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MethyIsuIfino benzaldehyde preparation method

A technology for p-methylsulfonyl and methylsulfonyl toluene is applied in the field of chemical oxidation to prepare p-methylsulfonyl benzaldehyde and p-methylsulfonyl benzaldehyde, and can solve problems such as environmental pollution, equipment corrosion, difficulty in product separation and purification, and the like , to achieve the effect of reducing costs and reducing pollution

Active Publication Date: 2013-10-23
YANGZHOU UNIV
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  • Summary
  • 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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Embodiment 1

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

[0052] Such as figure 1 As shown, a method for preparing p-methylsulfonyl benzaldehyde is a process method for preparing p-methylsulfonyl benzaldehyde through selective oxidation of p-methylsulfonyl toluene as a raw material, and the method steps are as follows:

[0053] (1) Melting: In a stirred tank, heat the p-methylsulfonyl toluene to 90° C. to melt the p-methylsulfonyl toluene in a solid state at room temperature into a liquid material;

[0054] (2) Preheating: Add sulfuric acid aqueous solution and oxidant potassium dichromate into the stirred tank, and heat to 90°C. The concentration of potassium dichromate in the system is 0.5 mol / L, and the concentration of sulfuric acid is 0.1 mol / L. The system is in a liquid state when the material is mixed with the raw material p-methy...

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, heat the p-methylsulfonyl toluene to 150°C, and melt the p-methylsulfonyl toluene in a solid state at room temperature into a liquid material;

[0067] (2) Preheating: Add sulfuric acid aqueous solution and oxidant potassium dichromate to the stirred tank, and heat to 120°C. The concentration of potassium dichromate in the system is 3.0 mol / L, and the concentration of sulfuric acid is 8.0 mol / L. The system is in a liquid state when the material is mixed with the raw material p-methylsulfonyl toluene by heating up;

[0068] (3) Chemical oxidation: In a static mixing reactor, add the preheated sulfuric acid aqueous solution of potassium dichromate in the previous step to the mol...

Embodiment 3

[0077] Main process equipment: static mixing reactor, flat 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, heat the p-methylsulfonyl toluene to 120° C. to melt the p-methylsulfonyl toluene in a solid state at room temperature into a liquid material;

[0080] (2) Preheating: In the stirred tank, add sulfuric acid aqueous solution and oxidant potassium dichromate, heat to 100℃, the concentration of potassium dichromate in the system is 2.0mol / L, and 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-methylsulfonyl toluene by heating up;

[0081] (3) Chemical oxidation: In a static mixing reactor, add the preheated sulfuric acid aqueous solution of potassium dichromate in the previous step to the molten reaction raw material p-methyl...

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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 method for preparing p-methylsulfone benzaldehyde, in particular to a method for preparing p-methylsulfone benzaldehyde by chemical oxidation using p-methylsulfone toluene as a raw material, and belongs to the technical field of fine chemicals. Background technique [0002] P-Methylsulfonyl toluene is an aromatic compound, it is a white crystalline powder at room temperature, the molecular formula is C 8 H 10 O 2 S, melting range 88℃~89℃, boiling point 312℃, density 1.154g / cm 3 , Soluble in organic solvents such as alcohol and ether, slightly soluble in water. [0003] The product of the invention, p-methylsulfonylbenzaldehyde, is also known as 4-methylsulfonylbenzaldehyde, 4-methylsulfonylbenzaldehyde and 4-methylsulfonylbenzaldehyde. 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-Methylsulfonyl benzaldehyde is yellow cry...

Claims

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Application Information

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Patent Type & Authority Applications(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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