Sulfate Ion → Hydrogen Peroxide

HRID 1647266Notes

Reaction equation

HRID 1647266 reaction equation
C(O)(=O)/C=C\C(O)=O.C12CC(C=C1)C1C(OC(=O)C21)=O.S([O-])([O-])(=O)=O.[OH-].[Na+:27].C(O)(=O)C=C.[S:33]([O:37][O:38][S:39]([O-:42])(=[O:41])=[O:40])([O-:36])(=[O:35])=[O:34].[Na+].[Na+].S(S([O-])=O)([O-])(=O)=O.[Na+].[Na+]>O>[S:33]([O:37][O:38][S:39]([O-:42])(=[O:41])=[O:40])([O-:36])(=[O:35])=[O:34].[Na+:27].[Na+:27].[OH:37][OH:38]

Participants

10

Reactant 7

HCID 1117Sulfate IonHCID 6581Acrylic Acid2×HCID 13223826-62-0HCID 14798Sodium Hydroxide2×HCID 62655Sodium PersulfateHCID 444266Maleic AcidHCID 656671Sodium Pyrosulfite

Product 2

HCID 784Hydrogen PeroxideHCID 62655Sodium Persulfate

Reagents, catalysts & solvents 1

HCID 962WaterSolvent5×

Conditions

Temperature
95 °C

Procedure

To a half liter, 4-neck flask equipped with a mechanical stirrer, reflux condenser, thermometer, and inlets for the gradual addition of monomer and initiator solution was added 31.9 grams of deionized water, 25.52 grams of maleic acid 28.75 grams of 5-norbornene-2,3-dicarboxylic acid anhydride, 3.83 grams of a 0.15% aqueous ferrous sulfate heptahydrate solution, 0.83 grams of a 0.15% aqueous coppper sulfate solution and 55.51 grams of 50% by weight aqueous sodium hydroxide. The contents of the flask were heated to 95° C. A monomer solution of 92.51 grams of acrylic acid and 63.8 grams of deionized water, and an initiator solution of 4.78 grams of sodium persulfate, 26.60 grams of 30% by weight aqueous hydrogen peroxide and 31.90 grams of deionized water were prepared. 9.57 grams of the glacial acrylic acid were added to the flask. After two minutes. 6.38 grams of the initiator solution were added to the flask. The contents of the flask were then heated to 100° C. The remainder of the monomer feed and initiator solution were then fed into the flask linearly and separately while stirring over two hours and thirty minutes. Once the additions were complete, 1.0 grams of sodium persulfate dissolved in 5.0 grams of deionized water was added. The system was kept at 100° C. for 30 minutes. The system was then cooled to 80° C. A solution of 5.0 grams of sodium metabisulfite dissolved in 20.0 grams of deionized water was added. The system was then cooled to 50° C. and the pH was adjusted from 3.9 to 7.9 with 100.0 grams of 50% by weight aqueous sodium hydroxide.

Workup

  1. customTo a half liter, 4-neck flask equipped with a mechanical stirrer
  2. temperaturereflux condenser
  3. additionthermometer, and inlets for the gradual addition of monomer and initiator solution
  4. temperatureThe contents of the flask were then heated to 100° C
  5. additionwas added
  6. waitThe system was kept at 100° C. for 30 minutes
  7. temperatureThe system was then cooled to 80° C
  8. additionwas added
  9. temperatureThe system was then cooled to 50° C.

Sources & evidence

ORD record
ord-902d91f3deae4e5eaa3d65bd8bf17dce
Source dataset
uspto-grants-1995_07
Patent number
US05430114

Reaction notes

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