Reaktion #1370079

ord-f657ab863d4744e585bef9bc2f919ab1

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONby adding 50 ml
  2. 2
    Sonstigeat 170°C
  3. 3
    SonstigeThe effluent from the autoclave passed through a let-down valve to a chamber at atmospheric pressure where most of the residual monomers and solvent

Vorschrift

A mixture of methyl acrylate, monoethyl maleate, and benzene (weight ratio: 68.28/2.46/29.26) was pressured to about 422 kg./sq. cm.; ethylene was separately pressured to about 422 kg./sq. cm. Separate streams of this mixture (0.91 kg./hr.) and ethylene (6.35 kg./hr.) were joined and pressured to 1900 kg./sq. cm. The resulting feed stream then entered the autoclave. Simultaneously, a catalyst solution, made by adding 50 ml. of tert-butyl peroxypivalate to 4.5 kg. of benzene was introduced at the rate of 0.00204 kg./hr. to keep the temperature at 170°C. The effluent from the autoclave passed through a let-down valve to a chamber at atmospheric pressure where most of the residual monomers and solvent flashed off. The ethylene/methyl acrylate/monoethyl maleate terpolymer thus isolated was freed from the small amount of residual volatiles by heating for 16 hours at 80°C. in a nitrogen stream. Acid-base titration indicated that 0.25 meq. of acid groups was present per gram of terpolymer. This corresponds to 3.6 weight percent of monoethyl ester of maleic acid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US03972961uspto-grants-1976_08