Sulfuric Acid → Sodium Dichromate

HRID 255397

Reaction equation

HRID 255397 reaction equation
O.O.[Cr:3]([O:7][Cr:8]([O-:11])(=[O:10])=[O:9])([O-:6])(=[O:5])=[O:4].[Na+:12].[Na+].OS(O)(=O)=O.O=[Sb]O[Sb]=O>C(O)CCCCCCC>[Cr:3]([O:7][Cr:8]([O-:11])(=[O:10])=[O:9])([O-:6])(=[O:5])=[O:4].[Na+:12].[Na+:12]

Participants

5

Reactant 3

HCID 1118Sulfuric AcidHCID 27652Oxo(oxostibanyloxy)stibaneHCID 108005Sodium dichromate dihydrate

Product 1

HCID 25408Sodium Dichromate

Reagents, catalysts & solvents 1

HCID 9571-OctanolSolvent2×

Conditions

Temperature
105 °C

Procedure

A sample of commercially available sodium dichromate dihydrate 85 percent liquor was stirred in a 1 liter flask while adding 246.5 g 96 percent H2SO4 (236.6 g 100 percent, 1.21 equiv.). External cooling was provided as needed to keep the temperature below 50° C. Antimony trioxide stock solution (6.88 g. 0.40 g 100 percent Sb2O 3 , 0.065 percent based on weight of 100 percent Na2Cr2O7 ), prepared as described in Example 1, was added along with 2 g (0.32 percent based on weight of 100 percent Na2Cr2O7 ) magnetite. Stirring was continued and octanol (12.89 g, 4.76 equiv.) was added over 30 minutes. Cooling was provided as needed to maintain the temperature between 60° and 70° C. After addition of all the octanol, the temperature was allowed to increase to 105° C. (reflux). Stirring at reflux was continued overnight, although based on CO2 release and viscosity the reduction had reached the partial and point of ca. 60 percent within the first hour. The finished paste was not carried through the synthesis cycle. The reactivity of the system toward the reducing agent and the final physical properties of the paste were sufficient confirmation that the overall paste process was the same as with reductions involving the use of CrO3 .

Workup

  1. temperatureExternal cooling
  2. customwas provided
  3. customthe temperature below 50° C
  4. temperatureCooling
  5. customwas provided
  6. temperatureto maintain the temperature between 60° and 70° C
  7. temperature(reflux)
  8. stirringStirring
  9. temperatureat reflux
  10. customThe finished paste was not carried through the synthesis cycle

Sources & evidence

ORD record
ord-179301a228bc4ea4a5a653c0f477b130
Source dataset
uspto-grants-1987_10
Patent number
US04698220

Linked notes

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