反应详情

温度

255 °C

A mixture of 213 gms. (0.715 moles) of STANDAMUL G from Henkel Co. (Octyldodecanol) and 15 mgms. Sodium borohydride was stirred at room temperature 25° C. under nitrogen. The mixture was then heated and brought to 60° C. and held at 60° C. for 1/2 hour. To this mixture was added 86.40 gms. (0.68 moles) Benzoic Acid and 450 mgms. of stannous oxalate. The reaction mixture was then further heated to 255° C. During the heat-up cycle, distillate was collected, particularly when the reaction mixture reached a temperature of 170° C. and higher. The reaction was rapidly heated from 60° C. to 177° C. over 45 minutes, and then from 177° C. to 228° C. over the next 60 minutes while still collecting the distillate. Further heating was continued to bring the temperature to 255° C. over the next 30 minutes. The distillate collected contained 7.5 gms. of water and also contained some benzoic acid trapped during the collection of distillate. The reaction was then cooled. The yield at this stage was 265 gm. and acidity was at 9.5 mgms. The KOH/gm. hydroxyl value of this mixture was 19.29. 220 gms. of this ester was treated with 2.2 gms. sodium carbonate, 1.1 gm. sodium chloride, 2.0 gms. Hydrogen peroxide in 35 gms. deionized water. The mixture was stirred and heated to 85°-90° C., held at 85°-90° C. for 30 minutes and allowed to stand for separation of the ester and water phases. The ester phase was separated and further washed with deionized water until reaction of the water was neutral. The ester collected was 200 gms. and was hydrous. The product was vacuum stripped to remove the residual moisture, and then filtered using filter-aids. The final product was a clear liquid and had the following formula: ##STR11##

1. additionA mixture of 213 gms
2. temperatureThe mixture was then heated
3. custombrought to 60° C.
4. additionTo this mixture was added 86.40 gms
5. distillationDuring the heat-up cycle, distillate was collected
6. customa temperature of 170° C.
7. temperatureThe reaction was rapidly heated from 60° C. to 177° C. over 45 minutes
8. distillationfrom 177° C. to 228° C. over the next 60 minutes while still collecting the distillate
9. temperatureFurther heating
10. customto 255° C.
11. customover the next 30 minutes
12. distillationThe distillate collected
13. distillationtrapped during the collection of distillate
14. temperatureThe reaction was then cooled
15. customThe yield at this stage
16. temperatureheated to 85°-90° C.
17. waitheld at 85°-90° C. for 30 minutes
18. customto stand for separation of the ester and water phases
19. customThe ester phase was separated
20. washfurther washed with deionized water until reaction of the water
21. customThe ester collected
22. customto remove the residual moisture
23. filtrationfiltered
24. filtrationusing filter-aids