反応 #457565

反応方程式

adipic acid

isodecyl alcohol

→

diisodecyl adipate

反応条件

後処理

1. 1
   温度The mixture was heated
2. 2
   温度to reflux
3. 3
   その他removing water
4. 4
   その他as formed
5. 5
   温度After 30 minutes of reflux the temperature
6. 6
   その他was 215° C.
7. 7
   その他40 ml of water was collected, at which time 0.9 g of catalyst compound ATC-I
8. 8
   workup.ADDITIONwas added to the flask
9. 9
   その他After an additional 45 minutes the water of reaction
10. 10
    その他was collected
11. 11
    温度Heating
12. 12
    その他excess alcohol removed as the pressure
13. 13
    温度The reaction mixture was cooled to 170° C.
14. 14
    その他the remaining alcohol removed by steam distillation
15. 15
    その他during 2 hours
16. 16
    ろ過The residue was filtered with a No

実験手順

A standard 2-liter esterification apparatus was charged with 292 g adipic acid and 727 g isodecyl alcohol. The mixture was heated to reflux, removing water as formed. After 30 minutes of reflux the temperature was 215° C. and 40 ml of water was collected, at which time 0.9 g of catalyst compound ATC-I was added to the flask. The pressure was reduced as needed to maintain the reflux temperature at 220° C. After an additional 45 minutes the water of reaction was collected and the acid number of the residue was measured to be 0.01 mg KOH/g. Heating was discontinued and excess alcohol removed as the pressure was reduced to 20 torr. The reaction mixture was cooled to 170° C., the catalyst was hydrolyzed and the remaining alcohol removed by steam distillation using 100 ml water during 2 hours at 100 torr. The residue was filtered with a No. 1 Whatman paper coated with diatomaceous earth to yield a clear residue product diisodecyl adipate (DIDA) (nD25 =1.4502) having an acid number of 0.05 mg KOH/g and color of 15 APHA. The product remained clear after storage for six months at ambient temperature.

出典