Carbon Dioxide → ZINC DIETHYLDITHIOCARBAMATE

HRID 2381560Notes

Reaction equation

HRID 2381560 reaction equation
[Zn:1].[CH2:2]([NH:4][CH2:5][CH3:6])[CH3:3].[OH-].[NH4+].C(=O)=O.[C:12](=[S:14])=[S:13]>O>[CH2:2]([N:4]([CH2:5][CH3:6])[C:12](=[S:13])[S-:14])[CH3:3].[Zn+2:1].[CH2:2]([N:4]([CH2:5][CH3:6])[C:12](=[S:13])[S-:14])[CH3:3]

Participants

7

Reactant 5

HCID 280Carbon DioxideHCID 6348Carbon DisulfideHCID 8021DiethylamineHCID 14923Ammonium HydroxideHCID 23994Zinc

Product 1

HCID 26633ZINC DIETHYLDITHIOCARBAMATE

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
40 °C

Procedure

The sequence of addition of the zinc compound and carbon disulfide is changed to conform to the method of Example 1 of U.S. Pat. No. 6,534,675, and zinc diethyldithiocarbamate (ZDEC-C) is prepared. Add 73 grams of diethylamine to 150 grams of water with temperature controlled at 25° C., then add 900 grams of solution with 3.4% ammonium hydroxide and 1% carbon dioxide which prevents the premature precipitation of the zinc content. Further add 346 grams of zinc ammonia complex solution A as in Example 1 containing 9.56% zinc to the solution and 1.7 grams of emulsifier Tanemul 1203. Lower the solution temperature to 15° C., add 78.5 grams of carbon disulfide slowly into the mixture under heavy agitation over 1 hour while keeping the temperature at or below 20° C. Yellowish white precipitates appear with the addition, and vapor comes out from the mixture. Continue the agitation for 3 hours, then heat the solution gradually to 40° C. Boil the solution, continue agitation for another 2 hours, then vacuum filter the precipitates. The filtrate has a pH of 8.45, and is substantially free of zinc and ammonia. The filtration is finished in 5 minutes. Wash the solid at the filter with 500 ml of 80° C. distilled water four times. Then dry the precipitate at 110° C. for 2 hours to obtain 172 grams of zinc diethyldithiocarbamate with 0.1% moisture content. We call this sample ZDEC-C.

Workup

  1. custom6,534,675, and zinc diethyldithiocarbamate (ZDEC-C) is prepared
  2. customcontrolled at 25° C.
  3. customthe premature precipitation of the zinc content
  4. additionLower the solution temperature to 15° C., add 78.5 grams of carbon disulfide slowly into the mixture under heavy agitation over 1 hour
  5. custombelow 20° C
  6. customYellowish white precipitates
  7. additionappear with the addition, and vapor
  8. customfor 3 hours
  9. customfor another 2 hours
  10. filtrationvacuum filter the precipitates
  11. filtrationThe filtration
  12. washWash the solid at the
  13. filtrationfilter with 500 ml of 80° C.
  14. distillationdistilled water four times
  15. customThen dry the precipitate at 110° C. for 2 hours

Sources & evidence

ORD record
ord-3f9d1be9bf2540398e432c734b8f2e1f
Source dataset
uspto-grants-2012_09
Patent number
US08258180B2

Reaction notes

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