxidation: In the static mixing reactor, the sulfuric acid aqueous solution of potassium dichromate preheated in the previous step is mixe...

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Abstract

The invention relates to a preparation method of p-methylsulfonylbenzoic acid. The method provided by the invention mainly comprises the following steps: (1) fusing; (2) preheating; (3) chemical oxidation; (4) solid-liquid separation; (5) neutralization for salt formation; (6) solid-liquid separation; (7) adsorption for removal of impurities; (8) solid-liquid separation; (9) acidification and crystallization; (10) solid-liquid separation; (11) washing; (12) dewatering and drying for obtaining a product p-methylsulfonylbenzoic acid; and (13) electrochemical oxidation. The preparation method provided by the invention is simple, has advantages of reasonable technology, low production cost, high product purity and safe process, is convenient to realize large-scale industrialization, and is a clean production technology which is used for preparing p-methylsulfonylbenzoic acid and accords with green chemical development requirements.

Description

technical field [0001] The invention relates to a method for preparing p-thiamphenicol benzoic acid, in particular to a method for preparing p-thiamphenicol benzoic acid by direct chemical oxidation using p-thiamphenicol toluene as a raw material, which belongs to the technical field of fine chemicals. Background technique [0002] The main raw material of the present invention is p-thymphenyltoluene, which is an aromatic compound, and is a white crystalline powder at normal temperature, and its molecular formula is C 8 h 10 o 2 S, melting range 88℃~89℃, boiling point 312℃, density 1.154g / cm 3 , Soluble in alcohol, ether and other organic solvents, slightly soluble in water. [0003] The product of the present invention is p-thymphenylbenzoic acid, another name is p-carboxy-p-thiamphenyl toluene, p-carboxyphenylmethyl sulfone, p-methylsulfonylbenzoic acid and 4-methylsulfonylbenzoic acid, etc., and its English name is 4-methylsulphonylbenzoic acid, 4-(methylsulfonyl)benz...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C317/44C07C315/04
Inventor 王雅琼李树亮孙黎张小兴许文林
Owner 扬州德耀电气有限公司
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