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Electrode material for synthesizing p-aminophenol by electrolyzing nitrobenzene, preparation method and application thereof

A technology of p-aminophenol and electrode materials, applied in electrodes, electrolytic components, electrolytic processes, etc., can solve the problems of excessive reduction of intermediate phenylene, low reaction selectivity, low solubility, etc., and achieve high total yield and dangerous operation low cost and low equipment investment

Pending Publication Date: 2021-12-17
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The electrode material of the present invention is used in the cathode of electrolyzing nitrobenzene to synthesize p-aminophenol, and the compound surfactant is introduced, which can effectively solve the problems of low solubility in water, slow diffusion of products, raw materials and intermediates in the traditional synthesis process, and intermediate benzene The problem of low reaction selectivity caused by excessive reduction of bromelain

Method used

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  • Electrode material for synthesizing p-aminophenol by electrolyzing nitrobenzene, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] Preparation of electrode materials for electrolysis of nitrobenzene to synthesize p-aminophenol:

[0075] (1) Put 38g of spherical copper metal particles (about 6,000 pieces) with a diameter of 0.3mm into acetone and ultrasonicate for 20min to remove surface grease;

[0076] Get 100g tetrabutyl titanate, 0.5g acetylacetone, 39.1g concentrated hydrochloric acid (37wt%), 500g deionized water and 1000g absolute ethanol and mix evenly, wherein, tetrabutyl titanate, acetylacetone, concentrated hydrochloric acid (37wt%) ), deionized water, and absolute ethanol in a mixing mass ratio of 1:0.005:0.4:5:10, then add 0.8g niobium pentachloride and 2.37g anhydrous copper chloride therein, and stir to obtain a sol solution.

[0077] Place the degreased copper particles in a centrifuge tube, add 7.6g of sol solution, mix the sol solution with the degreased copper metal particles at a mass ratio of 0.2:1, spin coat in a centrifuge for 20s, and spin the sol at 2000r / min The solution w...

Embodiment 2

[0080] Preparation of electrode materials for electrolysis of nitrobenzene to synthesize p-aminophenol:

[0081] (1) Put 22.5g of spherical copper metal particles (about 32,000 pieces) with a diameter of 0.1mm into acetone and ultrasonicate for 15 minutes to remove surface grease;

[0082] Get 100g tetrabutyl titanate, 0.4g acetylacetone, 30g concentrated hydrochloric acid (33wt%), 400g deionized water and 1000g absolute ethanol and mix evenly, wherein, tetrabutyl titanate, acetylacetone, concentrated hydrochloric acid (33wt%) , deionized water, absolute ethanol mixing mass ratio is 1: 0.004: 0.3: 4: 10, then adds 1.6g niobium pentachloride and 1.58g anhydrous cupric chloride wherein, stirs and makes sol solution;

[0083] Place the degreased copper particles in a centrifuge tube, add 6.8g sol solution, mix the sol solution with the degreased copper metal particles at a mass ratio of 0.3:1, spin coat in a centrifuge for 10s at a speed of 5000r / min, and dissolve the sol The so...

Embodiment 3

[0086] Preparation of electrode materials for electrolysis of nitrobenzene to synthesize p-aminophenol:

[0087] (1) Put 70.4g of spherical copper metal particles (about 25,000 pieces) with a diameter of 0.2mm into acetone and ultrasonicate for 30min to remove surface grease;

[0088] Get 100g tetrabutyl titanate, 0.6g acetylacetone, 60g concentrated hydrochloric acid (37wt%), 1000g deionized water and 1500g absolute ethanol and mix evenly, wherein, tetrabutyl titanate, acetylacetone, concentrated hydrochloric acid (37wt%) , deionized water, dehydrated ethanol mixed mass ratio is 1: 0.006: 0.6: 10: 15, then adds 2.4g niobium pentachloride and 1.2g anhydrous cupric chloride wherein, stirs and makes sol solution;

[0089] Place the degreased copper particles in a centrifuge tube, add 28.1g of sol solution, mix the sol solution with the degreased copper metal particles at a mass ratio of 0.4:1, spin coat in a centrifuge for 15s at a speed of 3000r / min, and dissolve the sol The s...

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Abstract

The invention provides an electrode material for synthesizing p-aminophenol by electrolyzing nitrobenzene, a preparation method and application thereof. The electrode material is a composite material formed by filling a copper wire cage with copper metal particles and hydrophobic particles, wherein the hydrophobic particles are copper metal particles of which the surfaces are covered with niobium (Nb) and copper (Cu) doped titanium dioxide (TiO2) films. According to the invention, the electrode material is used for electrolyzing nitrobenzene to synthesize a cathode of p-aminophenol, and a compound surfactant of polyglycerol decastearate and dodecyl dimethyl betaine is added into a catholyte, so that the method can effectively solve the problems of low solubility and slow diffusion of products, raw materials and intermediates in water and low reaction selectivity caused by excessive reduction of the intermediate benzene mass in the traditional synthesis process, has the advantages of simple process and low energy consumption, and is suitable for wide industrial application.

Description

technical field [0001] The invention relates to an electrochemical synthesis method, in particular to an electrode material for electrolyzing nitrobenzene to synthesize p-aminophenol, a preparation method and application thereof. Background technique [0002] p-aminophenol (p-aminophenol, referred to as PAP) is an important chemical raw material and organic synthesis intermediate, widely used in pharmaceuticals, dyes, rubber, photography and other industrial fields. At present, the production of p-aminophenol in China mostly adopts iron powder reduction method, using p-nitrochlorobenzene as raw material, adding alkali and pressurizing hydrolysis to generate p-nitrophenol sodium salt, and then using inorganic acid to acidify to obtain p-nitrophenol, and then using iron Powder reduction of p-nitrophenol to produce p-aminophenol. In addition to the disadvantages of high raw material cost, long production process, and high iron content in the product, this method also discharge...

Claims

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Application Information

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IPC IPC(8): C25B11/04C25B3/09C25B3/07C25B3/25
CPCC25B11/04C25B3/09C25B3/25
Inventor 栾谨鑫钱向阳杜旺明张永振
Owner WANHUA CHEM GRP CO LTD
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