Hydrochloric Acid → Resorcinol-formaldehyde resin
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
Reactant 4
Product 1
Reagents, catalysts & solvents 2
Conditions
- Temperature
- 50 °C
Procedure
After 2660 g of water, 1710 g of calcium chloride, 738 g of resorcinol, and 300 g of methyl ethyl ketone were placed in a 5 L flask made of glass and dissolved at 60° C., 9 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., 353 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 to obtain a methyl ethyl ketone solution of a resorcinol-formalin resin. The organic phase was diluted with 1000 g of methyl ethyl ketone and 500 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. The organic phase was again diluted with 1000 g of methyl ethyl ketone and distillation was conducted at the azeotropic temperature of water and methyl ethyl ketone to remove water. Then, the mixture was cooled to room temperature and filtrated to obtain a methyl ethyl ketone solution of a resorcinol-formalin resin.
Workup
- dissolutiondissolved at 60° C.
- temperaturemaintained at 50° C.
- additionafter the completion of the dropwise addition
- customa liquid-liquid heterogeneous reaction
- temperatureWhile the reaction system is maintained at the same temperature, it
- customseparate into two layers
Sources & evidence
- ORD record
- ord-448f6bede7094c0dac08cf243d8b7e37
- Source dataset
- uspto-grants-2010_05
- Patent number
- US07718752B2
Reaction notes
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