反应 #56347

ord-3c30bea125f6436ead167a3c70ae52bc

反应方程式

C=C
ethylene
C=CC(=O)OC
methyl acrylate
CCOC(=O)/C=C\C(=O)[O-]
monoethyl maleate
CC(C)(C)OOC(=O)C(C)(C)C
tert-butyl peroxypivalate
C=C
ethylene
C=C.C=CC(=O)OC.CCOC(=O)/C=C\C(=O)[O-]
ethylene/methyl acrylate monoethyl maleate

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONby adding 50 ml
  2. 2
    其他at 170° C
  3. 3
    其他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

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04225476uspto-grants-1980_09