MethyIsuIfino benzaldehyde preparation method

A technology for p-methylsulfonyl and methylsulfonyl toluene, which is used in the preparation of p-methylsulfonyl benzaldehyde and the field of chemical oxidation to prepare p-methylsulfonyl benzaldehyde, can solve the problem of difficult reaction control, complex reaction products, low product quality, etc. problem, to achieve the effect of convenient large-scale industrialization, simple preparation method and high product purity

Active Publication Date: 2014-11-19
YANGZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] (1) The preparation of p-thiamphenicyl benzaldehyde by the production process of halogenation and hydrolysis reaction requires a large amount of chlorine gas or liquid bromine. Usually, there are by-products such as mono-substitution and tri-substitution in the operation, accompanied by light and heat. The reaction is difficult to control and It is easy to cause pollution to the environment, and the corrosion of equipment by chlorine gas or liquid bromine is also quite serious;
[0012] (2) The process flow is long, the yield is low, and the reaction product obtained is complex, which makes the separation and purification of the product difficult, and the product quality is low;
[0013] (3) The reaction process is difficult to control, the safety and reliability are poor, and the pollution is serious

Method used

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Examples

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Effect test

Embodiment 1

[0051] Main process equipment: stirred tank reactor, flat plate electrochemical reactor, sedimentation solid-liquid separator, melting equipment, preheating equipment, washing equipment, drying equipment, etc.

[0052] Such as figure 1 Shown, a kind of preparation method of p-thiamphenicol benzaldehyde is to take p-thiamphenicol toluene as raw material through the process method of selective oxidation to prepare p-thiamphenicol benzaldehyde, and described method step is as follows:

[0053] (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;

[0054] (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 with t...

Embodiment 2

[0064] Main process equipment: static mixing reactor, three-dimensional electrochemical reactor, filter solid-liquid separator, melting equipment, preheating equipment, washing equipment, drying equipment, etc.

[0065] The method steps are as follows:

[0066] (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;

[0067] (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;

[0068] (3) Chemical oxidation: In the static mixing reactor, the sulfuric acid solution of potassium dichromate preheated in the previous step is added to the molten reac...

Embodiment 3

[0077] Main process equipment: static mixing reactor, flat plate electrochemical reactor, centrifugal solid-liquid separator, melting equipment, preheating equipment, washing equipment, drying equipment, etc.

[0078] The method steps are as follows:

[0079] (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;

[0080] (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;

[0081] (3) Chemical oxidation: In the static mixing reactor, the sulfuric acid solution of potassium dichromate preheated in the previous step is added to the molten reacti...

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Abstract

The invention relates to a methyIsuIfino benzaldehyde preparation method mainly comprising the steps of: (1) smelting; (2) preheating; (3) chemical oxidation; (4) solid-liquid separation; (5) alkali washing; (6) solid-liquid separation; (7) alcohol washing; (8) solid-liquid separation; (9) drying; and (10) electrochemical oxidation. The process provided by the invention is reasonable, the preparation method is simple, production cost is low, product purity is high, and the process is safe. The method is suitable for realizing large-scale industrialization. The process is a clean production process of methyIsuIfino benzaldehyde preparation. The process satisfies the requirement of green chemical engineering development.

Description

technical field [0001] The invention relates to a preparation method of p-thiamphenicol benzaldehyde, in particular to a method for preparing p-thiamphenicol benzaldehyde by chemical oxidation of p-thiamphenicol toluene as a raw material, which belongs to the technical field of fine chemicals. Background technique [0002] P-thiamphenicol toluene is an aromatic compound, it is a white crystalline powder at room 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 p-thymphenyl benzaldehyde of the present invention has another name called 4-methylsulfonyl benzaldehyde, 4-methylsulfonyl benzaldehyde, 4-methylsulfonyl benzaldehyde. English name 4-Methylsulfonyl benzaldehyde, English alias p-methylsufonyl benzaldehyde, molecular formula is C 8 h 8 o 3 S, the molecular weight is 184.21. P-thiamphenicol b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C317/24C07C315/04
Inventor 王雅琼李树亮孙黎张小兴许文林
Owner YANGZHOU UNIV
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