An Electrochemical Method for Online Analysis of Nitro Reduction Reaction

A technology of electrochemistry and nitro compounds, applied in the direction of electrochemical variables of materials, etc., can solve the problems of high detection consumption, complicated operation, long time consumption, etc., and achieve the effect of simple detection device, good electrochemical response, and feasibility of solving

Active Publication Date: 2021-06-04
LIANHE CHEM TECH +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical problem solved by the present invention is to overcome the cumbersome sample pretreatment, complicated and dangerous operation, long time-consuming, low efficiency, large detection consumption and inability to perform online testing in the analysis and test of nitro reduction reaction in the prior art. Defects such as real-time detection and high cost provide an electrochemical method for online analysis of nitro reduction reactions

Method used

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  • An Electrochemical Method for Online Analysis of Nitro Reduction Reaction
  • An Electrochemical Method for Online Analysis of Nitro Reduction Reaction
  • An Electrochemical Method for Online Analysis of Nitro Reduction Reaction

Examples

Experimental program
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Effect test

Embodiment 1

[0038](1) Add 510 mg of polydiallyl ammonium chloride to 50 mL of DMF and mix to prepare a polyelectrolyte solution. Take 3 to 5 mL of the polyelectrolyte solution and place it in a dialysis membrane device, wherein the molecular weight cut-off of the dialysis membrane is 3500;

[0039] (2) The surface of the working electrode (platinum disk microelectrode) needs to be cleaned before use. Use 0.05μm a-AL 2 o 3 Powder polished, then rinsed with ultrapure water; wipe dry for use.

[0040] (3) Place the working electrode (platinum disk microelectrode), counter electrode (platinum wire) and reference electrode (silver / silver chloride electrode) in the dialysis membrane device in (1), and then mix with 2,6-di The reaction solution of methylnitrobenzene (solvent is DMF) is connected to the electrochemical system circuit, and the working voltage is set in the range of -2.0 ~ 1.8v by electrochemical cyclic voltammetry, and the 2,6-dimethylnitrobenzene The reaction solution is analyz...

Embodiment 2

[0042] (1) Add 490mg of polystyrene sulfonic acid to 50ml of methanol and mix to prepare a polyelectrolyte solution. Get 3 to 5ml of the polyelectrolyte solution and place it in a dialysis membrane device, wherein the molecular weight cut-off of the dialysis membrane is 7000;

[0043] (2) The surface of the working electrode (platinum disk microelectrode) needs to be cleaned before use. Use 0.05μm a-AL 2 o 3 Powder polished, then rinsed with ultrapure water; wipe dry for use.

[0044] (3) Place the working electrode (platinum disk microelectrode), counter electrode (tungsten wire) and reference electrode (saturated calomel electrode) in the dialysis membrane device in (1), and then mix with 2-methyl-5- The nitrobenzenesulfonic acid reaction solution (the solvent is methanol) is connected to the electrochemical system circuit, and the operating voltage is set at -2.0 to 2.0v by electrochemical cyclic voltammetry, and the p-2-methyl-5-nitrobenzene The sulfonic acid reaction so...

Embodiment 3

[0046] (1) Add 512mg polydiallyldimethylammonium chloride to 50ml DMAC and mix to prepare a polyelectrolyte solution, take 3-5ml polyelectrolyte solution and place it in a dialysis membrane device, wherein the molecular weight cut-off of the dialysis membrane is 50000 ;

[0047] (2) The surface of the working electrode (platinum disk microelectrode) needs to be cleaned before use. Use 0.05μm a-AL 2 o 3 Powder polished, then rinsed with ultrapure water; wipe dry for use.

[0048] (3) Place the working electrode (platinum disk microelectrode), counter electrode (tungsten wire) and reference electrode (silver / silver chloride electrode) in the dialysis membrane device in (1), and then mix with 4-chloro-3 -The nitroanisole reaction solution (the solvent is DMAC) is connected to the electrochemical system circuit, using electrochemical cyclic voltammetry, the working voltage is set at -2.0 ~ 1.8v range, the 4-chloro-3-nitrobenzene The methyl ether reaction solution was analyzed a...

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Abstract

The invention discloses an electrochemical method for on-line analysis of nitro reduction reaction. The method comprises the following steps: (1) placing the mixed solution of the polyelectrolyte and the organic solvent in the dialysis membrane device; (2) placing the working electrode, the counter electrode and the reference electrode in the dialysis membrane device in step (1) After that, the dialysis membrane device is placed in the nitro compound reaction solution, and then connected to the electrochemical system circuit, the nitro reduction reaction can be analyzed and detected. The material used in the analytical method of the present invention has low toxicity, and can not only simplify the detection device for the nitro reduction reaction, but also can quickly complete the detection process through the diffusion of the nitro compound on the microelectrode, and because the membrane technology is applied to Electrochemical voltammetric detection technology, the combination of the two technologies, greatly solves the feasibility of online monitoring of organic reactions.

Description

technical field [0001] The invention belongs to the technical field of detection in the chemical industry, and in particular relates to an electrochemical method for on-line analysis of nitro reduction reaction. Background technique [0002] Nitrobenzene is a basic raw material widely used in the chemical industry, and is mainly involved in the reduction reaction to prepare various fine chemical intermediates. The nitro reduction reaction is one of the more common reactions in the chemical industry. In the current chemical production, the analysis and testing of this reaction mainly involves chromatographic methods such as liquid phase, gas phase, and mass spectrometry. [0003] For the monitoring of the reaction of nitro reduction, it is to take multi-point sampling of the central control sample, and analyze and detect it with analytical instruments such as high performance liquid chromatography (HPLC) or gas chromatography (GC). Although these analytical methods have high ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/48G01N27/40
CPCG01N27/40G01N27/48
Inventor 樊小彬沈启富喻谨奚奇
Owner LIANHE CHEM TECH
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