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A kind of synthesis technique of copper extractant 5-nonyl salicylaldoxime

A technology of nonylsalicylaldoxime and nonylsalicylaldoxime, which is applied in the field of synthesis of copper extractant 5-nonylsalicylaldoxime, can solve the problems of long reaction cycle, long reaction time, and great safety, and achieve the goal of reaction The effect of high yield and product purity, low requirements for reaction conditions, and reduced reaction steps

Active Publication Date: 2017-01-04
三诺新材料科技(洛阳)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The problems of the current general synthesis method are: (1) The process is cumbersome, and it needs to go through magnesium methanol → nonylphenol magnesium salt → 5-nonylsalicylaldehyde magnesium salt → 5-nonylsalicylaldoxime magnesium salt → 5-nonylsalicylaldoxime
(2) The reaction cycle is long, especially when preparing nonylphenol magnesium salt and 5-nonyl salicylaldoxime, the methanol produced must be taken out by azeotropic method, and the reaction time is very long if the reaction is to be complete; (3) Prepare methanol A large amount of hydrogen is released during the magnesium process, which poses a safety hazard; at the same time, the process uses a large amount of methanol and toluene, and these two organic solvents are relatively toxic, which poses a major safety hazard in industrial production

Method used

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  • A kind of synthesis technique of copper extractant 5-nonyl salicylaldoxime

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Embodiment 1

[0030] First add 440g (6 mol) of fully dried N,N-dimethylformamide into a 2L glass four-neck flask equipped with a mechanical stirrer, a thermometer, a dropping funnel, a drying tube, and a nitrogen device, and cool in an ice-salt bath. To below 0°C, slowly add 253g (1.65mol) phosphorus oxychloride dropwise, the reaction is violently exothermic, keep the low temperature not exceeding 10°C, after the dropwise addition of phosphorus oxychloride is completed, continue to cool the system to about -5°C , add dropwise 364g (1.65mol) p-nonylphenol in 300ml DCE solution, keep the low temperature not exceeding 5°C, after the dropwise addition, raise the temperature to 5°C and keep stirring for 2 hours, then raise the temperature to 65°C and stir for 1 hour. After the reaction was finished, the system was cooled to room temperature, added 1L of deionized water and stirred for 10 min, left to separate the water, continued to wash twice with pure water, dried, and evaporated the solvent to...

Embodiment 2

[0033] First add 147g (2 mol) of fully dried N,N-dimethylformamide into a 2 L glass four-neck flask equipped with a mechanical stirrer, a thermometer, a dropping funnel, a drying tube, and a nitrogen device, and put it in an ice-salt bath Cool down to below 0°C, slowly add 353g (2.3mol) of phosphorus oxychloride dropwise, the reaction is violently exothermic, keep the low temperature below 10°C, after the dropwise addition of phosphorus oxychloride is completed, continue to cool the system to -5°C Add dropwise 440g (2mol) p-nonylphenol in 400ml acetonitrile solution, keep the low temperature not exceeding 5°C, raise the temperature to 5°C and keep stirring for 2 hours after the dropwise addition, then raise the temperature to 65°C and stir for 1 hour. After the reaction was finished, the system was cooled to room temperature, added 1L of deionized water and stirred for 10 minutes, left standing to separate the water, continued to wash twice with pure water, dried, and evaporate...

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Abstract

A synthesis process of copper extractant 5-nonylsalicylaldoxime, the preparation steps of which are: (1) synthesis of iminium salt (2) preparation of 5-nonylsalicylaldehyde by hydrolysis (3) preparation of 5-nonylsalicylaldoxime Synthesis (4) Standing and stratifying, the water phase was separated, and the upper oil phase was distilled under reduced pressure to obtain 5‑nonylsalicylaldoxime. Compared with the traditional process, the present invention has significantly fewer reaction steps, and the reaction conditions require low reaction to be carried out at normal temperature and pressure. High yield and product purity.

Description

technical field [0001] The invention relates to the technical field of hydrometallurgy, in particular to a synthesis process of copper extractant 5-nonyl salicylaldoxime. Background technique [0002] Copper is one of the earliest ancient metals discovered by humans. Humans began to use copper as early as more than 3,000 years ago. Copper is a non-ferrous metal closely related to humans. It is widely used in electrical, light industry, machinery manufacturing, and construction industries. , national defense industry and other fields, it is second only to aluminum in the consumption of non-ferrous metal materials in my country. [0003] The development of copper smelting technology has gone through a long process, and the smelting of copper is still dominated by fire smelting. However, there are many problems in my country's copper industry, such as lack of copper resources, low copper content in minerals, and poor quality, which make it unable to meet the needs of the indust...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C249/08C07C251/48
Inventor 杨晓亮王亚涛刘麦女李亮亮张美景
Owner 三诺新材料科技(洛阳)有限公司