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 poll

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0021]Example 1, green high-efficiency synthesis of quinoline copper

[0022]Under normal temperature (25 ° C), 8-hydroxyquinoline 100g, alkali carbonate 40g and water 280g were added, and 50% sulfuric acid was slowly added dropwise to the above system in a stirred state in the stirring state. In this example, in this example, 8-hydroxyquinoline, the mass ratio of the base carbonate and the dilute sulfuric acid is 200: 80: 1, temperature rise to 50 ° C, the insulation reaction is 2 hours, then warmed to 75 ° C, heat insulation reaction 1 After the hour is completed, it is naturally cooled to room temperature.

[0023]The cooling crystal reaction system was filtered, the resulting solid product was washed 3 times with water, and the amount of water was about 150 g per time; the resulting solid product was transferred to an oven, dried at 80 ° C for 12 hours to give a green quinoline copper primary medicine. Those 133.7 g, the liquid chromatography was detected by 90.3%, and the reaction yi...

Example Embodiment

[0028]Example 2, green high efficiency synthesis of quinoline copper

[0029]Under normal temperature (25 ° C), 8-hydroxyquinoline 400g, aquohydride 135 g, water 1500g, and slowly added 30% sulfuric acid solution in the above system in the stiff condition in the stirring state 6g, this example, 8-hydroxyquinoline, basic ratio of copper carbonate and dilute sulfuric acid is 222: 75: 1, heating to 60 ° C, the holding reaction is 2 hours, then warmed to 80 ° C, heat insulation reaction for 1 hour . After the reaction is completed, it is naturally cooled to room temperature.

[0030]The cooling crystal reaction system was filtered, the resulting solid product was washed 3 times with water, and the amount of water was about 600 g per time; the resulting solid product was transferred to an oven, dried at 80 ° C for 12 hours to give a green quinoline copper primary medicine. The liquid phase chromatography was measured by 90.1%, and the calculated reaction rate was 99.6%, and 8.98% crystalline w...

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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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