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System and method for continuously preparing phenylhydroximic acid by using microreactor

A technology of phenylhydroxamic acid and microreactor, which is applied in the system field of preparing phenylhydroxamic acid, can solve the problems of many side reactions and low oximation rate, and achieves short reaction period, high commercial value, and product yield. high rate effect

Pending Publication Date: 2022-07-29
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to solve the problems such as low oximation rate, many side reactions, and safety caused by "hot spots" in the existing batch kettle production process, the present invention proposes a process for preparing phenylhydroxamic acid in a batch kettle according to the characteristics of the batch kettle production process. A system and method for continuously preparing mineral processing flotation agent phenylhydroxamic acid using a microreactor, utilizing the efficient mixing and excellent mass and heat transfer characteristics of the microreactor, which can enhance the mass transfer and reaction heat transfer capabilities of the reaction process , significantly reduce the volume and reaction time of batch reactors, improve reaction selectivity, reduce the occurrence of side reactions and process safety

Method used

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  • System and method for continuously preparing phenylhydroximic acid by using microreactor
  • System and method for continuously preparing phenylhydroximic acid by using microreactor
  • System and method for continuously preparing phenylhydroximic acid by using microreactor

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Example 1 Microreactor for continuous preparation of phenylhydroxamic acid

[0033] like figure 1 As shown, a micro-reaction system for preparing phenylhydroxamic acid, the micro-reaction system includes a first-stage microreactor 2 and a second-stage microreactor 3, a first-stage microreactor 2 and a second-stage microreactor The reactors 3 are connected in series through pipelines, the first-stage microreactor 2 and the second-stage microreactor 3 have built-in micro-heat exchangers, the first-stage microreactor 2 is connected to two advection pumps 1, and the second-stage microreactor The reactor 3 and the stirred tank 4 are connected by pipelines; the hydraulic diameter of the first-stage microreactor 2 and the second-stage microreactor 3 are both 0.5 mm and 25 cm in length.

[0034] The concrete steps that above-mentioned microreactor continuously prepares phenylhydroxamic acid are as follows:

[0035] (1) First add sodium methoxide (0.5mol, 34g), anhydrous metha...

Embodiment 2-5

[0037] Example 2-5 Continuous preparation of phenylhydroxamic acid in a microreactor

[0038]The same system and method as in Example 1 were used for the continuous preparation of phenylhydroxamic acid. During the reaction, the reaction temperature of the microreactor was different from that in Example 1. In Examples 2-5, the reaction temperatures were controlled to be 20°C, 25°C, 30°C, and 40°C, respectively. The specific results are shown in Table 1.

[0039] Table 1. Effects of different temperatures on the reaction

[0040]

Embodiment 6-8

[0041] Example 6-8 Continuous Preparation of Phenyl Hydroxamic Acid in Microreactors

[0042] The same system and method as in Example 1 were used for the continuous preparation of phenylhydroxamic acid. During the reaction, the total residence time of the materials in the microreactor was different from that in Example 1. In Examples 6-8, the total residence time of the reaction materials in the two reactors was 1.6 minutes, 0.8 minutes and 0.5 minutes, respectively. The reaction solution enters the stirring tank 4, and the dilute hydrochloric acid adjusts the pH to 5 to 6, and a large amount of white solid product phenylhydroxamic acid appears. Suction filtration to obtain the product phenylhydroxamic acid, and the liquid chromatography area normalization method analyzes the component content. The specific results are shown in Table 2.

[0043] Table 2. Effects of different residence times on the reaction

[0044]

[0045] The system and method for continuously preparin...

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Abstract

The invention belongs to the technical field of chemical engineering, and particularly relates to a micro-reaction system and method for continuously preparing phenylhydroxamic acid by using a micro-reactor, and the method is specifically as follows: raw materials methyl phenylformate and hydroxylamine hydrochloride or hydroxylamine sulfate are mixed in the micro-reactor in the presence of sodium alkoxide to react to generate sodium phenylhydroxamic acid salt; the device comprises a plurality of micro-reactors, the plurality of micro-reactors are connected in series through pipelines, and the last micro-reactor is connected with the reaction kettle through a pipeline. According to the method, the continuous preparation of the phenyl hydroximic acid is realized by adopting the microreactor, the process flow is simplified, the reaction period is short, the reaction is easy to control, the safety of the preparation process is improved, the selectivity is high, the yield of the phenyl hydroximic acid reaches 95% or above, and the method can be used for commercially producing a flotation agent phenyl hydroximic acid product.

Description

technical field [0001] The invention belongs to the technical field of chemical production, and in particular relates to a system and method for preparing phenylhydroxamic acid. Background technique [0002] Hydroxamic acids are a class of typical chelating agents with high selectivity to metal ions. Due to their molecular structure containing oxygen and nitrogen atoms with lone pairs of electrons, they can interact with metal ions Cu 2+ , Co 2+ , Ni 2+ , Fe 3+ and Zn 2+ Such metal ions form stable chelates (as shown in the following reaction formula), which is a very important metal complexing agent. Due to its unique molecular properties, hydroxamic acids have been widely used in hydrometallurgy, biomedicine, chemical separation, organic preparation and other fields. Hydroxamic acid can not only catalyze the oxidation of transition metal complexes, selectively extract metal ions, extract and separate rare earth metals, but also stably chelate with mineral metal ions ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J19/00B01J19/18C07C259/10
CPCB01J19/0093B01J19/18C07C259/10
Inventor 陈光文廉应江刘璇韩梅
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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