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Green synthesis method of oxine-copper technical material

A technology of quinoline copper and hydroxyquinoline, applied in the field of green synthesis of quinoline copper original drug, can solve problems such as environmental pollution, severe reaction conditions, layered precipitation, etc., and achieve green environmental protection in the process, high reaction conversion rate, The mild effect of the reaction process

Active Publication Date: 2021-03-30
CHINA KINGDOM AGRITECH QINGDAO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The existing production method is to use 8-hydroxyquinoline and copper sulfate, copper chloride, copper acetate, etc. as raw materials for chelation reaction to obtain copper quinoline. After the reaction, hydrogen equivalent to 8-hydroxyquinoline is needed Sodium oxide neutralizes the acid produced in the reaction process, adjusts the pH to weak acidity, and the reaction produces a large amount of inorganic waste salt or organic waste salt by-products, resulting in increased difficulty in sewage treatment and environmental pollution problems; the traditional process uses sodium hydroxide When the local hydroxide concentration is too high, it is easy to form copper hydroxide precipitation with copper ions, resulting in a decrease in the purity of the product; the reaction conditions of the conventional process are severe, and the obtained product does not contain crystal water, and this type of product is processed into a suspending agent When the stability is poor, it is easy to produce unstable results such as particle size growth and layered precipitation.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1, green efficient synthesis of quinoline copper original drug

[0022] At room temperature (25°C), add 100g of 8-hydroxyquinoline, 40g of basic copper carbonate and 280g of water to a reactor with a stirring condensing reflux device, and slowly add 50% sulfuric acid dropwise to the above system under stirring Solution 1g, in this embodiment, the mass ratio of 8-hydroxyquinoline, basic copper carbonate and dilute sulfuric acid is 200:80:1, heat up to 50°C, keep warm for 2 hours, then heat up to 75°C, keep warm for 1 After the reaction was completed, it was naturally cooled to room temperature.

[0023] Suction filter the reaction system after cooling and crystallization, and wash the obtained solid product with water three times, each time with about 150 g of water; transfer the obtained solid product to an oven, and dry it at 80°C for 12 hours to obtain the green copper quinoline original drug. Weighing 133.7g, the liquid chromatography detection content is...

Embodiment 2

[0028] Embodiment 2, the green high-efficiency synthesis of quinoline copper original drug

[0029] At room temperature (25°C), add 400g of 8-hydroxyquinoline, 135g of copper hydroxide, and 1500g of water to a reactor with a stirring condensing reflux device, and slowly add 30% sulfuric acid solution dropwise to the above system under stirring 6g, in this example, the mass ratio of 8-hydroxyquinoline, basic copper carbonate and dilute sulfuric acid is 222:75:1, the temperature is raised to 60°C, and the reaction is kept for 2 hours, then the temperature is raised to 80°C, and the reaction is kept for 1 hour . After the reaction was completed, it was naturally cooled to room temperature.

[0030] Suction filter the reaction system after cooling and crystallization, and wash the obtained solid product with water three times, with a water consumption of about 600g each time; transfer the obtained solid product to an oven, and dry it at 80°C for 12 hours to obtain the green coppe...

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PUM

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Abstract

The invention discloses a green synthesis method of oxine-copper technical material The preparation method comprises the following steps: reacting 8-hydroxyquinoline with copper salt in water under the catalysis of dilute sulfuric acid to obtain oxine-copper containing crystal water, wherein the copper salt is basic cupric carbonate or copper hydroxide. According to the invention, basic cupric carbonate or copper hydroxide is used as a copper source, a catalytic amount of sulfuric acid is used as a catalyst, water is used as a solvent, and a complexing reaction is carried out to obtain the oxine-copper technical material. The technological process of the synthesis method is more environmentally friendly, a reaction solvent is water, reaction byproducts are carbon dioxide and water, and a large amount of inorganic waste salt is not generated; the reaction process is mild, the reaction conversion rate is high, and the reaction process is fast; wherein the prepared product is a green quinoline copper raw drug containing crystal water.

Description

technical field [0001] The invention relates to a green synthesis method of quinoline copper raw drug, which belongs to the technical field of organic synthesis. Background technique [0002] Copper quinoline is a chemical substance, yellow to green powder, non-volatile, non-deliquescent, black at high temperature, insoluble in water and most solvents. Copper quinoline can be used as a pharmaceutical synthetic metal corrosion inhibitor; it is used as a fungicide in agriculture; it is also used as a fungicide for ropes, threads, leather, and vinyl plastics; it is used as a fungicide in agriculture to prevent and control bacterial horns in cucumbers Spot disease, mango bacterial angular spot, citrus canker, apple tree ring spot, etc. [0003] The existing production method is to use 8-hydroxyquinoline and copper sulfate, copper chloride, copper acetate, etc. as raw materials for chelation reaction to obtain copper quinoline. After the reaction, hydrogen equivalent to 8-hydrox...

Claims

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Application Information

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IPC IPC(8): C07D215/30
CPCC07D215/30
Inventor 赵帅祝帅柴泽宇但丽霞邱森森韩奉娟
Owner CHINA KINGDOM AGRITECH QINGDAO
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