[미국특허]
High molecular weight poly(2,6-dimethyl-1,4-phenylene ether) and process therefor
원문보기
IPC분류정보
국가/구분
United States(US) Patent
등록
국제특허분류(IPC7판)
B01D-069/04
C08G-061/02
C08K-003/08
출원번호
US-0205117
(2011-08-08)
등록번호
US-8215495
(2012-07-10)
발명자
/ 주소
Delsman, Erik Rene
Schoenmakers, Gert-Jan
출원인 / 주소
Sabic Innovative Plastics IP B.V.
대리인 / 주소
Cantor Colburn LLP
인용정보
피인용 횟수 :
0인용 특허 :
16
초록▼
A poly(2,6-dimethyl-1,4-phenylene ether) having a high molecular weight and a reduced content of low molecular weight species can be prepared by a method that includes specific conditions for the oxidative polymerization, chelation, and isolation steps. The poly(2,6-dimethyl-1,4-phenylene ether) is
A poly(2,6-dimethyl-1,4-phenylene ether) having a high molecular weight and a reduced content of low molecular weight species can be prepared by a method that includes specific conditions for the oxidative polymerization, chelation, and isolation steps. The poly(2,6-dimethyl-1,4-phenylene ether) is particularly useful for the fabrication of fluid separation membranes.
대표청구항▼
1. A poly(2,6-dimethyl-1,4-phenylene ether) made by a method comprising oxidatively polymerizing 2,6-dimethylphenol in toluene solvent in the presence of a catalyst comprising copper ion, N,N′-di-tert-butylethylenediamine, dimethyl-n-butylamine, and di-n-butylamine to form a reaction mixture compris
1. A poly(2,6-dimethyl-1,4-phenylene ether) made by a method comprising oxidatively polymerizing 2,6-dimethylphenol in toluene solvent in the presence of a catalyst comprising copper ion, N,N′-di-tert-butylethylenediamine, dimethyl-n-butylamine, and di-n-butylamine to form a reaction mixture comprising a dissolved poly(2,6-dimethyl-1,4-phenylene ether), water, and the catalyst; wherein the oxidative polymerizing comprises initiating oxidative polymerization in the presence of 1 to 3 weight percent of the 2,6-dimethylphenol;wherein at least 97 weight percent of the 2,6-dimethylphenol is added to the reaction mixture after the initiation of oxidative polymerization and over the course of 55 to 65 minutes;wherein the oxidatively polymerizing comprises adding molecular oxygen and 2,6-dimethylphenol to the reaction mixture in a mole ratio of 0.3:1 to 0.5:1;wherein the oxidatively polymerizing 2,6-dimethylphenol comprises a first stage in which the reaction mixture is cooled to maintain a temperature of 20 to 30° C., and a second stage in which the reaction mixture is heated to maintain a temperature of 30 to 40° C.;terminating the oxidative polymerization to form a post-termination reaction mixture;combining a chelant comprising an alkali metal salt of nitrilotriacetic acid with the post-termination reaction mixture to form a chelation mixture comprising an aqueous phase comprising chelated copper ion, andan organic phase comprising the dissolved poly(2,6-dimethyl-1,4-phenylene ether); wherein the chelation mixture excludes dihydric phenols and aromatic amines; maintaining the chelation mixture at a temperature of 45 to 55° C. for 40 to 70 minutes;separating the aqueous phase and the organic phase; wherein the separation is conducted at a temperature of 45 to 55° C.;isolating the poly(2,6-dimethyl-1,4-phenylene ether) from the separated organic phase;wherein time elapsed between termination of the oxidative polymerization and isolating the poly(2,6-dimethyl-1,4-phenylene ether) is 30 to 60 minutes;wherein the method excludes a solvent removal step between the terminating the oxidative polymerization and the isolating the poly(2,6-dimethyl-1,4-phenylene ether);wherein the isolated poly(2,6-dimethyl-1,4-phenylene ether) has a number average molecular weight of 20,000 to 35,000 atomic mass units and 16 to 20 weight percent of molecules having a molecular weight less than 30,000 atomic mass units; andwherein the isolated poly(2,6-dimethyl-1,4-phenylene ether) has a copper concentration of 0.5 to 5 parts per million by weight. 2. A fiber comprising the poly(2,6-dimethyl-1,4-phenylene ether) of claim 1. 3. An article comprising the poly(2,6-dimethyl-1,4-phenylene ether) of claim 1.
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이 특허에 인용된 특허 (16)
Malon Raymond F. (Edmundson MO) Zampini Anthony (St. Louis MO), Asymmetric gas separation membranes.
Moll David J. (Midland MI) Burmester Alan F. (Midland MI) Young Thomas C. (Walnut Creek CA) McReynolds Kent B. (Midland MI) Clark James E. (Midland MI) Hotz Charles Z. (Walnut Creek CA) Wessling Ritc, Gas separations utilizing glassy polymer membranes at sub-ambient temperatures.
Kramer Paul W. (Ellisville MO) Murphy Milton K. (Clayton MO) Stookey Donald J. (Creve Coeur MO) Henis Jay M. S. (St. Louis MO) Stedronsky Erwin R. (Richmond Heights MO), Membranes having enhanced selectivity and method of producing such membranes.
Cooper Glenn Dale (Delmar NY) Floryan Daniel Edwin (Glenmont NY), Removal of catalyst from polyphenylene oxide reaction mixtures with nitrogenous salts of nitrilotriacetic acid.
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