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Preparation method of potassium peroxymonosulfate

A technology of potassium monopersulfate compound salt and potassium monopersulfate, which is applied in the direction of peroxyhydrate/peroxyacid, can solve the problems of harsh reaction temperature, instability of peroxysulfuric acid, and danger, and achieve The active oxygen content is qualified, the product quality is stable, and the effect of reducing the degree of danger

Inactive Publication Date: 2018-11-16
SHANGYU JIEHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

High-concentration hydrogen peroxide reacts with fuming sulfuric acid. The raw material itself is a hazardous chemical. The reaction between the two is violent and exothermic. The requirements for the refrigeration system and reaction temperature are strict. Violent decomposition can cause explosion, causing danger

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1, step one, the potassium peroxodisulfate solution of 1630g 30% is joined in the four-neck flask of 2000mL band stirring and thermometer, adds 4.5g nano activated carbon loading Al 2 o 3 Catalyst, use a water bath to control the temperature of the solution inside the flask, keep the hydrolysis temperature at 50°C, and the hydrolysis time for 8 hours; step 2, detect that the monomeric active oxygen of potassium hydrogen persulfate reaches 1.68%, and add 6g of stabilizer after the solution is filtered to remove the catalyst Sodium tripolyphosphate, then slowly add 112.5g of potassium bisulfate, stir and mix; step 3, add 102g of 50% potassium hydroxide solution to neutralize, the temperature is controlled at about 40°C, after the addition, keep stirring for 30min in a vacuum The concentration is 0.098MPa, concentrated at 45°C under vacuum, then cooled to 0°C for crystallization, centrifuged, and dried to obtain 412g of potassium monopersulfate compound salt, th...

Embodiment 2

[0028] Embodiment 2, step one, the potassium peroxodisulfate solution of 1300g 15% is joined in the four-neck flask of 2000mL band stirring and thermometer, adds 6g nanometer activated carbon loading Al 2 o 3 Catalyst, use a water bath to control the temperature of the solution inside the flask, keep the hydrolysis temperature at 30°C, and the hydrolysis time for 12 hours; Step 2, detect that the monomer active oxygen of potassium hydrogen persulfate reaches 1.03%, and add 3.5g of coke after the solution is filtered to remove the catalyst Potassium phosphate, then slowly add 52g of solid potassium bisulfate, stirring and mixing; Step 3, then add 54g of 40% potassium hydroxide solution for neutralization, the temperature is controlled at about 30°C, after the addition, keep stirring for 1min, and in a vacuum of Concentrate at 35°C under 0.1MPa vacuum, then cool to -5°C to crystallize, centrifuge, and dry to obtain 208g of potassium monopersulfate compound salt, the active oxyge...

Embodiment 3

[0029] Embodiment 3, step one, 1580kg 30% potassium peroxodisulfate solution is added in 2 cubic hydrolysis kettles, add 5kg nano activated carbon loading Al 2 o 3 Catalyst, use frozen brine and steam coil to control the hydrolysis temperature of the solution, keep the solution hydrolysis temperature at 45°C, and the hydrolysis time for 10h; step 2, the detection of potassium hydrogen persulfate monomer active oxygen reaches 1.56%, and the solution passes through the filter Remove the catalyst and enter the neutralization kettle, add stabilizers 1.8kg sodium acid pyrophosphate and 2.5kg sodium pyrophosphate to the neutralization kettle, then slowly add 120kg potassium bisulfate solid, stir and mix for 1 hour; step 3, then add 118kg48% Potassium hydroxide solution is neutralized, the temperature is controlled at about 45°C, after the feeding is completed, it is kept under stirring for 1 hour, concentrated at 45°C under a vacuum of 0.099MPa, cooled to 0°C for crystallization, ce...

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PUM

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Abstract

The invention discloses a preparation method of potassium peroxymonosulfate. The preparation method comprises following steps: adding a potassium peroxydisulfate solution into a hydrolysis reactor, carrying out hydrolysis under the action of a catalyst to generate potassium peroxymonosulfate and potassium hydrogen sulfate; after the hydrolysis degree reaches the requirement, removing the catalystfrom the solution by a filter, adding the solution into a neutralization reactor, adding a stabilizing agent into the neutralization reactor, then adding potassium hydrogen sulfate solids, stirring, mixing; then adding potassium hydroxide into the neutralization reactor to carry out neutralization reactions; carrying out vacuum concentration, cooling, crystallizing, performing centrifugal separation, and baking to obtain a dry product of potassium peroxymonosulfate. Potassium peroxydisulfate is used to replace high concentration hydrogen peroxide, reacts with fuming sulfuric acid, and is hydrolyzed to generate potassium peroxymonosulfate and potassium hydrogen sulfate under the action of a catalyst; the reactions are mild, the reaction heat is little, the danger of reactions is reduced effectively; under the action of the catalyst, the degree of directional hydrolysis is high, the active oxygen content of products is qualified, and the product quality is stable.

Description

technical field [0001] The invention relates to the technical field of peroxide preparation, in particular to a preparation method of potassium monopersulfate compound salt. Background technique [0002] Potassium hydrogen persulfate compound salt is a compound salt composed of potassium hydrogen persulfate, potassium hydrogen sulfate and potassium sulfate. It is a widely used disinfectant and bactericide with strong oxidizing properties. It is mainly used for washing agent, denture cleaner, dry bleaching agent, anti-shrink treatment agent for wool fabrics, initiator for polymers, microetching agent for printed circuit boards and wastewater treatment. [0003] The methods for preparing potassium hydrogen persulfate compound salt are chlorosulfonic acid method, anodic oxidation method and fuming sulfuric acid method at present, wherein main method is fuming sulfuric acid method. [0004] The fuming sulfuric acid method is to add high-concentration fuming sulfuric acid dropwi...

Claims

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Application Information

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IPC IPC(8): C01B15/08
CPCC01B15/08
Inventor 罗力军陶彭均陶卓奇
Owner SHANGYU JIEHUA CHEM
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