Polyether carbonate polyol production method
View Patent ↗The invention relates to a method for producing polyether carbonate polyols by attaching alkylene oxides and carbon dioxide to one or more H-functional starters in the presence of a double-metal cyanide catalyst, characterized in that (alpha) a suspending agent which contains no H-functional groups is provided in a reactor, (ss) optionally, a moiety of alkylene oxide is added to the mixture from step (alpha) at temperatures of 90 to 150 DEG C., and the addition of the alkylene oxide compound is then interrupted; and (gamma) one or more H-functional starters are continuously metered into the reactor during the reaction.
1. A process for the preparation of polyether carbonate polyols by addition of alkylene oxides and carbon dioxide on to one or more H-functional starter substance(s) in the presence of a double metal cyanide catalyst (DMC), comprising:
(α) initially introducing a suspending agent which comprises no H-functional groups into a reactor and
(γ) metering into the reactor one or more H-functional starter substance(s), one or more alkylene oxide(s) and optionally carbon dioxide simultaneously or sequentially, wherein said one or more H-functional starter substance(s) are metered continuously into the reactor during the reaction.
2. The process according to claim 1 , wherein in step (α) a suspending agent which comprises no H-functional groups is initially introduced into the reactor and no H-functional starter substance is initially introduced into the reactor.
3. The process according to claim 1 , wherein in step (α) a suspending agent which comprises no H-functional groups and additionally a part of the H-functional starter substance(s) are initially introduced into the reactor.
4. The process according to claim 1 , wherein in step (α) a suspending agent which comprises no H-functional groups together with DMC catalyst are initially introduced into the reactor.
5. The process according to claim 1 , additionally comprising after step (α):
(β) adding a part amount of alkylene oxide to the mixture from step (α): at temperatures of from 90 to 150° C., in which case the addition of the alkylene oxide compound is then interrupted.
6. The process according to claim 5 , wherein step (β) is carried out under an inert gas atmosphere, under an atmosphere of an inert gas/carbon dioxide mixture or under a carbon dioxide atmosphere.
7. The process according to claim 5 , wherein step (β) comprises:
(β1) in a first activation stage the addition of a first part of alkylene oxide is carried out under an inert gas atmosphere and
(β2) in a second activation stage the addition of a second part of alkylene oxide is carried out under a carbon dioxide atmosphere.
8. The process according to claim 1 , wherein in step (γ) one or more H-functional starter substance(s) and one or more alkylene oxide(s) are metered continuously in the presence of carbon dioxide.
9. The process according to claim 1 , wherein in step (γ) the metering of the one or more H-functional starter substance(s) is ended completed at a time before the addition of the alkylene oxide.
10. The process according to claim 8 , wherein in step (γ) DMC catalyst is metered continuously into the reactor and the resulting reaction mixture is removed continuously from the reactor.
11. The process according to claim 10 , wherein the DMC catalyst is added continuously as a suspension in the H-functional starter compound.
12. The process according to claim 10 , comprising:
(δ) transferring the reaction mixture removed continuously in step (γ) having a content of from 0.05 wt. % to 10 wt. % of alkylene oxide into an after-reactor in which the content of free alkylene oxide is reduced in the reaction mixture to less than 0.05 wt. % by an after-reaction.
13. The process according to claim 1 , wherein in step (α) at least one compound selected from the group consisting of 4-methyl-2-oxo-1,3-dioxolane, 1,3-dioxolan-2-one, acetone, methyl ethyl ketone, acetonitrile, nitromethane, dimethylsulfoxide, sulfolane, dimethylformamide, dimethylacetamide, N-methylpyrrolidone, dioxane, diethyl ether, methyl tert-butyl ether, tetrahydrofuran, ethyl acetate, butyl acetate, pentane, n-hexane, benzene, toluene, xylene, ethylbenzene, chloroform, chlorobenzene, dichlorobenzene and carbon tetrachloride is employed as the suspending agent.
14. The process according to claim 1 , wherein in step (α) 4-methyl-2-oxo-1,3-dioxolane and 1,3-dioxolan-2-one or a mixture of 4-methyl-2-oxo-1,3-dioxolane and 1,3-dioxolan-2-one is employed as the suspending agent.
15. The process according to claim 1 , wherein the H-functional starter substance is at least one substance selected from the group consisting of ethylene glycol, propylene glycol, 1,3-propanediol, 1,3-butanediol, 1,4-butanediol, 1,5-pentanediol, 2-methylpropane-1,3-diol, neopentyl glycol, 1,6-hexanediol, 1,8-octanediol, diethylene glycol, dipropylene glycol, glycerol, trimethylolpropane, pentaerythritol, sorbitol and polyether polyols having a molecular weight Mn in the range of from 150 to 4,500 g/mol and a functionality of from 2 to 3.