Process for preparing polyether carbonate polyols

Patent metadata

Field	Value
Publication number	US-2016194441-A1
Application number	US-201414911669-A
Country	US
Kind code	A1
Filing date	Aug 11, 2014
Priority date	Aug 12, 2013
Publication date	Jul 7, 2016
Grant date	—

Abstract

The present invention relates to a process for the preparation of polyether carbonate polyols in the presence of a double metal cyanide catalysts that can be obtained by a process comprising (a) synthesizing a solid double metal cyanide catalyst in the presence of an organic complexing agent and a polyether polyol ligand; and (b) first washing the catalyst obtained in step a) with an aqueous solution comprising 90-100% by weight of water and 0-10% by weight of a polyether polyol ligand, to form a slurry, wherein the aqueous solution does not contain any organic complexing agent other than the polyether polyol ligand.

First claim

1 . A process for the preparation of polyether carbonate polyols comprising copolymerizing one or more H-functional initiator substances, one or more alkylene oxides and carbon dioxide in the presence of a double metal cyanide catalyst, wherein the double metal cyanide catalyst is obtainable by a process comprising:
(a) synthesizing a solid double metal cyanide catalyst in the presence of an organic complexing agent and a polyether polyol ligand; and (b) first washing the catalyst obtained in step a) with an aqueous solution comprising:
90-100% by weight of water; and
0-10% by weight of a polyether polyol ligand,
to form a slurry, wherein the aqueous solution does not contain any organic complexing agent other than the polyether polyol ligand.

2 . The process according to claim 1 , which further comprises:
(c) isolating the catalyst from the slurry obtained in step b); and (d) washing the solid catalyst obtained in step c) with a solution comprising:
90-100% by weight of an organic complexing agent; and
0-10% by weight of a polyether polyol,
to form a slurry.

3 . The process according to claim 1 , wherein the amount of polyether polyol ligand in the aqueous solution in step b) is between 0.05% and 10% with respect to the total weight of solution, preferably between 0.1% and 2%.

4 . The process according to claim 1 , wherein the catalyst obtained in step a) is first brought into contact with water and then brought into contact with the polyether polyol ligand which is preferably in a 0.1 to 5% by weight with respect to the total weight of solution.

5 . The process according to claim 1 , wherein the polyether polyol ligand has a number average molecular weight lower than 2000 Da.

6 . The process according to claim 1 , wherein the polyether polyol is a poly(oxypropylene) polyol.

7 . The process according to claim 1 , wherein the organic complexing agent is selected from monoalcohols, aldehydes, ketones, ethers, esters, amides, ureas, nitriles, sulfides and mixtures thereof, preferably it is a monoalcohol.

8 . The process according to claim 1 , wherein the alkylene oxide is selected from ethylene oxide, propylene oxide, butene oxides, pentene oxides, hexene oxides, heptene oxides, octene oxides, nonene oxides, decene oxide, undecene oxides, dodecene oxides, cyclopentene oxide, cyclohexane oxide, cycloheptene oxide, cyclooctene oxide and styrene oxide optionally substituted with a C 1 -C 6 alkyl group.

9 . The process according to claim 1 , wherein the H-functional initiator substance is a polyether polyol.

10 . The process according to claim 1 , wherein the H-functional initiator substance is a polyether polyol obtained by acidic catalysis.

11 . The process according to claim 1 , wherein at least one activation step of the DMC catalyst is performed before the copolymerization reaction.

12 . The process according to claim 11 , wherein two, three or four activation steps are performed and only the last activation step is performed in the presence of carbon dioxide.

13 . The process according to claim 1 , which comprises the following steps:
(i) the one or more H-functional initiator substances is placed in a vessel and heating and/or vacuum is applied (“drying”), wherein the DMC catalyst is added to the one or more H-functional initiator substances before or after the drying; (ii) for activation
(ii-1) in a first activation step, a first partial amount of alkylene oxide (based on the total amount of alkylene oxide used in the process of the invention) is added to the mixture resulting from step (i), in the presence of CO 2 or preferably in the absence of CO 2 ,
(ii-2) in a second activation step, after the activation in the preceding step has been observed, a second partial amount of alkylene oxide (based on the total amount of alkylene oxide used in the process of the invention) is added to the mixture resulting from the preceding step, in the presence or in the absence of CO 2 ,
(ii-3) optionally in a third activation step, after the activation in the preceding step has been observed, a third partial amount of alkylene oxide (based on the total amount of alkylene oxide used in the process of the invention) is added to the mixture resulting from the preceding step, in the presence or in the absence of CO 2 ,
(ii-4) optionally in a further activation step, after the activation in the preceding step has been observed, a fourth partial amount of alkylene oxide (based on the total amount of alkylene oxide used in the process of the invention) is added to the mixture resulting from the preceding step in the presence of CO 2 ;
(iii) the rest of alkylene oxide and carbon dioxide are metered continuously into the mixture from step (ii) (“copolimerization”).

14 . The process according to claim 13 , wherein the partial amount of alkylene oxide used in the activation steps is in each step from 1.0 to 15.0 wt. %, based on the total amount of alkylene oxide used in the process.

15 . A polyether carbonate polyol obtainable by a process as defined in claim 1 .

16 . Use of a polyether carbonate polyol as defined in claim 15 for the manufacture of polyurethane.

Assignees

• Repsol Sa

Inventors

• BLANCO GONZÁLEZ María Dolores
• García Ruiz Mónica
• González Rivero Julián Pedro

Classifications

• C08G65/2663

  Metal cyanide catalysts, i.e. DMC's · CPC title

• C08G65/2603

  the other compounds containing oxygen · CPC title

• C08G64/34 Primary

  and cyclic ethers · CPC title

• C08G65/26

  from cyclic ethers and other compounds · CPC title

• B01J37/06

  Washing {(B01J37/0009, B01J37/0018 take precedence)} · CPC title