Hydroquinone bis(2-hydroxyethyl)ether synthesis
- Product Name:Hydroquinone bis(2-hydroxyethyl)ether
- CAS Number:104-38-1
- Molecular formula:C10H14O4
- Molecular Weight:198.22
Yield:104-38-1 99.3%
Reaction Conditions:
Stage #1: hydroquinonewith 1,1'-bis-(diphenylphosphino)ferrocene in diethylene glycol dimethyl ether at 100;Autoclave;Inert atmosphere;
Stage #2: oxirane in diethylene glycol dimethyl ether at 130 - 135; for 4 h;Solvent;Temperature;
Steps:
9 Example 9
432 g of the diethylene glycol dimethyl ether obtained in Example 9 was recovered, together with 550 g of hydroquinone,1,1'-bis (diphenylphosphine) ferrocene 1.0g was charged into a reaction kettle and evacuated by means of a vacuum pump,The air inside the reaction kettle was replaced with nitrogen, and the temperature was raised under nitrogen protection after replacing three timesTo 100 , insulation 3-4 hours, the kettle completely material. When the hydroquinone is completely finished,The temperature was then evacuated for 20 minutes to remove the low boiling point substance in the kettle and then continued to the ringEthylene oxide 506g, added within 5 hours, the control reaction temperature of 130-135 ° C, the reactor pressureForce in -0.05-0.4Mpa, plus 4 hours after the end of incubation to continue the reaction; reaction is completed, cooling to80 ° C, vacuum degassing to remove unreacted ethylene oxide, the mother liquor gradually heated to 120 ° C by minusPressure distillation 7 hours in the product, the solvent vapor cooling can be re-applied after receiving.The product was detected by analysis: hydroquinone dihydroxyethyl ether content of 99.1%, unreacted pairsThe color of the sample was 20 and the hydroxyl value was determined to be 559.8 mg KOH / g.
References:
CN105523905,2016,A Location in patent:Paragraph 0023; 0057; 0058; 0059
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