反応 #699142

反応方程式

epichlorohydrin

methyl violet

Butoxytriglycol

1-chlorooctane

epichlorohydrin

→

BTG H2O

溶媒

toluene

water

acetic acid

toluene

acetic acid

反応条件

後処理

1. 1
   その他To a first 250 ml round bottom flask equipped with a stirrer, nitrogen inlet tube
2. 2
   workup.ADDITIONa distillation head were added 1 part of NP
3. 3
   その他To a second 250 ml round bottom flask equipped with a stirrer, nitrogen inlet tube
4. 4
   workup.ADDITIONa distillation head were added 1 part of NP
5. 5
   温度Both flasks were heated
6. 6
   workup.DISTILLATIONto azeotropically distill off the water
7. 7
   その他sparge
8. 8
   濃縮After the water concentration in each flask
9. 9
   workup.ADDITIONSodium methoxide was added to each flask in an amount that OH
10. 10
    温度Heat
11. 11
    workup.DISTILLATIONto distill off
12. 12
    その他formed methanol
13. 13
    workup.DISTILLATIONby distilling off half of the initial weight of toluene from the flask
14. 14
    温度In the first flask, the reaction mixture was then refluxed for 1 hour
15. 15
    温度The reaction mixture was then maintained at 70° C. for about 2 hours
16. 16
    温度the contents heated to 75-85° C. for 2 hours
17. 17
    workup.ADDITIONwas added such that the mole ratio of Cl
18. 18
    温度The reaction mixture was then refluxed until the alkalinity titration value

実験手順

To a first 250 ml round bottom flask equipped with a stirrer, nitrogen inlet tube, and a distillation head were added 1 part of NP--(EO)150 --OH (surfactant) and 2 parts of toluene. To a second 250 ml round bottom flask equipped with a stirrer, nitrogen inlet tube, and a distillation head were added 1 part of NP--(EO)50 --OH (surfactant) and 2 parts of toluene. Both flasks were heated to azeotropically distill off the water with stirring +N2 sparge. After the water concentration in each flask was less than 50 ppm the mixture was cooled to 55° C. Sodium methoxide was added to each flask in an amount that OH:NaOMe =1:1 based on the calculated hydroxyl value of surfactant. Heat was applied to distill off formed methanol by distilling off half of the initial weight of toluene from the flask. In the first flask, the reaction mixture was then refluxed for 1 hour. The flask was cooled to 60° C. after which 1.1 moles of epichlorohydrin were added per mole sodium alkoxide. The reaction mixture was then maintained at 70° C. for about 2 hours. When alkalinity by titration approached zero, the excess epichlorohydrin was vacuum stripped. A 4.0 gram aliquot of the reaction mixture +4 grams of tetraethylammonium bromide were dissolved in 50 ml of glacial acetic acid and the resulting solution titrated with a 0.1036 N HClO4 in glacial acetic acid solution to a methyl violet end point for the amount of epoxide (epoxy titration). The difference in the total alkalinity minus the HClO4 titration equals the amount of epoxide. The contents of the first and second flasks were mixed in a third flask such that the epoxy/alkoxide molar ratio was equal to 1:1 and the contents heated to 75-85° C. for 2 hours. When the epoxy titration value equaled zero, 1-chlorooctane was added such that the mole ratio of Cl:ONa was 1:1. The reaction mixture was then refluxed until the alkalinity titration value was zero. Butoxytriglycol (BTG) and water were added to give a clear yellow BTG/H2O/product ratio of 1:2:2 by weight.

出典