Hydrochloric Acid → Resorcinol-formaldehyde resin

HRID 2238346Notes

Reaction equation

HRID 2238346 reaction equation
[Cl-].[Ca+2].[Cl-].[C:4]1([CH:11]=[CH:10][CH:9]=[C:7]([OH:8])[CH:6]=1)[OH:5].Cl.[CH2:13]=[O:14]>C(C(C)=O)C.O>[C:4]1([CH:11]=[CH:10][CH:9]=[C:7]([OH:8])[CH:6]=1)[OH:5].[CH2:13]=[O:14]

Participants

7

Reactant 4

HCID 313Hydrochloric AcidHCID 712Formaldehyde2×HCID 5054ResorcinolHCID 5284359Calcium Chloride

Product 1

HCID 159980Resorcinol-formaldehyde resin

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 6569Methyl Ethyl KetoneSolvent

Conditions

Temperature
50 °C

Procedure

After 1336 g of water, 850 g of calcium chloride, 1107.0 g of resorcinol, and 450 g of methyl ethyl ketone were placed in a 5 L flask made of glass and dissolved at 60° C., 4.5 g of 35% hydrochloric acid was charged into the reaction vessel. While the reaction system was cooled to 50° C. and maintained at 50° C., 490 g of 37% formalin was added dropwise over a period of 45 minutes and, after the completion of the dropwise addition, the mixture was further stirred at 50° C. for 1 hour to cause a liquid-liquid heterogeneous reaction to proceed. Thereafter, 40 g of 37% formalin was added dropwise over a period of 45 minutes and, after the completion of the dropwise addition, the mixture was further stirred at 50° C. for 1 hour to cause a liquid-liquid heterogeneous reaction to proceed. While the reaction system is maintained at the same temperature, it was allowed to stand and separate into two layers, and then an underlying aqueous phase was drawn off. The organic phase was diluted with 1500 g of methyl ethyl ketone and 750 g of water was added thereto. Furthermore, while maintaining the same temperature, the reaction system was stirred for 1 hour and, after allowing to stand, separated into two layers and then the aqueous layer was drawn off to obtain a methyl ethyl ketone solution of a resorcinol-formalin resin.

Workup

  1. dissolutiondissolved at 60° C.
  2. temperaturemaintained at 50° C.
  3. additionafter the completion of the dropwise addition
  4. customa liquid-liquid heterogeneous reaction
  5. additionafter the completion of the dropwise addition
  6. stirringthe mixture was further stirred at 50° C. for 1 hour
  7. customa liquid-liquid heterogeneous reaction
  8. temperatureWhile the reaction system is maintained at the same temperature, it
  9. customseparate into two layers
  10. additionThe organic phase was diluted with 1500 g of methyl ethyl ketone and 750 g of water
  11. additionwas added
  12. temperatureFurthermore, while maintaining the same temperature
  13. stirringthe reaction system was stirred for 1 hour
  14. customseparated into two layers

Sources & evidence

ORD record
ord-541c38f783654fb5ad2116444e17debb
Source dataset
uspto-grants-2010_05
Patent number
US07718752B2

Reaction notes

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