Continuous preparation method of acetoacetamido triethylamine sulfonate

Abstract

The invention discloses a continuous preparation method of acetoacetamido triethylamine sulfonate, comprising the following steps of: continuously mixing and dissolving sulfamic acid and dichloromethane, continuously neutralizing with a triethylamine solution to obtain a neutralization reaction solution, introducing the neutralization reaction solution and diketene into a continuous reactor, and carrying out addition acylation reaction to obtain a DKA reaction solution; wherein the molar ratio of n (sulfamic acid) to n (dichloromethane) in the continuous mixing and dissolving process is 1: (1-20), and the temperature is 0-40 DEG C; in the continuous neutralization, the pH of the neutralization is equal to 7-9, and the neutralization temperature is 10-40 DEG C; in the addition acylation reaction, the molar ratio of n (sulfamic acid) to n (diketene) is 1: (0.5-1.5), the acylation reaction temperature is 0-30 DEG C, and the acylation retention time is 0.01 s to 30 min. The invention provides a process for continuously preparing a DKA solution. The process is simple, low in cost, continuous in the whole process and high in yield.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a continuous preparation method of triethylamine acetoacetamidosulfonate. Background technique [0002] The structural formula of triethylamine acetoacetamidosulfonate: [0003] Molecular weight: 282 [0004] Function and use: It is a triethylamine salt of acetoacetamidosulfonic acid, and it is an important intermediate in the process of preparing potassium acesulfonate by sulfamic acid-sulfur trioxide method. [0005] Prior art processing technology: [0006] At present, the conventional process of triethylamine acetoacetamidosulfonate (DKA, the same below) is a tank-type batch production process, and the reaction temperature is low (0 ° C), the reaction time is long (4 ~ 16h), and the acylating agent The dropping speed is slow. If the speed is too fast, the reaction temperature will rise rapidly, which is difficult to control. In severe cases, material flushing...

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Problems solved by technology

[0006] At present, the conventional process of triethylamine acetoacetamidosulfonate (DKA, the same below) is a tank-type batch production process, and the reaction temperature is low (0 ° C), the reaction time is long (4 ~ 16h), and the acylating agent The dropping speed is slow. If the speed is too fast, the reaction temperature will rise rapidly, which is difficult to control. In severe cases, material flushing will occur, and the production safety factor is high, which will affect product quality and yield.

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