Method for intermittent preparing diisopropyl ester amber acid
A technology of diisopropyl succinate and succinic acid, which is applied in the field of preparation of diisopropyl succinate, can solve the problems of many equipment, large material and energy consumption, large investment, etc. The effect of relatively low material consumption and low energy consumption
Active Publication Date: 2012-02-29
CINIC CHEM SHANGHAI +3
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Problems solved by technology
[0009] In the current production method, in order to increase the esterification rate, it is necessary to intermittently add anhydrous isopropanol to the esterification reactor, and generate more water-containing isopropanol at the same time, which must be recovered in a fractional distillation recovery system consisting of at least two towers. , to be able to fractionate hydrous isopropanol into anhydrous isopropanol, and then return to esterification, so that there are many equipments, large investment, large material consumption and energy consumption
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Embodiment 1
[0031] (1) 140 kilograms of succinic acid, 250 kilograms of isopropanol, 2.1 kilograms of 98% sulfuric acid and 70 kilograms of toluene are added into an esterification reactor with a fractionation tower top provided with a condenser and a water separator, heated to the reaction The temperature of the kettle is 83°C, and the vapor phase temperature of the condenser is 76.5±0.5°C. Under reflux, the esterification reaction is carried out until the water separator is free of water, and the temperature of the reactor is gradually increased to 98°C, and the vapor phase temperature of the condenser is greater than 77°C, reclaim the dehydrating agent and excess isopropanol in the reactor, then carry out post-treatment and refining of the crude ester generated by the esterification reaction, and collect 52 kg of the previous fraction;
[0032] (2) the dehydrating agent that 100 kilograms of steps (1) reclaims and excessive Virahol and 140 kilograms of succinic acid, 150 kilograms of Vi...
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This invention provides an intermittent method for preparing diisopropyl succinate. The method comprises: (1) adding succinic acid, isopropanol, catalyst and dehydrating agent into an esterification kettle with a rectification column with condenser and water separator at the top, esterifying, recovering dehydrating agent and excess isopropanol when there is no water from the water separator, and refining; (2) adding recovered dehydrating agent and excess isopropanol, and new succinic acid, isopropanol, catalyst and dehydrating agent into the reactor, and dropping front cut fraction; (3) refluxing, and esterifying; (4) recovering dehydrating agent and excess isopropanol; (5) refining crude ester to obtain diisopropyl succinate and front cut fraction. The method has such advantages as recoverable dehydrating agent and excess isopropanol, low energy consumption, low raw material consumption, short process, low investment, easy operation and stable product quality.
Description
technical field [0001] The present invention relates to the preparation method of diisopropyl succinate. Background technique [0002] Diisopropyl succinate is an organic synthesis intermediate, the main raw material for the synthesis of diketopyrrolopyrrole advanced organic pigments, and is also used as a stationary liquid for gas chromatography. [0003] At present, there are few reports on the direct synthesis of diisopropyl succinate. EP844,231, EP728,731, U.SP4,795,824 have reported that by maleic anhydride and alkyl alcohol (such as methyl alcohol and ethanol) through repeatedly catalytic esterification to generate dialkyl maleate, then catalytic hydrogenation becomes Diisopropyl succinate method. [0004] For intermittent batch production, the traditional esterification process is mostly used, that is, succinic acid and isopropanol are used as raw materials, under acidic conditions, catalytic synthesis under normal pressure, and the esterification reaction is carrie...
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IPC IPC(8): C07C69/40C07C67/08
Inventor 高云鹤孙松良
Owner CINIC CHEM SHANGHAI