Reaktion #58677

ord-63640d58b96546409d29e4cc79283a53

Reaktionsgleichung

Cl
hydrogen chloride
Cl
HCl
C[CH2][Al+2].[Cl-].[Cl-]
ethylaluminum dichloride
C[CH2][Al+2].[Cl-].[Cl-]
ethylaluminum dichloride
C[CH2][Al+2].[Cl-].[Cl-]
ethylaluminum dichloride
C[CH2][Al+2].[Cl-].[Cl-]
ethylaluminum dichloride
Cl
hydrogen chloride
Cl
HCl
C[CH2][Al+2].[Cl-].[Cl-]
ethylaluminum dichloride
C[CH2][Al+2].[Cl-].[Cl-]
EADC
Cl
HCl
C=C(Cl)Cl
1,1-dichloroethene

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigePolymerizations were terminated with the addition of 0.2 ml of methanol
  2. 2
    SonstigePolymerization in 3,3,3-trifluoropropene
  3. 3
    Sonstigeresulted in rubber particles that
  4. 4
    Sonstigetested near reaction temperature
  5. 5
    Sonstigeresulted in rubber particles that

Vorschrift

Polymerizations were run by the dropwise addition of this stock of ethylaluminum dichloride (EADC)/hydrogen chloride (HCl) solution to the stirred monomer solutions. A stock solution of EADC and HCl was prepared in methyl chloride by adding 0.320 ml of a 1.0 mol/L HCl solution in 1,1,1,2-tetrafluoroethane and 0.960 ml of a 1.0 mol/L ethylaluminum dichloride solution in hexane to 100 ml of methyl chloride. The total volume of the stock solution added to the polymerization for each example is listed in Table 15. A separate stock solution of ethylaluminum dichloride and hydrogen chloride was used for Examples 125 and 126. This solution was prepared from the addition of 2.0 ml of a 0.16 mol/L HCl solution in 1,1,1,2-tetrafluoroethane and 0.960 ml of a 1.0 mol/L ethylaluminum dichloride solution in hexane to 100 ml of methyl chloride. The final mol/L concentrations of ethylaluminum dichloride and hydrogen chloride in the stock solution is the same for both preparations. Polymerizations were terminated with the addition of 0.2 ml of methanol. Polymerization in 3,3,3-trifluoropropene resulted in rubber particles that did not adhere to the walls of the reactor or to the stirring bar. The particles floated to the surface of the liquid when stirring stopped. The particles were hard as evidenced by pressing on them with a chilled spatula when tested near reaction temperature. Polymerization in methyl chloride resulted in rubber particles that adhered to both the reactor walls and the stirring shaft. Polymerization in 1,1-dichloroethane or 1,1-dichloroethene resulted in solvent swollen polymer particles that adhered to the reactor walls and the stirring bar.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07423100B2uspto-grants-2008_09