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Novel synthesis method of 2-hydroxy-5-nonylbenzaldoxime

A technology of nonylbenzaldehyde oxime and synthesis method, which is applied in the novel synthesis field of 2-hydroxy-5-nonylbenzaldehyde oxime, can solve the problems such as low conversion rate and purity, insufficient resource utilization, complicated process, etc. The effect of conversion rate and product purity, short synthesis process route and high synthesis efficiency

Inactive Publication Date: 2021-01-22
福建紫金选矿药剂有限公司
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Problems solved by technology

[0005] The traditional processing method will produce a large amount of gas and cause environmental pollution. At the same time, the synthesis path is long, the process is complicated, the conversion rate and purity after the reaction are low, and the resource utilization is insufficient, resulting in the waste of raw materials and the increase of production costs.
[0006] For this reason, a new synthetic method of 2-hydroxy-5-nonylbenzaldehyde oxime is provided to solve the problems of conversion rate, purity and efficiency

Method used

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  • Novel synthesis method of 2-hydroxy-5-nonylbenzaldoxime

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Embodiment 1

[0025] Embodiment 1, the present invention provides a kind of technical scheme, the novel synthetic method of 2-hydroxyl-5-nonylbenzaldehyde oxime, and this synthetic method comprises the following steps:

[0026] Step 1: Adding raw materials, respectively adding nonylphenol, toluene, and magnesium chloride into the reaction flask, the feeding molar ratio is 1:5.6:1.2, adding 76 g of triethylamine dropwise under stirring and gradually raising the temperature;

[0027] Step 2: Formylation reaction, weigh 52.5g of paraformaldehyde, add it to the reaction bottle in step 1 in batches, 3-4g each time, the interval is 5-10 minutes, and the process of adding paraformaldehyde is maintained at about 3 hours;

[0028] Step 3: Acidification reaction, lower the temperature of the reaction product after the formylation reaction in step 2 to 60°C, then slowly add 2.5N hydrochloric acid solution into the reaction flask in step 1, and keep the reaction at a temperature of 80°C 1 hour;

[00...

Embodiment 2

[0031] Embodiment two, the present invention provides a kind of technical scheme, the novel synthetic method of 2-hydroxyl-5-nonylbenzaldehyde oxime, and this synthetic method comprises the following steps:

[0032] Step 1: Adding raw materials, respectively adding nonylphenol, toluene, and magnesium chloride into the reaction flask, the feeding molar ratio is 1:5.6:1.2, adding 76 g of triethylamine dropwise under stirring and gradually raising the temperature;

[0033] Step 2: Formylation reaction, weigh 52.5g of paraformaldehyde, add it to the reaction bottle in step 1 in batches, 3-4g each time, the interval is 5-10 minutes, and the process of adding paraformaldehyde is maintained at about 3 hours;

[0034] Step 3: Acidification reaction, lower the temperature of the reaction product after the formylation reaction in step 2 to 60°C, then slowly add 2.5N hydrochloric acid solution into the reaction flask in step 1, and keep the reaction at 100°C 1 hour;

[0035] Step 4: Di...

Embodiment 3

[0037] Embodiment three, the present invention provides a kind of technical scheme, the novel synthetic method of 2-hydroxyl-5-nonylbenzaldehyde oxime, and this synthetic method comprises the following steps:

[0038] Step 1: Adding raw materials, respectively adding nonylphenol, toluene, and magnesium chloride into the reaction flask, the feeding molar ratio is 1:5.6:1.2, adding 76 g of triethylamine dropwise under stirring and gradually raising the temperature;

[0039] Step 2: Formylation reaction, weigh 52.5g of paraformaldehyde, add it to the reaction bottle in step 1 in batches, 3-4g each time, the interval is 5-10 minutes, and the process of adding paraformaldehyde is maintained at about 3 hours;

[0040] Step 3: Acidification reaction, lower the temperature of the reaction product after the formylation reaction in step 2 to 60°C, then slowly add 2.5N hydrochloric acid solution into the reaction flask in step 1, and keep the reaction at 60°C 1 hour;

[0041] Step 4: D...

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Abstract

The invention relates to the technical field of chemical extraction processing, in particular to a novel synthesis method of 2-hydroxy-5-nonylbenzaldoxime, which comprises the following steps of 1, adding raw materials, 2, formylation reaction, 3, carrying out an acidification reaction, and 4, distilling and purifying. The synthesis method has the beneficial effects that compared with the conventional magnesium-methoxide method, the synthesis method disclosed by the invention has the characteristics of shorter synthesis route, higher synthesis efficiency, no hydrogen generation, high conversion rate, high purity and the like, and can be compounded with 2-hydroxy-5-nonyl acetophenone oxime and an ester modifier to exert the optimal extraction and reverse extraction performance. A triethylamine-magnesium chloride method is adopted as a complex base catalyst, the 2-hydroxy-5-nonyl salicylaldehyde is synthesized by a one-pot method, the synthesis process route is short, and very high conversion rate and product purity can be obtained.

Description

technical field [0001] The invention relates to the technical field of chemical extraction and processing, in particular to a novel synthesis method of 2-hydroxy-5-nonylbenzaldehyde oxime. Background technique [0002] Copper solvent extraction has been based on two main oxime extractants for many years, aldoxime and ketoxime. Due to their own advantages and disadvantages, the two oxime extractants are generally ineffective in extracting copper. Usually, 2-hydroxy-5-nonylbenzaldehyde oxime and 2-hydroxy-5-nonylphenylethyl alcohol are combined Ketoxime is compounded in a certain ratio or 2-hydroxy-5-nonylbenzaldehyde oxime is compounded with an ester modifier to obtain the best extraction and stripping performance. [0003] Due to the long-term mining of copper resources, high-grade copper ore resources have become increasingly scarce, while the development and utilization of low-grade copper ore resources have promoted the development of copper extraction technology. More ...

Claims

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Application Information

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IPC IPC(8): C07C249/04C07C251/48C07C45/68C07C47/565B01J31/22
CPCB01J31/1805C07C45/68C07C249/04C07C251/48C07C47/565
Inventor 罗忠岩邹刚余海城杨占会
Owner 福建紫金选矿药剂有限公司
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