Stepwise execution of exothermic reactions with participation of carbocations
View Patent ↗The invention relates to a method for carrying out reactions with participation of carbocations, whereby the initial most strongly exothermic phase of the reaction is carried out at high temperature (60 to 120° C.) and short residence time (1 to 30 seconds) in a microreactor and the subsequent less exothermic phases are carried out at optionally lower temperatures in two or more residence time units with longer residence times (1 to 30 seconds).
1. An improved process for the execution of a reaction with participation of carbocations, which comprises:
(a) carrying out a most strongly exothermic initial phase of the reaction in a microreactor at a high temperature of from 60 to 120° C. and a short residence time of 1 to 30 seconds, and then subsequently
(b) carrying out less exothermic phases of the reaction in two or more residence time units, wherein the residence time in a first residence time unit is from 1 to 30 minutes and the reaction temperature in the first residence time unit is lower by 5 to 30° C. than the microreactor.
2. The process as claimed in claim 1 , wherein, for the initial phase, microreactors are used which have a mixing module from the group of the T-type mixers, microjet reactors, substream injection mixers, Y- or V-type mixers, interdigital mixers, rectangular mixers, slot mixers, triangular multilamination mixers, caterpillar mixers, cyclone micromixers, or combinations of these, and a heat-exchange module which has from one to a plurality of microheat-exchangers from the group of the micro-crossflow heat-exchangers, crossflow heat-exchangers with crossmixing, or stacked countercurrent heat-exchangers.
3. The process as claimed in claim 1 , wherein the first residence time unit following the microreactor comprises at least one of a capillary, a heat-exchanger, an optionally thermostatable loop reactor, a stirred tank, or a stirred-tank cascade.
4. The process as claimed in claim 1 , which comprises using a stirred-tank or a stirred-tank cascade is used as a second residence time unit.
5. The process as claimed in claim 1 , wherein the residence time in a second residence time unit following the first residence time unit is from 1 to 10 hours, and the reaction temperature in the second residence time unit is from 60 to 100° C.
6. The process as claimed in claim 1 , wherein the reaction is a Ritter reaction which is executed as a reaction with participtation of carbocations.
7. The process as claimed in claim 1 , wherein, the reaction with participation of carbocations is a reaction of acrylonitrile with diacetone alcohol, acetone, or mesityl oxide, in the presence of sulfuric acid, followed by hydrolysis to give diacetoneacrylamide.