Equilibrium reaction and gas/liquid reaction in a loop reactor
View Patent ↗The invention relates to a process for simultaneously performing two chemically successive reactions in a loop reactor, specifically reaction I) an optionally catalyzed equilibrium reaction between high-boiling liquid reactants, in which essentially one high boiler is formed as an intermediate and at least one low boiler as a by-product, and reaction II) a substantially diffusion-controlled reaction in which the liquid intermediate is reacted with at least one gaseous reactant to give the end product, wherein reactions (I) and (II), optionally after a start phase, are allowed to proceed simultaneously in the same apparatus, specifically loop reactor, and the loop reactor has a connectable gas-liquid circulation system coupled via an ejector mixing nozzle, in which circulated liquid phase is mixed in the ejector mixing nozzle with newly supplied gaseous reactant of reaction (II) ( 6 ) and/or gaseous reactant of reaction (II) aspirated by means of the ejector from the reactor via a connectable condenser ( 5 ), and fed to the reactor by a liquid jet ejector ( 2 ) for the reaction, the low-boiling by-product(s) of reaction (I) and also any low-boiling solvent being condensed and discharged in the condenser continuously over the duration of the process. In particular, the invention relates to a process for etherifying high-boiling polyether alcohols.
1. A process for performing two chemically successive reactions in a loop reactor, comprising
(reaction I) an optionally catalyzed equilibrium reaction of at least two high-boiling liquid reactants, in which essentially one high boiler is formed as an intermediate and at least one low boiler as a by-product, and
(reaction II) a substantially diffusion-controlled reaction in which the liquid intermediate is reacted with at least one gaseous reactant to give the end product,
wherein reactions (I) and (II), optionally after a start phase, are allowed to proceed simultaneously in the same loop reactor, and the loop reactor has a connectable gas-liquid circulation system coupled via an ejector mixing nozzle, in which circulated liquid phase is mixed in the ejector mixing nozzle with newly supplied gaseous reactant of reaction (II) ( 6 ) and/or gaseous reactant of reaction (II) aspirated by means of the ejector from the reactor via a connectable condenser ( 5 ), and fed to the reactor by a liquid jet ejector ( 2 ) for the reaction, the low-boiling by-product(s) of reaction (I) and also any low-boiling solvent being condensed and discharged in the condenser continuously over the duration of the process.
2. The process as claimed in claim 1 , which is carried out batchwise.
3. The process as claimed in claim 1 , which is carried out continuously.
4. The process as claimed in claim 1 , wherein, in a start phase, the high-boiling liquid reactants and optionally one or more catalysts are initially charged, the high-boiling liquid reactants optionally being present in a low-boiling solvent, and reaction (I) is carried out with condensation and discharge of the volatile by-product(s) and any solvent, either in a closed condensation gas circuit or by aspirating the inert gases by means of a vacuum unit via a condenser, until the distillation parameters predefined according to the process and plant technology have been attained.
5. The process as claimed in claim 1 , wherein the high-boiling liquid reactants and optionally one or more catalysts are initially charged, and the high-boiling liquid reactants may be present in a low-boiling solvent, and reactions (I) and (II) are carried out substantially without a start phase.
6. The process as claimed in claim 1 , in which offgas incineration is additionally carried out and the by-product from reaction (I) is used as carrier fuel.
7. The process as claimed in claim 1 for etherifying high-boiling, liquid alkyl- or alkenyl-started polyether alcohols of the general formula (1)
where
R 1 is an alkyl- or alkenyl radical having 1 to 5 carbon atoms,
Me is a methyl radical,
n and m are each an integer in the range from 0 to 90 and the sum of n+m is in the range from 5 to 90,
in a loop reactor, comprising,
as reaction (I) a deprotonation of the polyether alcohol, with a high-boiling, liquid alkali metal methylate, ethoxide or propoxide, optionally in the presence of a low-boiling solvent to form substantially a high-boiling alkali metal polyether alkoxide intermediate and at least one low-boiling alcohol as a by-product and,
as reaction (II), an ether coupling in which the liquid alkali metal polyether alkoxide intermediate is reacted with gaseous alkyl halide to give the end product,
wherein reactions (I) and (II), optionally after a start phase, are allowed to proceed simultaneously and the loop reactor has a gas-liquid circulation system coupled via an ejector mixing nozzle, in which circulated liquid phase is mixed in the ejector mixing nozzle with newly supplied gaseous alkyl halide of reaction (II) ( 6 ) and/or gaseous alkyl halide of reaction (II) aspirated by means of the ejector from the reactor via a condenser ( 5 ), and fed to the reactor by a liquid jet ejector ( 2 ) for the reaction, the low-boiling alcohol(s) of reaction (I) and also any low-boiling solvent being condensed and discharged in the condenser continuously over the duration of the process.
8. The process as claimed in claim 7 , wherein a start phase is provided in which the high-boiling liquid polyether alcohol is initially charged, alkali metal methylate, ethoxide or propoxide, optionally dissolved in low-boiling solvent, is added, and reaction (I) is carried out with condensation and discharge of the volatile alcohol(s) and any solvent, either in a closed condensation gas circuit or by aspirating the inert gases by means of a vacuum unit via a condenser, until the distillation parameters predefined according to the process and plant technology have been attained.
9. The process as claimed in claim 7 , wherein an upper temperature limit of 130° C. is not exceeded.
10. The process as claimed in claim 7 , wherein the reaction is carried out down to a residual alkali number of less than 0.1 mg KOH/g.
11. The process of claim 8 , wherein the low-boiling solvent is selected from the group consisting of especially methanol, ethanol, propanol and mixtures thereof.