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Synthesis method of high-purity 8-hydroxyquinoline copper

A technology of copper hydroxyquinoline and synthesis method, which is applied in the direction of copper organic compounds, etc., and can solve problems such as unstable quality and low purity of 8-quinolinol copper products

Pending Publication Date: 2021-09-10
无锡颐景丰科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The production method mainly adopted in the prior art is to obtain 8-hydroxyquinoline by cyclization, neutralization and steam distillation with o-aminobenzene, o-nitrophenol and acrolein as main raw materials, and then use 8-hydroxyquinoline Quinoline and copper sulfate are used as raw materials to carry out complexation reaction to obtain 8-hydroxyquinoline copper. The purity (95%-97%) of the 8-hydroxyquinoline copper product produced by this method is low, and the color of the product changes with time. This method The 8-hydroxyquinoline produced is then reacted with copper salt to synthesize quinolinone. The 8-hydroxyquinoline copper product obtained by the above method has lower purity and unstable quality

Method used

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  • Synthesis method of high-purity 8-hydroxyquinoline copper
  • Synthesis method of high-purity 8-hydroxyquinoline copper
  • Synthesis method of high-purity 8-hydroxyquinoline copper

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A kind of synthetic method of high-purity 8-hydroxyquinoline copper, comprises the following steps:

[0025] In a 5-ton reactor, add 790kg of ethanol, 525kg of 8-hydroxyquinoline, the heating rate is 3°C / min, steam is heated to 50°C, stirred and dissolved, the stirring rate is 150r / min, and 462kg of copper sulfate and 2370kg of water are added dropwise. The mixed solution was added dropwise for 1 hour. After the drop was completed, keep it at 50°C for 1 hour, take a sample for HPLC test, cool to 25°C, stir for 2 hours at a stirring rate of 150r / min, and the color of the solid turned green, as figure 1 shown. Centrifuge at a speed of 3000r / min for 15min to obtain 800kg of green powdery solid, and the test indicators meet the enterprise standards and can be bagged. The calculated yield is 99.28%, and the purity is 99.45%. Such as figure 2 Shown is the HPLC test result of this product. Its reaction equation is as follows:

[0026]

Embodiment 2

[0028] A kind of synthetic method of high-purity 8-hydroxyquinoline copper, comprises the following steps:

[0029] In a 5-ton reactor, add 903kg of ethanol, 600kg of 8-hydroxyquinoline, steam heated to 52°C, stir to dissolve, the stirring rate is 200r / min, dropwise add a mixed solution of 528kg of copper sulfate and 2708kg of water, 1h dropwise, After dripping, keep at 52°C for 1.5h, take samples for HPLC test, cool to 25°C, stir for 2.5h, the color of the solid turns green, centrifuge at 3200r / min for 20min, and obtain 914.4kg. Ready to bag. The yield is 99.27%, and the purity is 99.44%.

Embodiment 3

[0031] A kind of synthetic method of high-purity 8-hydroxyquinoline copper, comprises the following steps:

[0032] In a 10-ton reactor, add 1580kg of ethanol and 1050kg of 8-hydroxyquinoline, heat it with steam to 55°C, stir and dissolve at a stirring rate of 200r / min, add dropwise a mixed solution of 924kg of copper sulfate and 4740kg of water, and complete the dropwise addition within 1 hour. After dripping, keep at 55°C for 2h, take samples for HPLC test, cool to 25°C, stir for 3h, the color of the solid turns green, centrifuge at 3500r / min for 30min, and get 1600kg of green powdery solid. The standard can be bagged, the yield is 99.28%, and the purity is 99.43%.

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Abstract

The invention discloses a synthesis method of high-purity copper 8-hydroxyquinoline, which is characterized by comprising the following steps of: S1, dissolving 8-hydroxyquinoline in ethanol, and heating to obtain a heated solution; S2, keeping the temperature in S1, dropwise adding a mixed solution of water and copper sulfate pentahydrate into the heated solution, and stirring after dropwise adding; and S3, cooling the reaction liquid in S2 to 25-28 DEG C, stirring, and centrifuging to obtain the product. The method is high in yield, and the prepared copper 8-hydroxyquinoline is high in purity, stable in color and stable in product quality.

Description

technical field [0001] The invention relates to the technical field of copper 8-hydroxyquinolate, in particular to a method for synthesizing high-purity copper 8-quinolate. Background technique [0002] 8-Hydroxyquinoline is white, light yellow or crystalline powder, insoluble in water, soluble in ethanol and alkenoic acid, capable of sublimation, widely used in the determination and separation of metals, and is an important intermediate for the preparation of dyes and drugs. Its copper Salt complex is a yellow to green powder chemical substance of 8-hydroxyquinoline copper, suitable for storage in ventilated, low-temperature, dry warehouses, often used as fungicides, used to prevent and control apple tree ring disease, and used as antiseptic materials , including mildew repellent for rope, cord, leather, vinyl. [0003] At present, the production of 8-hydroxyquinoline copper adopts the following methods, including wet solid phase-vacuum hot melting method, direct synthesis...

Claims

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Application Information

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IPC IPC(8): C07F1/08
CPCC07F1/08
Inventor 张前军魏义春
Owner 无锡颐景丰科技有限公司
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