Reaktion #1745658

Reaktionsgleichung

tannic acid

sodium chloride

acrolein

Sodium chloride

→

divinylbenzene

Ausbeute 81.1%

diethyleneglycoldivinylether

Lösungsmittel

water

water

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONcontaining an efficient two-tiered stirrer, condenser, and nitrogen inlet tube
2. 2
   workup.ADDITIONThis solution is then added to the stirred flask
3. 3
   SonstigeThis aqueous phase is then sparged with nitrogen
4. 4
   Sonstigeof acrolein is sparged for 20 - 30 minutes with nitrogen
5. 5
   workup.ADDITIONadded to the aqueous phase in the reaction flask after the stirrer
6. 6
   Sonstigethe nitrogen sparge
7. 7
   SonstigeA suspension formed in 20 - 30 minutes on intermittent agitation at 145 rpm
8. 8
   SonstigeAfter the dispersion is formed
9. 9
   Temperaturwith intermittent heating
10. 10
    Temperaturair cooling for 16 hours
11. 11
    SonstigeThe reaction contents
12. 12
    Temperaturare then cooled to room temperature
13. 13
    WaschenAfter washing with methanol
14. 14
    Sonstigethe resin is dried at 75°C. for 16 hours

Vorschrift

Sodium chloride (116 g), 4 drops concentrated sulfuric acid and 150 g of water are added to a 1-liter flask containing an efficient two-tiered stirrer, condenser, and nitrogen inlet tube. Polyacrylic acid dispersant, such as 5 gm of Primafloc C-7 available from Rohm and Haas Company, is then added to a solution containing a 0.1 g tannic acid dissolved in 136 g of water. This solution is then added to the stirred flask containing sodium chloride. This aqueous phase is then sparged with nitrogen. In a separate flask, 314 mls. of acrolein is sparged for 20 - 30 minutes with nitrogen. In a separate flask a solution of 29.6 g of divinylbenzene (DVB-81.1% active), 6.0 g of diethyleneglycoldivinylether (DEGDVE), and 9.0 g of Percadox 16 (bis-t-butylcyclohexyl percarbonate) is prepared. This latter solution is then added to acrolein, shaken until homogeneous, and added to the aqueous phase in the reaction flask after the stirrer had been turned off and the nitrogen sparge had been converted to a nitrogen atmosphere. A suspension formed in 20 - 30 minutes on intermittent agitation at 145 rpm. The position of the stirrer blade must be at the interfaces of the two liquid phases. After the dispersion is formed, the reaction mixture is heated to 50°C. and held there with intermittent heating and air cooling for 16 hours. The reaction contents are then cooled to room temperature, the liquid drained, and the resin given three water washes. After washing with methanol, the resin is dried at 75°C. for 16 hours.

Quelle