公开(公告)号：US3029216A

公开(公告)日：1962-04-10

申请号：US75414658

申请日：1958-08-11

申请人： UNION CARBIDE CORP

发明人： BAILEY JR FREDERICK E ,  FRANCE HAYWOOD G

IPC分类号： C08F4/00 ,  C08G65/08 ,  C08G65/12

CPC分类号： C08G65/12 ,  C08G65/08

公开(公告)号：US2870100A

公开(公告)日：1959-01-20

申请号：US56315656

申请日：1956-02-02

申请人： SHELL DEV

发明人： STEWART DAVID G ,  WADDAN DHAFIR Y ,  BORROWS EDWARD T

IPC分类号： C07D319/12 ,  C08G65/08 ,  C08G65/10 ,  C08G65/12

CPC分类号： C07D319/12 ,  C08G65/08 ,  C08G65/10 ,  C08G65/12

摘要： Alkylene oxide polymers of high molecular weight suitable for use as thickening agents and for processing into thin water-soluble films are obtained by reacting an alkylene oxide, particularly ethylene and propylene oxide, in presence of a catalyst of formula MeRR1x, where Me is a metal of the II or III Groups of the Periodic System, particularly Mg, Al, or Zn, R is a hydrocarbon radical and R1x are x members selected from hydrogen, halogens, hydrocarbon radicals, alkoxy radicals and secondary amino radicals and x is the valency of the metal Me minus one. Examples of the catalysts are triethyl aluminium, tri-isobutyl aluminium, trioctyl aluminium, di - isobutyl aluminium hydride, diethyl aluminium ethoxide, diethyl aluminium chloride, ethyl aluminium dibutoxide, diethyl piperidyl aluminium and similar magnesium and zinc compounds. During the polymerization dioxane and the tetramer of ethylene oxide are formed and can be separated by fractionation. Reaction temperatures of 0-200 DEG C. and pressures up to 40 atmospheres are employed. The polymerization may be carried out in presence of solvents, e.g. aliphatic aromatic and chlorinated hydrocarbons or ethers. In examples: (1) gaseous ethylene oxide is passed into a solution of triethyl aluminium in benzene, the mixture being cooled and maintained at 0 DEG C. for five days; excess ethylene oxide was distilled off and the polymer precipitated by addition of petroleum ether; (6) liquid ethylene oxide in benzene and diethyl magnesium were heated at 110 DEG C. for 65 hours; (10) 1,2-propylene oxide in hexane was added dropwise to a solution of triethyl aluminium in hexane; (18) liquid ethylene oxide was added to a solution of tri-iso-butyl aluminium in benzene and heated in an autoclave at 100 DEG C. The product was diluted with benzene, unreacted oxide distilled off and the solution added to petroleum ether to precipitate the polymer. Dioxane was distilled from the filtrate and the residue was distilled to recover the cyclic tetramer.ALSO:The invention comprises the cyclic tetramer of ethylene oxide which is obtained along with dioxane and higher polymers by polymerizing ethylene oxide in presence of catalysts of formula MeR.R1x where Me is a metal of Group II or III, R is an hydrocarbon radical and R1x and x members selected from hydrogen, halogens, hydrocarbon radicals, alkoxy radicals and secondary amino radicals, and x is the valency of the metal Me minus one. Examples of the catalysts are triethyl aluminium, tri-isobutyl aluminium, trioctyl aluminium, di-isobutyl aluminium hydride, diethyl aluminium ethoxide, diethyl aluminium chloride, ethyl aluminium dibutoxide, diethyl piperidyl aluminium, diethyl zinc, ethyl zinc butoxide, diethyl magnesium. Reaction temperatures from 0-200 DEG C. and pressures up to 40 atmospheres may be employed. The alkylene oxide, viz. ethylene oxide, is preferably added to a solution of the catalyst in benzene or diethyl ether. The resulting polymeric material may be treated to remove catalyst therefrom by precipitating the metal (Me) as hydroxide or by extracting the metal as a water-soluble salt by treatment with aqueous acid. The remaining polymeric material is preferably separated into a lower molecular weight and a higher molecular weight polymer fraction (comprising dioxane and mainly non-cyclic polymer), or the cyclic tetramer of ethylene oxide being recovered from the lower molecular weight polymer fraction.

