Abstract: The efficient production of poly(tetramethylene ether) diacetate [PTMEA] or other diesters, from tetrahydrofuran [THF] is obtained utilizing an acid-based catalyst that is based on a morphologically reconfigured and Bronsted acidity enhanced halloysite derived from a preparation method of using naturally occurring halloysites. More specifically, the method relates to morphological modification of the internal pore structure of halloysites via supercritical carbon dioxide treatment directly applied onto the raw halloysite minerals, that yields highly synergistic and reproducible results of elimination of inaccessible and detrimental extra-small pores.
Type:
Grant
Filed:
March 1, 2018
Date of Patent:
December 18, 2018
Assignee:
KOREA PTG CO., LTD.
Inventors:
Hyung Ju Kim, Hwan Bock Lee, Jung Keun Lee
Abstract: The efficient production of poly(tetramethylene ether) diacetate [PTMEA] or other diesters, from tetrahydrofuran [THF] is obtained utilizing an acid-based catalyst that is based on a morphologically reconfigured and Bronsted acidity enhanced halloysite derived from a preparation method of using naturally occurring halloysites. More specifically, the method relates to morphological modification of the internal pore structure of halloysites via supercritical carbon dioxide treatment directly applied onto the raw halloysite minerals, that yields highly synergistic and reproducible results of elimination of inaccessible and detrimental extra-small pores. PTMEA is readily converted to poly(tetramethylene ether) glycol (PTMEG) by a transesterification reaction.
Type:
Grant
Filed:
March 1, 2018
Date of Patent:
December 11, 2018
Assignee:
KOREA PTG CO., LTD
Inventors:
Hyung Ju Kim, Hwan Bock Lee, Jung Keun Lee
Abstract: The efficient production of poly(tetramethylene ether) diacetate [PTMEA] or other diesters, from tetrahydrofuran [THF] is obtained utilizing an acid-based catalyst that is based on a morphologically reconfigured and Bronsted acidity enhanced halloysite derived from a preparation method of using naturally occurring halloysites. More specifically, the method relates to morphological modification of the internal pore structure of halloysites via supercritical carbon dioxide treatment directly applied onto the raw halloysite minerals, that yields highly synergistic and reproducible results of elimination of inaccessible and detrimental extra-small pores. PTMEA is readily converted to poly(tetramethylene ether) glycol (PTMEG) by a transesterification reaction.
Type:
Grant
Filed:
April 4, 2017
Date of Patent:
May 29, 2018
Assignee:
KOREA PTG CO., LTD
Inventors:
Hyung Ju Kim, Hwan Bock Lee, Jung Keun Lee
Abstract: An improved process for the preparation of polytetramethylene ether glycol diesters of the formula
R—CO—O(—CH2-CH2-CH2-CH2-O)n-COR1
in which R and R1 are identical or different and are an alkyl radical or a derivative thereof, by polymerization of tetrahydrofuran in the presence of a fixed-bed polymerization catalyst and a carboxylic acid anhydride.
Through use of neutral or weakly basic magnesium-aluminium hydrosilicates instead of the known acidic montmorillonite, zeolite or kaolin catalysts, polymers with more uniform properties and a narrower molecular weight distribution are obtained at a higher rate of polymerization, even when technical-grade tetrahydrofuran is used.
Abstract: An improved process for Polytetramethylene-Ether-Glycol-Diesters of the formula R—CO—O(CH2—CH2—CH2—CH2—O)n-COR1, in which R and R1 are identical or different and are alkyl radicals or derivatives thereof, by polymerization of tetrahydrofuran in the presence of a heterogeneous polymerization catalyst and in the presence of a carboxylic anhydride. The use of aluminum silicate catalyst composed of acid-activated and calcinated natural halloysite instead of the known catalytic silicates as bentonite, zeolite or kaolinite. The new catalyst with a very long lifetime produces polymers having more uniform properties and narrow molecular weight distribution even with a relative impure monomer.