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Method for preparing permonosulfuric hydrogen-pottassium compound salt

A technology of potassium hydrogen persulfate compound salt and hydrogen peroxide, which is applied in the direction of peroxyhydrate/peroxyacid, can solve the problems of -15°C, severe heat release, difficulty in realizing industrial production, etc., and achieve good results Stability, simple production process, and easy operation

Inactive Publication Date: 2004-09-15
陶华西
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There are mainly three kinds of existing methods for preparing potassium monopersulfate compound salt; one is to react hydrogen peroxide with measured chlorosulfonic acid to obtain peroxymonosulfuric acid, and then add a certain proportion of potassium carbonate to obtain hydrogen peroxymonosulfate Potassium compound salt, the reaction temperature of this method requires -15°C, and the heat release during the reaction is too violent, it is difficult to realize industrial production
Another method is the anodic oxidation method, that is, using a platinum electrolytic cell to electrolyze sulfuric acid to generate peroxodisulfuric acid, which is then hydrolyzed into peroxymonosulfuric acid at room temperature, and potassium carbonate is added to obtain potassium bisulfate compound salt. This method requires a large investment , high energy consumption, complicated operation
Another method is the sulfuric acid method, that is, using concentrated sulfuric acid, hydrogen peroxide and potassium hydroxide at a lower concentration as raw materials. Product Quality Requirements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Add 180g of 50% hydrogen peroxide to a 2000ml four-necked flask with stirring and a thermometer, add 2.0g of sodium tripolyphosphate stabilizer, and use an ice bath to control the temperature so that the system temperature reaches about 5°C, and start adding 50 % oleum 280g, now the temperature is controlled at about 10°C, the stirring speed is 300 rev / min, keep the same temperature after fully stirring, add dropwise 436g of 45% potassium hydroxide solution and 6.0g magnesium hydroxide crystal form modifier , let stand for 10 minutes, the mixture was vacuum concentrated, cooled and crystallized, centrifuged, and the crystals were dried at 50-60° C. to obtain 322 g of dry potassium monopersulfate compound salt.

Embodiment 2

[0014] Take 128.5g of 70% hydrogen peroxide, add 1.5g of sodium acid pyrophosphate, 1.2g of sodium hexametaphosphate crystal form improver, mix well and put it into a four-necked flask, start to drop 50% of the fuming Sulfuric acid 280g, after the reaction, add dropwise 436g of 45% potassium hydroxide solution and a crystal form modifier composed of 3.0g magnesium oxide and 3.5g magnesium sulfate, leave standstill for 10 minutes, the mixture is concentrated in vacuo, crystallized by cooling, and centrifuged to obtain 330g over Potassium bisulfate salt dry product.

Embodiment 3

[0016] Get 128.5g of 70% hydrogen peroxide, add a stabilizer composed of 0.5g sodium acid pyrophosphate, 0.6g sodium pyrophosphate, and 1.0g potassium acid pyrophosphate, mix well and put it into a four-necked flask. In the case of temperature control, add 256g of 55% oleum. At this time, the temperature of the system is about 10°C. After the dropwise addition, keep it warm for 2-3 hours, add 300ml of water to dilute, and then add 453g of 40% potassium hydroxide solution , and a crystal form modifier composed of 2.0g magnesium oxide, 1.5g magnesium hydroxide, and 2.0g magnesium carbonate, left to stand for 10 minutes, the mixture was concentrated in vacuo, crystallized by cooling, and centrifuged to obtain 332g of potassium hydrogen persulfate compound salt dry product .

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Abstract

The invention is a potassium peroxy-monohydrosulfate compound salt preparing method, using oleum, perhydrol and potassium hydroxide as raw material. Firstly, adding stabilizing agent-containing perhydrol in the reactor, then dropping in the oleum to react, then dropping in potassium hydroxide solution and at the same time adding in crystal shape modifier, vacuum-condensing, cooling and crystallizing, and then drying to obtain its dried product; the perhydrol solution concentration is 45-80% and the oleum concentration 35-65%. It uses oleum to replace the vitriol oil and thick perhydrol solution to replace dilute perhydrol solution, and adds in potassium hydroxide to adjust the components. It has better stability.

Description

technical field [0001] The invention relates to a preparation method of potassium hydrogen persulfate compound salt, which belongs to the technical field of preparation of inorganic peroxides. Background technique [0002] Potassium hydrogen persulfate compound salt is also called potassium hydrogen persulfate compound salt and potassium monopersulfate compound salt. It is a compound salt composed of three components: potassium hydrogen persulfate, potassium hydrogen sulfate and potassium sulfate. The molecular formula is 2KHSO 5 -KHSO 4 -K 2 SO 4 , with a molecular weight of 614.7, is a widely used disinfectant and bactericide with strong oxidizing properties. It is mainly used as detergent, denture cleaner, dry bleaching agent, anti-shrink treatment agent for wool fabrics, polymer initiator, Printed circuit board microetch and waste water treatment. [0003] There are mainly three kinds of existing methods for preparing potassium monopersulfate com...

Claims

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Application Information

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IPC IPC(8): C01B15/08
Inventor 陶华西郑龙罗力军杨国男
Owner 陶华西
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