Potassium perchlorate synthesis method
  • 2017-04-20 17:59:40
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1. electrolytic-metathesis method

The industrial sodium chlorate in the dissolved tank by adding water, through the steam at 45 ~ 50 ℃ to dissolve, so saturated (solution of sodium chlorate 650 ~ 700 g / L) after the addition of barium hydroxide to remove impurities such as chromate, filter The electrolytic solution was sent to the electrolytic cell and subjected to continuous electrolysis at a current intensity of 1500 A, a tank voltage of 5 to 6 V, DH 6 to 7, and an electrolysis temperature of 50 to 70 ° C to produce a solution of sodium perchlorate 700 g / L into the reactor, preheated to 60 ~ 80 ℃, and then with the solution of potassium chloride solution decomposition reaction, when the temperature rose to 90 ~ 100 ℃ when the reaction is completed, the reaction solution cooled to 30 ° C precipitation of potassium perchlorate crystals , Centrifuged, impregnated, centrifugal separation, at 100 ~ 110 ℃ air drying, made of potassium perchlorate finished. The reaction equation is as follows:
2. From the disproportionation reaction of potassium chlorate, add 50 ~ 80g KClO3 in 100 ~ 150mL refractory crucible. Slowly heated to about 100 ℃, and then increase the fire to make it quickly melt, but to prevent overheating. 30 ~ 35min after the crucible material thickened, the surface into a hard shell. When there is no more oxygen to escape, stop heating, and the crucible cooling, the material for the powder. Take 65 ~ 70g powder, add 200mL water, boil to dissolve, hot filter. The filtrate was rapidly cooled, filtered, and the precipitated crystals were washed twice with cold water. Verify that there is no Cl- (with AgNO3). If necessary, recrystallize again. The crystals were dried at 80 ° C and yielded 25 to 30 g.
3. Preparation of NaClO4 and KCl 100g pure NaClO4 was dissolved in 80mL water and filtered. 54 g of pure KCl was dissolved in 170 mL of water. To the NaClO4 solution was added KCl solution. The mixture will warm to 40 ° C (exothermic reaction). The mixture was cooled to 15 to 20 ° C to precipitate KClO4 crystals. Filter and wash to remove all Cl-. The washed crystals were further filtered and dried at 80 ° C to yield 90 g.
4. The industrial product of potassium perchlorate dissolved in boiling water, hot filter, the filtrate heated to the crystallization of crystalline film, cooling crystallization, filtration drying, with a small amount of ice water washing crystallization, drying, drying at 80 ℃, that reagent Potassium perchlorate.
5. The reagent sodium perchlorate solution was formulated as an aqueous solution with a content of 55% and an aqueous potassium chloride solution with a content of 25% was added to carry out the reaction:

After the reaction is completed, the mixture is cooled to 15 to 20 ° C, filtered and dried, and the resulting crystals are washed with water to a Cl-content and centrifuged and dried at 80 ° C to obtain potassium perchlorate.

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