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Diisopropyl succinate and intermittent preparation method thereof

A technology of diisopropyl succinate and succinic acid is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., and can solve the problems of large materials and energy consumption, large equipment, large investment, etc. , to achieve the effect of small investment, small number of equipment and low energy consumption

Inactive Publication Date: 2011-06-22
SHANGHAI YOUHAO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] In the current production method, in order to improve 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 materials and energy consumption

Method used

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  • Diisopropyl succinate and intermittent preparation method thereof
  • Diisopropyl succinate and intermittent preparation method thereof
  • Diisopropyl succinate and intermittent preparation method thereof

Examples

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Embodiment 1

[0039] (1) with 140 kilograms of succinic acid, 250 kilograms of Virahol, 2.1 kilograms of 98% sulfuric acid and 70 kilograms of toluene, add the esterification reactor that has a condenser and a water trap at the top of the fractional distillation column, be heated to reaction The temperature of the kettle is 83°C, the temperature of the vapor phase of the condenser is 76.5±0.5°C, and under reflux, the esterification reaction is carried out until the water separator has no water out, and then the temperature of the reactor is gradually increased to 98°C, and the temperature of the vapor phase of the condenser is greater than At 77°C, the dehydrating agent and excess isopropanol in the reclaimer were recovered, and then the crude ester generated by the esterification was post-treated and refined, and 52 kg of front distillate was collected;

[0040] (2) dehydrating agent and excessive Virahol and 140 kilograms of succinic acid, 150 kilograms of Virahol, 2.1 kilograms of 98% sul...

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Abstract

The invention provides a diisopropyl succinate and an intermittent preparation method thereof. The molecular formula of the diisopropyl succinate is C10H18O4. The preparation method comprises the following steps: 1) adding succinic acid, isopropanol, a catalyst and a dehydrating agent into an esterification kettle for esterification, recovering the dehydrating agent and excessive isopropanol after no water is distributed from a water distributor, processing coarse ester, refining the coarse ester, and collecting a front fraction; 2) adding the recovered dehydrating agent, the recovered excessive isopropanol, new succinic acid, new isopropanol, new catalyst and new dehydrating agent into a reactor and dripping a front fraction; 3) performing esterification under reflux; 4) recovering the dehydrating agent and excessive isopropanol in the reactor; and 5) refining coarse ester to obtain diisopropyl succinate and the front fraction. In the invention, azeotropic esterification, azeotropic fractionation, reflux, water distribution and recovery are integrated, the recovery and recycling of the dehydrating agent and the excessive isopropanol are realized, energy consumption and material consumption are reduced, the process flow is short, less equipment is used, operation and control are easy, and product quality is stable.

Description

technical field [0001] The invention relates to a diisopropyl succinate and a batch preparation method thereof. Background technique [0002] Diisopropyl succinate is an organic synthesis intermediate, the main raw material for the synthesis of diketopyrrolopyrrole advanced organic pigments, and also used as a stationary liquid for gas chromatography, but the existing ones are used for the synthesis of Pigment Red 254 and 264 raw materials, there are quality problems, can not guarantee the quality of synthetic pigments. [0003] At present, there are few reports on the direct synthesis of diisopropyl succinate. EP844,231, EP728,731, U.SP4,795,824 reported that the catalysis of maleic anhydride and alkyl alcohols (such as methanol and ethanol) for many times Esterification generates dialkyl maleate, and then catalytic hydrogenation becomes diisopropyl succinate. [0004] For batch production, the traditional esterification process is mostly used, that is, succinic acid and ...

Claims

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Application Information

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IPC IPC(8): C07C69/40C07C67/08B01J20/22B01J20/292
Inventor 袁文平
Owner SHANGHAI YOUHAO CHEM
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