ChemicalBook CAS DataBase List peroxomonosulphuric acid

peroxomonosulphuric acid synthesis

13synthesis methods

Product Name:peroxomonosulphuric acid
CAS Number:7722-86-3
Molecular formula:H2O5S
Molecular Weight:114.08

peroxomonosulphuric acid may be prepared by several methods depending on what form of the reagent is desired. Most commonly, it is made by treating potassium perfulfate (K2S2O8) with sulfuric acid. The dry form is prepared by slowly stirring 100 g K2S2O8 into 60 mL of concentrated H2SO4, followed by adding 300 g potassium sulfate. A liquid Caro’s acid is obtained by slowly stirring K2S2O8 into three times the mass of H2SO4. The dilute form of the reagent may be obtained by either mixing K2S2O8 to 40% H2SO4 or by treating K2S2O8 with H2SO4 and adding ice to the mixture.
Alternatively, peroxomonosulphuric acid may be prepared from hydrogen peroxide by treatment with either chlorosulfonic acid or with H2SO4 at –40°C. A 90% H2O2 is used in the preparation.
peroxomonosulphuric acid is a strong oxidizing agent and is very unstable. All laboratory preparations must be carried out in an explosion-proof fume hood under temperature- controlled conditions and in the absence of impurities and oxidizable substances.

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Yield:-

Reaction Conditions:

Stage #1:sulfuric acid;dihydrogen peroxide in water at -2 - 8;
Stage #2:sulfur trioxide in water at -2 - 8; for 1.5 h;Product distribution / selectivity;

Steps:

2, 3
2. Recipe No.2 20.54 g of 76% H₂O₂(approx. 0.46 mol H₂O₂) was slowly added to 10.02 g 98% H₂SO₄(approx. 0.1 mol H₂SO₄). 46.67 g of 26% oleum was slowly added through a drip tube to the weak Caro's acid over a period of 1.5 hours. The temperature was maintained at between -2 to 8° C. during both steps of the Caro's acid production. The rich Caro's acid solution was added to 47.23 g deionized H₂O while controlling the temperature between 0-6° C.; 3. Recipe No.3 Add a supra-stoichiometric ratio of 70-99.6% H₂O₂to agitated 90-100% H₂SO₄while controlling the temperature at <20° C., and preferably <15° C., and more preferably <10° C. The resulting weak Caro's acid solution is converted to a rich Caro's acid solution by slowly or incrementally adding to a solution of 1-75% oleum while controlling the temperature at <20° C., preferably <15° C., and more preferably <10° C. to produce a rich Caro's acid solution.

References:

Martin, Perry L.;Martin, Roy W. US2005/167635, 2005, A1 Location in patent:Page/Page column 4

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References

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