METHOD FOR PRODUCING POLYETHER CARBONATE POLYOLS
First Claim
1. A process for preparing polyether carbonate polyols comprising adding an alkylene oxide and carbon dioxide onto an H-functional starter substance in the presence of a double metal cyanide (DMC) catalyst or in the presence of a metal complex catalyst based on the metals zinc and/or cobalt, wherein the process comprises(γ
- ) adding the alkylene oxide and carbon dioxide onto the H-functional starter substance in a reactor at a total (absolute) pressure of 5 to 120 bar in the presence of a double metal cyanide catalyst or in the presence of a metal complex catalyst based on the metals zinc and/or cobalt to obtain a reaction mixture comprising the polyether carbonate polyol,(δ
) allowing the reaction mixture comprising the polyether carbonate polyol obtained in step (γ
) in the reactor or optionally transferring the reaction mixture continuously into a postreactor at an initial total (absolute) pressure of 5 to 120 bar, wherein the content of free alkylene oxide in the reaction mixture is reduced in each case by way of a postreaction, and wherein the total (absolute) pressure during step (δ
) can decrease by up to 50%, and(ζ
) thermally reducing the content of readily volatile constituents in the reaction mixture obtained at a temperature of 80°
C. to 200°
C., wherein;
(ε
) prior to step (ζ
), the reaction mixture resulting from step (δ
) is brought to a total (absolute) pressure of ≤
2.0 bar and then held at a temperature of 80 to 180°
C. for a residence time of at least 0.5 h, and after this residence time has elapsed, adding 5 to 100 ppm of component K to the resulting mixture, where component K comprises at least one compound containing a phosphorus-oxygen-hydrogen group.
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Abstract
The invention relates to a method for producing polyether carbonate polyols by adding alkylene oxides and carbon dioxide to an H-functional starter substance in the presence of a double metal cyanide (DMC) catalyst or in the presence of a metal complex catalyst based on the metals zinc and/or cobalt, wherein (γ) alkylene oxide and carbon dioxide are added to an H-functional starter substance in a reactor with a total pressure (absolute) of 5 to 120 bar in the presence of a double metal cyanide catalyst or in the presence of a metal complex catalyst based on the metals zinc and/or cobalt, and a reaction mixture containing the polyether carbonate polyol is obtained, (δ) the reaction mixture obtained in step (γ) remains in the reactor or is optionally continuously transferred to a downstream reactor at a starting total pressure (absolute) of 5 to 120 bar, the content of free alkylene oxide in the reaction mixture being reduced in the course of a downstream reaction in each case, and the total pressure (absolute) can be reduced by up to 50% during the step (δ), and (ζ) the content of highly volatile components of the obtained reaction mixture is thermally reduced at a temperature of 80° C. to 200° C. The invention is characterized in that (ε) the reaction mixture resulting from step (δ) is brought to a total pressure (absolute) of ≤2.0 bar, preferably 0.5 bar to 2.0 bar, particularly preferably 0.9 bar to 1.1 bar, prior to step (ζ) and then left at a temperature of 80 to 180° C. for a dwell time of at least 0.5 h. After the dwell time has expired, 5 to 100 ppm of component K is added to the resulting mixture, component K being selected from at least one compound which contains a phosphorus-oxygen-hydrogen group.
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17 Claims
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1. A process for preparing polyether carbonate polyols comprising adding an alkylene oxide and carbon dioxide onto an H-functional starter substance in the presence of a double metal cyanide (DMC) catalyst or in the presence of a metal complex catalyst based on the metals zinc and/or cobalt, wherein the process comprises
(γ - ) adding the alkylene oxide and carbon dioxide onto the H-functional starter substance in a reactor at a total (absolute) pressure of 5 to 120 bar in the presence of a double metal cyanide catalyst or in the presence of a metal complex catalyst based on the metals zinc and/or cobalt to obtain a reaction mixture comprising the polyether carbonate polyol,
(δ
) allowing the reaction mixture comprising the polyether carbonate polyol obtained in step (γ
) in the reactor or optionally transferring the reaction mixture continuously into a postreactor at an initial total (absolute) pressure of 5 to 120 bar, wherein the content of free alkylene oxide in the reaction mixture is reduced in each case by way of a postreaction, and wherein the total (absolute) pressure during step (δ
) can decrease by up to 50%, and(ζ
) thermally reducing the content of readily volatile constituents in the reaction mixture obtained at a temperature of 80°
C. to 200°
C., wherein;(ε
) prior to step (ζ
), the reaction mixture resulting from step (δ
) is brought to a total (absolute) pressure of ≤
2.0 bar and then held at a temperature of 80 to 180°
C. for a residence time of at least 0.5 h, and after this residence time has elapsed, adding 5 to 100 ppm of component K to the resulting mixture, where component K comprises at least one compound containing a phosphorus-oxygen-hydrogen group. - View Dependent Claims (2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16)
- ) adding the alkylene oxide and carbon dioxide onto the H-functional starter substance in a reactor at a total (absolute) pressure of 5 to 120 bar in the presence of a double metal cyanide catalyst or in the presence of a metal complex catalyst based on the metals zinc and/or cobalt to obtain a reaction mixture comprising the polyether carbonate polyol,
-
17. A polyether carbonate polyol mixture comprising polyether carbonate polyol and component K, wherein at least 98 mol % of the polyether carbonate polyol end groups consist of a terminal block of at least two alkylene oxide units in each case, and wherein component K comprises at least one compound containing a phosphorus-oxygen-hydrogen group.
Specification