Patent GB-801429-A (GB)
Title: Improvements in or relating to the production of polyethers
Inventor: STANLEY HERBERT MUGGLETON
IPC: C08G65/34
Filed: 1954-10-23
Abstract: The invention comprises an ungelled mixture of linear polyethers obtainable by heating metaor para-bis-(a -hydroxyethyl) benzene or mixtures thereof at an elevated temperature in the presence of a carboxylic acid catalyst having a dissociation constant greater than 6 X 10-4 and stopping the reaction before gelation of the reaction mixture occurs.  The reaction mixture is cooled and/or the acid catalyst is neutralized or removed by washing to stop the reaction. To a small extent some of the aromatic nuclei may be substituted in the ortho-position due to condensation between hydroxy groups and nuclear hydrogen atoms.  The products are substantially colourless liquids or fusible glass-like solids.  The polyethers may be esterified to provide plasticisers for vinylidene chloride polymers, i.e. polyvinylidene chloride and copolymers of vinylidene chloride with other copolymerizable monomers such as vinyl chloride.  In an example, para- and metal-bis-(a -hydroxyethyl) benzenes and anhydrous oxalic acid are heated under nitrogen whilst water is distilled off and the products are fractionated by precipitation from diethyl either solutions with n-heptane and in similar processes 1,4-bis-(a -hydroxyethyl) benzene is heated until gelation takes place in the presence of lactic, formic, citric, phthalic, chloracetic, cyanacetic, oxalic, di- and trichloracetic acids, substantially linear polyethers being stated to be formed on heating for less time than that required for gelation.  When acetic acid is employed no polyethers are formed.  Specification 801,430 is referred to.ALSO:The invention comprises an ungelled mixture of linear polyethers obtainable by heating meta- or para-bis-(a -hydroxyethyl) benzene or mixtures thereof at an elevated temperature in the presence of a carboxylic acid catalyst having a dissociation constant greater than 1 X 10-4 and stopping the reaction before gelation of the reaction mixture occurs.  The reaction mixture is cooled and (or the acid catalyst is neutralized or removed by washing to stop the reaction. To a small extent some of the aromatic nuclei may be substituted in the orthoposition due to condensation between hydroxy groups and nuclear hydrogen atoms.  The products are substantially colourless liquids or fusible glass-like solids.  The polyethers may be esterified to provide plasticizers for vinylidene chloride polymers, i.e. polyvinylidene chloride and copolymers of vinylidene chloride with other copolymerizable monomers such as vinyl chloride.  In an example para- and metabis-(a -hydroxyethyl) benzenes and anhydrous oxalic acid are heated under nitrogen whilst water is distilled off and the products are fractionated by precipitation from diethyl ether solutions with n-peptane and in similar processes 1,4-bis-(a -hydroxyethyl)-benzene is heated until gelation takes place in the presence of lactic, formic, citric, phthalic, chloracetic, cyanacetic, oxalic, di- and trichloracetic acids, substantially linear polyethers being stated to be formed on heating for less time than that required for gelation.  When acetic acid is employed no polyethers are formed.  Specification 801,430, [Group IV (a)], is referred to.