阅读说明：本技术 一种8-羟基喹啉的生产方法 (Production method of 8-hydroxyquinoline ) 是由 殷文 于 2020-08-07 设计创作，主要内容包括：本发明适用于化工生产技术领域,提供了一种8-羟基喹啉的生产方法,该生产方法包括以下步骤：将邻氨基苯酚、邻硝基苯酚与酸液进行搅拌混合,得到混合料；将甘油滴加至上述混合料中进行环合反应,得到反应液；用碱液将上述反应液中和至pH为7~8后,再进行分离,得到有机相；将上述有机相进行水洗分层后,再依次进行减压蒸馏、冷凝和粉碎处理,得到所述8-羟基喹啉。本发明提供的8-羟基喹啉的生产方法,通过先投入邻氨基苯酚和邻硝基苯酚,以及滴加浓硫酸后,再投入甘油,可以实现一锅法直接合成产品,此生产方法有效减少副反应的发生,进而提高8-羟基喹啉产品的收率和产品质量,其产品转化率可达96%,产品收率可达91%。(The invention is suitable for the technical field of chemical production, and provides a production method of 8-hydroxyquinoline, which comprises the following steps: stirring and mixing o-aminophenol, o-nitrophenol and acid liquor to obtain a mixture; dripping glycerin into the mixture for cyclization reaction to obtain reaction liquid; neutralizing the reaction solution with alkali liquor until the pH value is 7-8, and then separating to obtain an organic phase; and (3) washing and layering the organic phase, and then sequentially carrying out reduced pressure distillation, condensation and crushing treatment to obtain the 8-hydroxyquinoline. According to the production method of 8-hydroxyquinoline, provided by the invention, the o-aminophenol and the o-nitrophenol are firstly added, the concentrated sulfuric acid is dropwise added, and then the glycerol is added, so that the product can be directly synthesized by a one-pot method, the production method effectively reduces the occurrence of side reactions, the yield and the product quality of the 8-hydroxyquinoline product are further improved, the product conversion rate can reach 96%, and the product yield can reach 91%.)

1. The production method of 8-hydroxyquinoline is characterized by comprising the following steps:

stirring and mixing o-aminophenol, o-nitrophenol and acid liquor to obtain a mixture;

dripping glycerin into the mixture for cyclization reaction to obtain reaction liquid;

neutralizing the reaction solution with alkali liquor until the pH value is 7-8, and then separating to obtain an organic phase;

and (3) washing and layering the organic phase, and then sequentially carrying out reduced pressure distillation, condensation and crushing treatment to obtain the 8-hydroxyquinoline.

2. The method for producing 8-hydroxyquinoline according to claim 1, wherein the temperature for stirring and mixing is 60 to 80 ℃.

3. The method for producing 8-hydroxyquinoline according to claim 1, wherein the temperature of the cyclization reaction in the step is 140-160 ℃.

4. The method for producing 8-hydroxyquinoline according to claim 1, wherein the temperature of neutralization in the step is 80 to 90 ℃.

5. The method for producing 8-hydroxyquinoline according to claim 1, wherein the temperature of the vacuum distillation in the step is 220 to 240 ℃.

6. The method for producing 8-hydroxyquinoline according to claim 1, wherein the acid solution is concentrated sulfuric acid, and the mass concentration of the concentrated sulfuric acid is 95-98%.

7. The method for producing 8-hydroxyquinoline according to claim 6, wherein the mass ratio of the o-aminophenol to the acid solution is 1 (1.8 to 2.2).

8. The method for producing 8-hydroxyquinoline according to claim 1, wherein the alkali solution is a liquid alkali, and the concentration of the liquid alkali is 20% to 40%.

9. The method for producing 8-hydroxyquinoline according to claim 1, wherein the mass ratio of the o-aminophenol, the o-nitrophenol and the glycerol is 1 (0.5-0.7) to 1.2-1.5.

Technical Field

The invention belongs to the technical field of chemical production, and particularly relates to a production method of 8-hydroxyquinoline.

Background

8-hydroxyquinoline can be used as a medical intermediate, is a raw material for synthesizing kexieling, chloroiodoquinoline and chlorphenamine, and is also an intermediate of dye and pesticide.

Disclosure of Invention

The embodiment of the invention aims to provide a method for producing 8-hydroxyquinoline, aiming at solving the problems in the background technology.

The embodiment of the invention is realized in such a way that the method for producing 8-hydroxyquinoline comprises the following steps:

stirring and mixing o-aminophenol, o-nitrophenol and acid liquor to obtain a mixture;

dripping glycerin into the mixture for cyclization reaction to obtain reaction liquid;

neutralizing the reaction solution with alkali liquor until the pH value is 7-8, and then separating to obtain an organic phase;

and (3) washing and layering the organic phase, and then sequentially carrying out reduced pressure distillation, condensation and crushing treatment to obtain the 8-hydroxyquinoline.

In a preferable scheme of the embodiment of the invention, in the step, the temperature for stirring and mixing is 60-80 ℃.

As another preferable scheme of the embodiment of the invention, in the step, the temperature of the cyclization reaction is 140-160 ℃.

As another preferable scheme of the embodiment of the invention, in the step, the temperature of neutralization is 80-90 ℃.

In another preferable scheme of the embodiment of the invention, in the step, the temperature of reduced pressure distillation is 220-240 ℃.

As another preferable scheme of the embodiment of the invention, the acid solution is concentrated sulfuric acid, and the mass concentration of the concentrated sulfuric acid is 95-98%.

In another preferable mode of the embodiment of the invention, the mass ratio of the ortho-aminophenol to the acid solution is 1 (1.8-2.2).

As another preferable scheme of the embodiment of the invention, the alkali liquor is liquid alkali, and the concentration of the liquid alkali is 20-40%.

As another preferable scheme of the embodiment of the invention, the mass ratio of the o-aminophenol, the o-nitrophenol and the glycerol is 1 (0.5-0.7) to 1.2-1.5.

According to the production method of 8-hydroxyquinoline provided by the embodiment of the invention, the o-aminophenol and the o-nitrophenol are firstly added, the concentrated sulfuric acid is dropwise added, and then the glycerol is added, so that the product can be directly synthesized by a one-pot method, the production method effectively reduces the occurrence of side reactions, the yield and the product quality of the 8-hydroxyquinoline product are further improved, the product conversion rate can reach 96%, and the product yield can reach 91%.

Drawings

FIG. 1 is a process flow diagram of a method for producing 8-hydroxyquinoline according to example 1 of the present invention.

FIG. 2 is a diagram showing the mass balance analysis of a method for producing 8-hydroxyquinoline according to example 1 of the present invention (unit: kg/lot).

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.