公开(公告)号：DE1103320B

公开(公告)日：1961-03-30

申请号：DEST013818

申请日：1958-05-30

Applicant: STANDARD OIL CO

Inventor： CORCORAN JAMES TIMOTHY ,  PETERSON KENNETH CARL

IPC: C07C69/82

Abstract: Dimethyl terephthalate having an acid number less than 0.05 and a melting point of 140.62 \sB 0.02 DEG C. is prepared by purifying crude dimethyl terephthalate partly by distillation and partly by methanol treatment, where the distillation may precede or follow the methanol treatment and where the methanol treatment comprises slurrying the crude ester with 1 to 10 parts by weight of methanol per part of crude ester, agitating the slurry for such a time that the acid number of the solid ester is substantially reduced and recovering solid dimethyl terephthalate of reduced acid number from the slurry. When the methanol treatment is carried out before distillation preferably 2 to 6 parts of methanol are used per part of ester at a temperature of 10 DEG to 60 DEG C. The solid ester is then separated from the slurry, freed from adhering methanol and distilled in a known manner. The forerun and residue from the distillation may be recycled to the methanol treatment. The crude ester purified in this manner generally has an original acid number of 0.1 to 50. When the acid number is below 25 the crude ester may first be distilled in a known manner to give a purified fraction of ester and a less-pure fraction which is then subjected to the slurrying treatment with methanol, preferably at 50 DEG -60 DEG C. The purified ester from the slurrying treatment may be blended with the purified fraction from the distillation. In the Examples (1) an ester of acid number 20 is slurried with 3 lbs. of methanol per lb. of ester for 30 minutes at 25 DEG C., the solid ester separated and distilled, (2) an ester of acid number 8 is distilled to give 65% recovery of pure ester, the less-pure ester is slurried with 3 parts of methanol at 60 DEG C. for 15 minutes and an ester of acid number 0.02 recovered.

公开(公告)号：GB942749A

公开(公告)日：1963-11-27

申请号：GB4327059

申请日：1959-12-21

Applicant: STANDARD OIL CO

Inventor： COOPERSMITH JOHN MAYER ,  PETERSON KENNETH CARL ,  SUTTON MACK

IPC: C08F10/00

Abstract: A cyclic process for polymerizing an olefin comprises passing the olefin through a cooling zone and then into a reaction zone, introducing catalyst at the inlet of the reaction zone, diluting a major portion of the reaction zone effluent with incoming olefin charge comprising fresh charge and recycled unreacted olefin in an amount sufficient to stop the reaction, recycling the thus diluted portion of the reaction zone effluent through the cooling zone and reaction zone, withdrawing the residual minor portion of the reaction zone effluent for product recovery and recycling unreacted olefin from said residual minor portion to the incoming olefin charge. Catalyst in the withdrawn stream may be converted to an adduct (e.g. by the use of NH3) which is then removed prior to the addition of an oil to form a solution of polymer in lubricating oil. The process is applicable to the polymerization of propylene, alpha-methyl styrene, butene and butene/isobutene mixture, but is advantageously applied to the polymerization of isobutylene using BF3 as catalyst. Up to 20% of closely boiling hydrocarbons also may be present. The invention is illustrated by reference to a suitable apparatus.