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Production method of isatin

A production method, the technology of isatin, is applied in the direction of organic chemistry to achieve the effect of increasing the treatment capacity and reducing the amount of wastewater

Inactive Publication Date: 2018-05-11
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

From the perspective of safety, industrial production cannot be implemented directly from the laboratory-scale data of the above-mentioned literature and patents

Method used

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  • Production method of isatin
  • Production method of isatin
  • Production method of isatin

Examples

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Comparison scheme
Effect test

Embodiment 10

[0087] Example 10 is leaching with crushed ice; Example 12 and Example 13 are leaching with -8°C supercooled water; Example 11 is leaching with -14°C supercooled water, and there is no significant difference in the yield and amount of isatin, but In the treatment capacity of kilomole level, the ice-breaking process can be exempted, and supercooled water is preferred. In order to use supercooled water in the closed-loop process, it is advisable to establish a supporting filtrate process for recovering the process.

[0088] As can be seen from the embodiment of the closed-loop process in Table 2: (1) Reducing the reaction temperature or reducing the concentration of sulfuric acid can improve the safety of the process, which is different from the closed-loop reaction reported in the above-mentioned literature, and improves the safety of the closed-loop reaction to prolong the reaction time , in exchange for reducing the double safety factor of reaction temperature and reaction su...

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Abstract

The invention relates to a production method of isatin. The production method comprises the following steps: (1) aniline hydrochloride (or containing part of un-salinized aniline) produced by reactionof aniline and hydrochloric acid is subjected to oximation reaction with chloral hydrate, hydroxylamine hydrochloride, water and sodium sulfate decahydrate or sodium sulfate in an acid medium, oximido acetanilide is obtained in the range of the ratio determined by the action mechanism of sodium sulfate, part of solid-phase sodium sulfate is retained in the system in the initial stage of the reaction, and the ratio of aniline (mol) / water (kg) can be increased; (2) in the closed-loop reaction, the reaction time is prolonged in exchange for low reaction temperature and low sulfuric acid concentration in order to improve the reaction safety and increase the yield of isatin. Compared with typical processes, the method has the advantages that the reaction safety is improved, the yield of isatinis increased, unit consumption and production cost can also be reduced, the utilization rate of equipment is increased, and the amount of produced waste water is reduced. According to the process, noobvious amplification effect is found by tests in thousands of moles.

Description

technical field [0001] The invention belongs to the technical field of isatin production technology, in particular to an isatin production method with safety, low unit consumption, high equipment utilization rate, high yield and less waste water. Background technique [0002] It is reported in the literature that isatin is a raw material for the synthesis of disperse dyes Disperse Yellow E-3-G and azo disperse dyes 4-nitro-2-cyanoaniline in terms of dyes, and is a synthetic quinolinonephthalein pigment Dilight yellow in terms of pigments. Raw materials for GR. The practical and mature typical two-step synthesis process of isatin was first seen in: C.S.Marvel, G.S.Hiers.ISATIN.Org.Syn.Coll.Vol.I, p.327 (1941); The patent technology and literature of the preparation of derivatives. The typical two-step process described above is as follows: [0003] (1) Aniline oximation: use aniline, hydrochloric acid, chloral, sodium sulfate decahydrate, and hydroxylamine hydrochloride as...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/38
CPCC07D209/38
Inventor 方建波周永生陈建梅顾浩
Owner CHANGZHOU UNIV
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