公开(公告)号：US11718705B2

公开(公告)日：2023-08-08

申请号：US17386844

申请日：2021-07-28

申请人： Covestro LLC

发明人： Sharlene A. Lewis ,  Jack R. Reese

IPC分类号： C08G18/16 ,  C08G18/18 ,  C08G18/20 ,  C08G18/24 ,  C08G18/28 ,  C08G18/48 ,  C08G18/76 ,  C08G65/12 ,  C08G65/26 ,  C08J9/12 ,  C08L71/02

CPC分类号： C08G18/485 ,  C08G18/7621 ,  C08G18/7671 ,  C08G65/12 ,  C08J9/125 ,  C08G2110/0083 ,  C08J2203/10 ,  C08J2375/08

摘要： This invention relates to an in-situ formed polyether polyol blend having an overall functionality of 2 to 3 and an overall hydroxyl number of 40 to 220 mg KOH/g. A process for preparing these in-situ formed polyether polyol blends is also disclosed. These in-situ formed polyether polyol blends are suitable for a process of preparing viscoelastic flexible polyurethane foams.

公开(公告)号：US20230082443A1

公开(公告)日：2023-03-16

申请号：US17944371

申请日：2022-09-14

申请人： SUMITOMO SEIKA CHEMICALS CO., LTD.

发明人： Yuika IMAMURA ,  Akira KIMURA

IPC分类号： C08G65/12 ,  C08K5/05 ,  C08J3/28

摘要： The present invention provides a production method for obtaining, by a simple method, a polyalkylene oxide whose molecular weight and polydispersity are controlled in the desired range.
The method for producing a polyalkylene oxide of the present disclosure comprises step 1 of performing a polymerization reaction of an alkylene oxide in the presence or absence of a chain transfer agent to obtain a high-molecular-weight polyalkylene oxide; and step 2 of irradiating the high-molecular-weight polyalkylene oxide obtained in step 1 with radiation to obtain a polyalkylene oxide; wherein the amount of the chain transfer agent when used is less than 300 mass ppm relative to the alkylene oxide, and the high-molecular-weight polyalkylene oxide has a viscosity in a 1 mass % aqueous solution of 7500 mPa·s or more.

公开(公告)号：US10961347B2

公开(公告)日：2021-03-30

申请号：US16225549

申请日：2018-12-19

申请人： COVESTRO LLC

发明人： Edward P. Browne ,  Anthony R. Loveday ,  Jose F. Pazos

IPC分类号： C08G65/12 ,  C08G65/26

摘要： This invention relates to an improved process for the preparation of a high molecular weight polyoxyalkylene polyether polyol by the continuous addition of starter (CAOS) process. This process enables a shorter cycle time while maintaining a low viscosity in high molecular weight polyoxyalkylene polyether polyols.

公开(公告)号：US10738155B2

公开(公告)日：2020-08-11

申请号：US16582149

申请日：2019-09-25

申请人： Covestro LLC ,  Covestro Deutschland AG

发明人： Jack R. Reese ,  Edward P. Browne ,  Yue Yang ,  Jose F. Pazos

IPC分类号： C08G65/12

摘要： This invention relates to process for preparing low viscosity polyoxyalkylene polyols (P) that have a narrow molecular weight distribution. This process comprises reacting a H-functional starter substance (Si), a H-functional starter substance (Sx) and a H-functional starter substance (Sc) with one or more alkylene oxides in the presence of a double metal cyanide catalyst. The resultant polyoxyalkylene polyols (P) have a functionality of 2 to 8 and a hydroxyl number of greater than 35 to 115 mg KOH/g polyol.

公开(公告)号：US10479863B2

公开(公告)日：2019-11-19

申请号：US15513972

申请日：2016-03-30

申请人： Huaian Bud Polyurethane Science & Technology Co., Ltd.

