Process for preparing potassium hydrogen persulfate composite salts

Abstract

The present invention discloses the preparation process of potassium monopersulfate composite salt. The preparation process includes the following steps: the oxidation reaction between hydrogen peroxide and fuming sulfuric acid; the neutralization between the potassium hydroxide aqua and the product of the preceding step to obtain the water solution of the destination product potassium monopersulfate; concentration; adding stabilizer, cooling to crystallize, collecting solid potassium monopersulfate, and drying to obtain the product. The reaction may be performed in a conventional reactor, and the process of the present invention has simple operation, no need of special equipment and high product stability, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of potassium hydrogen persulfate compound salt. Background technique [0002] Potassium monopersulfate compound salt, also known as potassium persulfate compound salt, potassium monopersulfate compound salt, potassium monopersulfate compound salt or potassium monopersulfate compound salt, is a free-flowing white granular powder, Soluble in water, its molecular formula is KHSO 5 . [0003] Potassium monopersulfate compound salt is a very effective oxidizing agent and disinfectant. It is stable, convenient and has a wide range of uses. Its application fields involve oral hygiene, swimming pool and hot spring water disinfection, circuit board etchant, pulp bleaching, wool fabric Anti-shrinkage treatment, precious metal extraction, etc.; Potassium hydrogen persulfate compound salt is also an important auxiliary agent in organic synthesis, which can epoxidize the double bonds in organic molecules, and is a fre...

AI Technical Summary

Problems solved by technology

[0004] At present, the method for industrialized preparation of potassium monopersulfate compound salt is the anodic oxidation method, that is, electrolyzing sulfuric acid with a platinum electrolytic cell to generate peroxodisulfuric acid, then hydrolyzing it into peroxymonosulfuric acid at room temperature, adding potassium carbonate, and obtaining potassium hydrogen persulfate Compound salt, this method requires large investment, high energy consumption and complicated operation

[0005] In order to solve the problem of high energy consumption and large investment in the preparation of potassium monopersulfate compound salt by anodic oxidation, U.S. authorized patent US 5,139,763 discloses the chemical preparation method of potassium monopersulfate compound salt. Sulfuric acid is reacted to produce Caro's acid, and potassium compound is commonly used to react with Caro's acid to prepare KHSO 5 、KHSO 4 and K 2 SO mixture, this mixture was added to enriched KHSO 5 A solution in which KHSO is adjusted 5 / (KHSO 4 +K 2 SO) ratio, so that KHSO in the final mixture 5 / (KHSO 4 +K 2 SO) between 1.4-6.1, separate the mixture to form a slurry sample, crystallize and dry through a vacuum tube, so that the final weight concentration is 14-60%

Although this method overcomes the high energy consumption problem of the electrochemical method, the reaction steps are more loaded down with trivial details, and there are still the following four problems: 1) still need to prepare the KHSO rich in addition 5 mother liquor to enhance KHSO 5 / (KHSO 4 +K 2 SO) ratio; 2) adding MgCO 3 To prevent the mixture from agglomerating, etc.; 3) when making Caro's acid, hydrogen peroxide and oleum carry out oxidation reaction, the reaction temperature is higher, the exotherm is violent, and it is easy to boil, and the opening of the reaction device is easy to cause danger and affect the environment Hygienic; 4) the obtained potassium hydrogen persulfate compound salt humidity is big, and active oxygen content is low, is difficult to reach the quality requirement of product

However, there are still high impurity content of the product due to the addition of stabilizers and crystal modifiers, low vacuum concentration efficiency, large water content after concentration, serious pollution in the open preparation process, adverse effects on human body and environment, large-scale industrial application There are still some problems in