Preparation method of m-methanesulfonamide

Abstract

The invention discloses a preparation method of m-methanesulfonamide. The preparation method is characterized in that methylsufonyl chloride is dropwise added into a suspension of an optionally proportioned mixture acid-binding agent of m-phenylenediamine, a surface active agent, superfine calcium carbonate or magnesium carbonate or superfine calcium carbonate and magnesium carbonate with the meangrain size of 1 micron or below and water, low-temperature adding is performed, heat insulation is performed after adding, heating and heat insulation are performed, and cooling, filtration and the like are performed to obtain the m-methanesulfonamide. Calcium chloride wastewater or magnesium chloride wastewater or mixed wastewater of calcium chloride and magnesium chloride produced by the process reacts with sodium carbonate in the presence of polyethylene glycol to obtain a superfine acid-binding agent required by the process, and resources are fully utilized. By adding and jointly using the superfine acid-binding agent and the surface active agent, the product yield and quality are obviously improved. Compared with a traditional process, the method has the advantages of being quick, uniform and complete in reaction, producing by-products, simplifying operation, improving the yield and quality, decreasing the three wastes and the like and has good industrial prospect.

Description

technical field [0001] The invention relates to a preparation method of m-methylsulfonamidoaniline, which belongs to the field of organic synthesis. Background technique [0002] m-Methanesulfonamidoaniline is an intermediate of dyes such as disperse red 343, and is also an important intermediate of medicine, pesticides, materials, etc. [0003] The classic synthetic method of m-methanesulfonamidoaniline is to take m-phenylenediamine and methanesulfonyl chloride as raw materials, and is synthesized through aqueous phase reaction in the presence of an acid-binding agent. The literature generally uses calcium carbonate as an acid-binding agent, but calcium carbonate The water solubility is small, and the ordinary calcium carbonate particles are relatively thick and the surface area is small. The reaction product m-methanesulfonamidoaniline is insoluble in water, and it will wrap calcium carbonate, resulting in incomplete acid binding. It is necessary to add more acid to destr...

AI Technical Summary

Problems solved by technology

[0003] The classic synthetic method of m-methanesulfonamidoaniline is to take m-phenylenediamine and methanesulfonyl chloride as raw materials, and in the presence of acid-binding agent, it is synthesized through aqueous phase reaction. Documents generally use calcium carbonate as acid-binding agent, but calcium carbonate The water solubility is small, and the ordinary calcium carbonate particles are relatively coarse and the surface area is small. The reaction product m-methanesulfonamidoaniline is insoluble in water, and it will wrap calcium carbonate, resulting in incomplete acid binding. It needs to add more acid to destroy the excess calcium carbonate, so there are disadvantages such as uneven reaction, low product yield and content, and cumbersome post-treatment.

In addition, the process also produces a large amount of calcium chloride wastewater