发明人： Weixin Qi ,  Bing Hu ,  Yong Han

IPC分类号： C08G65/26 ,  C08G65/02 ,  C08G65/12

摘要： A method for preparing a polyether polyol in a continuous reaction cycle is described. In the method, a low molecular-weight alcohol is polymerized with an alkylene oxide to obtain a low molecular-weight polymer. The low molecular-weight polymer is used as an initiator to react with the alkylene oxide and the low molecular-weight alcohol in the presence of a DMC catalyst and an acid promoter to obtain an intermediate-target polymer. A portion of the intermediate-target polymer is used for producing the target polymer, and the other portion is recycled for reproduction of the intermediate-target polymer. No initiator prepared with a base catalyst is used, and thus the loss of material and the discharge of residue and waste water are reduced. The DMC concentration is kept constant in the target polymer during the production such that the dewatering time and induction time are greatly reduced.

公开(公告)号：US20190315916A1

公开(公告)日：2019-10-17

申请号：US16472130

申请日：2017-12-11

申请人： UNIVERSITÉ DE LIÈGE

发明人： Jean-Christophe MONBALIU ,  Morgan HANS

IPC分类号： C08G65/12

摘要： A continuous-flow process for the polymerization of an alkylene oxide is provided that includes: (a) Mixing an alkylene oxide (1) with a monomer solvent (12), to form a monomer solution (121); wherein the monomer solvent is a polar aprotic solvent (b) Forming a reaction mixture (3) by mixing the monomer solution with an anionic initiator (2) selected among the alkali or alkaline-earth alkoxides of general formula R-O-M, wherein, R is a straight, branched or cyclic alkyl chain, a heterocycle, a glycol or a combination of two or several of these, O is oxygen, and M is or includes at least an alkali, an alkaline-earth metal or salt thereof; (c) Allowing the reaction mixture to react, thus forming a polymerized solution (5); and (d) Separating the solvent (5s).

公开(公告)号：US10377775B2

公开(公告)日：2019-08-13

申请号：US14959088

申请日：2015-12-04

申请人： Shin-Etsu Chemical Co., Ltd.

发明人： Yuki Suka ,  Yuji Harada ,  Takeru Watanabe ,  Shiori Nonaka

IPC分类号： C07F7/10 ,  C07F7/08 ,  C08G65/12 ,  C08G65/26 ,  C08G65/333

摘要： A method simply produces a narrowly distributed and high-purity polyalkylene glycol derivative having an amino group at an end without using a heavy metal catalyst. A method for producing a polyalkylene glycol derivative having an amino group at the end by reacting a compound represented by the general formula (V) with an alkylene oxide, then reacting a reaction product with an electrophile represented by the general formula (I), and deprotecting the obtained product without using a heavy metal: RA3O(RA4O)k-1RA4O−M+  (V) wherein RA3 represents a linear, branched, or cyclic hydrocarbon group having 1 to 20 carbon atoms; RA4 represents an alkylene group having 2 to 8 carbon atoms; k represents an integer of 2 to 5; and M represents an alkali metal; wherein RA1a and RA1b each independently represent a protective group of the amino group, or one of RA1a and RA1b represents H and the other represents a protective group of the amino group, or RA1a and RA1b bind to each other to form a cyclic protective group, and the protective group is deprotectable without using a heavy metal; RA2 represents a linear, branched, or cyclic hydrocarbon group having 1 to 6 carbon atoms; and X represents a leaving group.

公开(公告)号：US10329382B2

公开(公告)日：2019-06-25

申请号：US16036580

申请日：2018-07-16

申请人： Sumitomo Seika Chemicals Co., Ltd.

发明人： Toru Ido ,  Noboru Yamaguchi

IPC分类号： C08G65/10 ,  C08G65/12 ,  C08G65/26

摘要： Provided is a method to produce an alkylene oxide polymer having a high polymerization degree on an industrial scale and with high reproducibility. The method includes the step of carrying out a polymerization reaction of an alkylene oxide in an inert hydrocarbon solvent in the presence of a zinc catalyst to produce an alkylene oxide polymer. The zinc catalyst is produced by reaction of an organozinc compound with a monohydric alcohol in an amount of 12-fold equivalent or less relative to the amount of the organozinc compound and an aliphatic polyhydric alcohol in an amount of 0.2- to 1.1-fold equivalent relative to the amount of the organozinc compound. The polymerization reaction is carried out under such a condition that the amount of the monohydric alcohol in the polymerization reaction system becomes 0.01-fold equivalent or less relative to the amount of the organozinc compound.