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A kind of preparation method of succinimide

A technology of succinimide and pyroglutamic acid, applied in the field of compounds, can solve problems such as waste of resources, and achieve the effects of avoiding corrosion, simple preparation method and wide source.

Active Publication Date: 2016-05-25
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the production of fuel ethanol, distiller's grains are usually discarded, thereby causing a waste of resources, so the application provides a method for utilizing glutamic acid to prepare succinimide

Method used

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  • A kind of preparation method of succinimide
  • A kind of preparation method of succinimide
  • A kind of preparation method of succinimide

Examples

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preparation example Construction

[0022] The embodiment of the present invention discloses a preparation method of succinimide, comprising:

[0023] The aqueous solution of one or both of pyroglutamic acid and pyroglutamate is mixed with silver salt and persulfate to obtain succinimide after reaction.

[0024] In the process of preparing succinimide, this application uses pyroglutamic acid and pyroglutamate as raw materials, and utilizes the nitrogen source of the amino acid itself without adding an additional nitrogen source; and the above-mentioned raw materials can all come from available sources. Regenerated by-products of fermentation metabolism from a wide variety of sources.

[0025] According to the present invention, the pyroglutamic acid is preferably prepared by heating and dehydrating glutamic acid, and the pyroglutamate is preferably prepared by heating and dehydrating glutamate. The preparation of the pyroglutamic acid can be done in a manner well known to those skilled in the art, and the prepa...

Embodiment 1

[0034] The preparation method of pyroglutamic acid or pyroglutamate is with reference to existing literature report, and concrete preparation method is as follows: add 100 grams of glutamic acid or glutamate in the 500 milliliter beaker, heat the beaker with oil bath, wait for temperature When it rises to 145-150°C, keep it warm for 45 minutes for dehydration reaction, and the solution after dehydration is brown; after the dehydration reaction is completed, pour the solution into boiling water with a volume of about 350 ml, and the solution is completely dissolved in water, and cooled to 40 After ~50°C, add an appropriate amount of activated carbon for decolorization, and repeat twice to obtain a colorless and transparent solution. Heat the obtained colorless and transparent solution directly to evaporate and concentrate until the volume is reduced to about half, then transfer to a water bath and continue to concentrate until the volume is about 1 / 3, then stop heating, and let ...

Embodiment 2

[0037] Put pyroglutamic acid 0.13g, 1mmol in the reaction tube, add AgNO 3 (1.7mg, 0.01mmol), add by weighing (NH 4 ) 2 S 2 o 8 (0.50g, 2.2mmol), add 3mL of water, stir at room temperature for 2h. After completion of the reaction, the reaction mixture was concentrated to dryness under reduced pressure to obtain succinimide. Add the prepared succinimide to deuterated chloroform, filter, and test the H NMR spectrum of succinimide, as figure 1 shown.

[0038] Add water to the prepared succinimide and perform HPLC detection; the specific detection conditions of HPLC are as follows: liquid phase instrument: HitachiL2000 high performance liquid chromatography; chromatographic column: AlltimaC185u250mm*4.6mm; mobile phase: methanol: water=10: 90 (v / v, containing 0.1% phosphoric acid); flow rate: 1.0mL / min; column temperature: 30°C; detector: diode array; detection wavelength: 204nm. The HPLC chromatogram of the succinimide prepared by the present embodiment is as follows figur...

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Abstract

The invention provides a preparation method of succinimide. The preparation method comprises the following steps: mixing one or two aqueous liquor of pyroglutamic acid and pyroglutamate with silver salt and peroxysulphate; and reacting to obtain succinimide. In the process of preparing succinimide provided by the invention, by taking pyroglutamic acid and pyroglutamate as a raw material, the nitrogen source of amino acids is utilized, and corrosion caused by adopting an external nitrogen source is avoided, so that the method is mild in condition of preparing succinimide. Furthermore, the raw material is wide in source, and succinimide can be obtained just under the effect of the silver salt and peroxysulphate, so that the preparation method is simple.

Description

technical field [0001] The invention relates to the technical field of compounds, in particular to a preparation method of succinimide. Background technique [0002] Succinimide, also known as succinimide and 2,5-dipyrrolidone, is an important class of organic chemical raw materials. Succinimide is mainly used in the synthesis of N-chlorosuccinimide (NCS), N-bromosuccinimide (NBS) and N-iodosuccinimide (NIS). It is an important intermediate in the preparation of pesticide products, and is widely used in chemical analysis and cyanide-free silver plating process. [0003] The synthesis process of succinimide reported so far is mainly realized by the amidation reaction of succinic acid and other external nitrogen sources, and the external nitrogen sources generally use ammonia gas, ammonia water and urea. The specific process of industrially synthesizing succinimide is as follows: put succinic acid into a reaction pot, add ammonia water dropwise, and stir to dissolve and reac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D207/404
CPCC07D207/404
Inventor 傅尧邓晋宋海杰
Owner UNIV OF SCI & TECH OF CHINA
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