Process for alkoxylation with DMC catalysts in a loop reactor with ejector
View Patent ↗The invention relates to a process for preparing polyethers of the formula (I) R 1 —(CHR 2 CHR 3 —O) n —H (I) where n=1 to 12 000, R 1 =a radical comprising at least one carbon atom and R 2 and R 3 are each independently H or a hydrocarbon radical, where the units designated with the index n may be the same or different (the R 2 and R 3 radicals in the different units n may thus be the same or different), by alkoxylating a starter compound which comprises the R 1 radical in the presence of a double metal cyanide catalyst (DMC catalyst) in a loop reactor, which is characterized in that the alkoxylation is performed in a loop reactor which has an ejector mixing nozzle, in which all substances involved in the reaction or assistants can be added to the circulated reaction mixture, an alkylene oxide or a plurality of different alkylene oxides being metered into the reaction mixture via the ejector mixing nozzle at the same time (random addition) or at different times (block addition).
1. Process for preparing polyethers of the formula (I)
R 1 —(CHR 2 CHR 3 —O) n —H (I)
where
n=1 to 12 000,
R 1 =a radical comprising at least one carbon atom
and
R 2 and R 3 are each independently H or a hydrocarbon radical, where the units designated with the index n may be the same or different, by alkoxylating a starter compound which comprises the R 1 radical in the presence of a double metal cyanide catalyst (DMC catalyst) in a loop reactor, characterized in that the alkoxylation is performed in a loop reactor which has an ejector mixing nozzle, in which all substances involved in the reaction or assistants can be added to the circulated reaction mixture, an alkylene oxide or a plurality of different alkylene oxides being metered into the reaction mixture via the ejector mixing nozzle at the same time or at different times wherein an equal total amount of added starter compound and of alkylene oxides, a relatively short sole addition of alkylene oxides carried out after the combined addition leads to a broad molar mass distribution.
2. Process according to claim 1 , characterized in that the polyether of the formula (I) prepared is the polyether of the formula (II)
where
a is 0 to 300,
b is 0 to 300,
c is 0 to 300,
d is 0 to 300,
R 1 is a radical comprising at least one carbon atom
and
with the proviso that at least one of the indices a to d is unequal to zero.
3. Process according to claim 1 , characterized in that it is performed batchwise.
4. Process according to claim 1 , characterized in that it is performed continuously.
5. Process according to claim 1 , characterized in that an inert gas is supplied to the reaction mixture via the ejector mixing nozzle and, in a vacuum system integrated in the loop reactor, components more volatile than the polyether are removed from the reaction mixture by applying a reduced pressure.
6. Process according to claim 1 , characterized in that a polyether and a DMC catalyst are initially charged as the reaction mixture in the start phase and then, simultaneously, the starter compound and at least one alkylene oxide are metered into the reaction mixture.
7. Process according to claim 1 , characterized in that the starter compound is selected from the group of the alcohols, carboxylic acids, aldehydes and ketones.
8. Process according to claim 7 , characterized in that the starter compound used is a mono- or polyhydric alcohol.
9. Process according to claim 1 characterized in that starter compound and at least one alkylene oxide are added simultaneously in a first phase and this phase is followed by a phase of addition of one or more alkylene oxides in which no starter compound is added.
10. Process according to claim 1 , characterized in that starter compound and at least one alkylene oxide are added exclusively simultaneously.
11. Process according to claim 2 , characterized in that an inert gas is supplied to the reaction mixture via the ejector mixing nozzle and, in a vacuum system integrated in the loop reactor, components more volatile than the polyether are removed from the reaction mixture by applying a reduced pressure.
12. Process according to claim 11 , characterized in that a polyether and a DMC catalyst are initially charged as the reaction mixture in the start phase and then, simultaneously, the starter compound and at least one alkylene oxide are metered into the reaction mixture.
13. Process according to claim 12 , characterized in that the starter compound is selected from the group of the alcohols, carboxylic acids, aldehydes and ketones.
14. Process according to claim 13 , characterized in that the starter compound used is a mono- or polyhydric alcohol.
15. Process according to claim 14 characterized in that starter compound and at least one alkylene oxide are added simultaneously in a first phase and this phase is followed by a phase of addition of one or more alkylene oxides in which no starter compound is added.
16. Process according to claim 15 , characterized in that starter compound and at least one alkylene oxide are added exclusively simultaneously.