1-(2,3-Epoxypropoxy)-2,2-bis((2,3-epoxypropoxy)methyl)butane → Trimethylolpropane

Temperature

50 °C

A 0.15 liter autoclave was charged with 23.2 g of MMA (0.75 moles). The temperature was maintained at 50° C. With agitation, 41.8 g of a 50% solution trimethylolpropane triglycidyl ether (0.05 moles; 0.15 eq) in methanol was added slowly at 0.7 g/min. No temperature increase was observed during the addition. After addition was complete, the reaction mixture was agitated for 30 minutes. The reaction was complete when the IR bands for the epoxy group at 914, 840 and 755 cm-1 were no longer present. The unreacted MMA was then removed from the reaction mixture by venting to a collection vessel. Residual MMA and methanol were removed from the product by reduced pressure distillation. 24.3 g of the MMA adduct of the triglycidyl ether of trimethylolpropane was obtained (95% of theory). The product had a total amine value of 291.3 mg KOH/g, an N--H equivalent weight of 254.2. This product will be identified as TMPTGEMMA-2 in following examples.

1. additionA 0.15 liter autoclave was charged with 23.2 g of MMA (0.75 moles)
2. temperatureNo temperature increase
3. additionwas observed during the addition
4. additionAfter addition
5. customThe unreacted MMA was then removed from the reaction mixture
6. customby venting to a collection vessel
7. customResidual MMA and methanol were removed from the product by reduced pressure distillation

ORD record

ord-7819466b0397402ea5a8d653369bbfcb

Source dataset

uspto-grants-1997_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05681907