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Preparation method of quinolinic acid

A technology of quinolinic acid and quinoline, which is applied in the field of quinolinic acid preparation, can solve the problems of low equipment utilization, short reaction time, and restrictions on the mass production of quinolinic acid, and achieve the effects of reducing production costs and saving resources

Inactive Publication Date: 2017-06-13
FOSHAN SHANGHAO DOOR & WINDOW CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

low equipment utilization
The sodium chlorate oxidation method has mild reaction conditions, relatively short reaction time, good selectivity, and high synthesis yield, but the traditionally used catalysts are expensive, which seriously restricts the mass production of quinolinic acid

Method used

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  • Preparation method of quinolinic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 1. Oxidation.

[0019] Put copper oxide and dilute sulfuric acid in a 1:1 mixture into a reaction vessel and heat to 40°C.

[0020] After the copper oxide is completely dissolved, add quinoline and 2% potassium permanganate, stir and heat to 97°C.

[0021] Sodium chlorate solution was added dropwise and cooled to 30°C after completion.

[0022] The copper quinolinic acid filter cake was obtained by vacuum filtration, the filter cake was washed with water at 30°C until the filtrate was neutral, and the blue copper quinolinic acid product was obtained after the filter cake was dried.

[0023] 2. Alkaline hydrolysis

[0024] Stir and heat the copper quinolinic acid product and lye to 70°C, adjust the pH to 10, after the reaction is completed, cool down to 60°C, vacuum filter while it is hot, wash the filter cake copper oxide with hot water at 50°C, and then recycle it, and the filtrate Sodium quinolinate solution.

[0025] 3. Acidification

[0026] Add the sodium quin...

Embodiment 2

[0029] 1. Oxidation.

[0030] Put copper oxide and dilute sulfuric acid in a 1:1 mixture into a reaction vessel and heat to 45°C.

[0031] After the copper oxide is completely dissolved, add quinoline and 3% potassium permanganate, stir and heat to 100°C.

[0032] Sodium chlorate solution was added dropwise and cooled to 35°C after completion.

[0033] The copper quinolinic acid filter cake was obtained by vacuum filtration, the filter cake was washed with water at 35°C until the filtrate was neutral, and the blue copper quinolinic acid product was obtained after the filter cake was dried.

[0034] 2. Alkaline hydrolysis

[0035] Stir and heat the copper quinolinic acid product and lye to 70°C, adjust the pH to 10, after the reaction is completed, cool down to 60°C, vacuum filter while it is hot, wash the filter cake copper oxide with hot water at 50°C, and then recycle it, and the filtrate Sodium quinolinate solution.

[0036] 3. Acidification

[0037] Add the sodium qui...

Embodiment 3

[0040] 1. Oxidation.

[0041] Put copper oxide and dilute sulfuric acid in a 1:1 mixture into a reaction vessel and heat to 50°C.

[0042] After the copper oxide is completely dissolved, add quinoline and 4% potassium permanganate, stir and heat to 103°C.

[0043] Sodium chlorate solution was added dropwise and cooled to 40°C after completion.

[0044] The copper quinolinic acid filter cake was obtained by vacuum filtration, the filter cake was washed with water at 40°C until the filtrate was neutral, and the blue copper quinolinic acid product was obtained after the filter cake was dried.

[0045] 2. Alkaline hydrolysis

[0046] Stir and heat the copper quinolinic acid product and lye to 70°C, adjust the pH to 10, after the reaction is completed, cool down to 60°C, vacuum filter while it is hot, wash the filter cake copper oxide with hot water at 50°C, and then recycle it, and the filtrate Sodium quinolinate solution.

[0047] 3. Acidification

[0048] Add the sodium qui...

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Abstract

The invention discloses a preparation method of quinolinic acid. The preparation method uses quinoline as the raw material, and comprises the following steps of oxidizing, alkaline hydrolysis and acidifying. The preparation method has the advantages that the preparation is simple and quick, and the sewage zero-drainage is realized in the production process; compared with the quinolinic acid produced by the electrolysis method, the production efficiency is increased by 3 to 4 times; compared with common sodium chloride oxidizing method, the cost is low; the auxiliary material for production can be repeatedly recycled; the filtrate after separation of quinolinic acid can be repeatedly added with acid to separate, the recycling rate can reach 90%, the resource is greatly saved, and the market prospect is broad.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of quinolinic acid. [0002] technical background [0003] Quinolinic acid is an important intermediate of pesticides, medicines and pressure-sensitive pigments. It can be used to synthesize imidazolinone herbicides containing pyridine or quinoline rings. It can also be used to synthesize antibiotics. There are many synthetic methods of quinolinic acid, which can be divided into the following two methods according to the difference of starting materials: 8-hydroxyquinoline oxidation method and quinoline oxidation method. Due to the high price of 8-hydroxyquinoline, quinoline oxidation is mostly used at present. According to different oxidants, quinoline oxidation can be divided into four methods: (1) Potassium permanganate oxidation; (2) Hydrogen peroxide oxidation ; (3) hydrogen peroxide - sodium hypochlorite combined oxidation method; (4) sodium chlorat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/48
CPCC07D215/48
Inventor 刘正英
Owner FOSHAN SHANGHAO DOOR & WINDOW CO LTD
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