Continuous process method for Carroll reaction
A process method and reaction technology, applied in the field of Carroll reaction continuous process and tank series continuous reaction, to achieve the effect of improving selectivity, stable product quality and increasing yield
Active Publication Date: 2015-02-04
SHANDONG NHU PHARMA +1
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Problems solved by technology
[0013] (2) Waste gas cannot be recycled
Irregularly emitted CO2 will entrain some organic matter, which cannot be recycled and is not environmentally friendly
[0014] (3) Full automation has not been realized, and there are potential safety hazards
[0015]If the above-mentioned low yield and safety and environmental protection requirements cannot be effectively solved, not only will the product cost lose its market competitiveness, but there will be a risk of being eliminated in terms of safety and environmental protection
Method used
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[0048] according to figure 1 Shown process flow diagram, a kind of Carroll reaction continuous process method, comprises the following steps:
[0049] a. Transesterification:
[0050] First prepare a part of the crude product of the reaction solution in the first normal pressure reactor, raise the temperature, drop the raw material tertiary alcohol, acylating agent diethyl methyl ester and catalyst organic aluminum salt into the first normal pressure reactor according to a certain ratio, and carry out transesterification Reaction, control transesterification reaction temperature and residence time;
[0051] b. Rearrangement reaction:
[0052] The product of the first atmospheric pressure reactor slowly enters the second atmospheric pressure reactor through the overflow port of the reactor for ester rearrangement reaction, and the rearrangement reaction temperature is controlled to ensure a certain residence time;
[0053] c. Decarboxylation reaction:
[0054] The pr...
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Abstract
The invention discloses a continuous process method for Carroll reaction. The method comprises the following steps: ester exchange; rearrangement reaction; decarboxylic reaction; thermal reaction; and raw material recovery. The method specifically comprises the following steps: carrying out ester exchange reaction on reaction raw material R-alcohol and an acylating agent to generate acetoacetic acid-R-ester and rearranging the ester to generate R-ketonic acid; and along with gradual rise of reaction temperature, carrying out decarboxylic reaction on the R-ketonic acid to obtain a product R-ketone. The reaction which is divided into three sections with five kettles in a kettle serial connection manner is carried out continuously, so that the reactions are fully and thoroughly carried out in a way of separately controlling temperatures of the kettles. According to the process method disclosed by the invention, the reaction is thoroughly carried out, less side reactions are caused, and the yield is greatly improved; stably output exhaust gas CO2 is comprehensively recycled; the process is fully automatic in the field, so that the production safety coefficient is improved.
Description
technical field [0001] The invention relates to a continuous Carroll reaction process, in particular to a Carroll reaction process and a kettle-type series continuous reaction method in the key process of plant ketone synthesis, belonging to the field of fine chemicals. Background technique [0002] Phytoketone is a colorless or light yellow oily liquid with a delicate fragrance. Because of its good fragrance-fixing and light characteristics, it is widely used in perfumery and is suitable for the preparation of flower-flavored essences. It is a very valuable spice , is an important high value-added intermediate product for the synthesis of vitamin E. In recent years, vitamin E is gradually being paid attention to by people because of its multiple uses of promoting human metabolism, enhancing physical vitality, reducing tissue aging, adjusting reproductive function, improving blood circulation and preventing arteriosclerosis, and the demand is increasing year by year, result...
Claims
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IPC IPC(8): C07C49/203C07C45/67
CPCC07C45/676C07C51/09C07C67/03C07C69/72C07C49/203C07C59/76
Inventor 李耀林马啸梁百安陈亚君梁晓东邱贵生
Owner SHANDONG NHU PHARMA