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Electrochemical preparation method of p-aminophenyl-beta-hydroxyethyl sulfone

A technology of hydroxyethyl sulfone and aminophenyl, which is applied in the field of electrochemical preparation of p-aminophenyl-β-hydroxyethyl sulfone, can solve the problems of polluted environment, low product yield and high production cost, and achieves the reaction Mild conditions, selectivity and high yield

Pending Publication Date: 2021-04-02
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The purpose of this invention is to provide a kind of electrochemical preparation method of p-aminophenyl-β-hydroxyethyl sulfone, which solves the high production cost existing in the preparation of p-aminophenyl-β-hydroxyethyl sulfone technology , low product yield and technical problems of environmental pollution

Method used

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  • Electrochemical preparation method of p-aminophenyl-beta-hydroxyethyl sulfone
  • Electrochemical preparation method of p-aminophenyl-beta-hydroxyethyl sulfone
  • Electrochemical preparation method of p-aminophenyl-beta-hydroxyethyl sulfone

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Embodiment 1

[0057] An H-type electrolytic cell is used as the reactor, the anode plate 3 is an anode plated titanium mesh, the cathode plate 4 is a cathode lead plate, and the cation membrane 7 is a cation exchange membrane Nafion PFSA Membranes (N-324).

[0058] The concentration of 1.5mol·L was added to the cathode compartment and anode compartment respectively. -1 250ml of sulfuric acid solution, and add 5g raw material p-nitrophenyl-β-hydroxyethyl sulfone (the raw material is provided by Henan Nayu New Material Co., Ltd., the purity is ≥98%.) in the cathode chamber, that is, 20g·L -1 , stirred and heated to 60°C with circulating water to maintain a constant temperature. After the raw materials were basically dissolved, electrolysis was started. Electrolysis was performed at a constant current of 0.74A, and the current density was 300A m -2 , when the incoming electricity reaches 7.2F·mol -1 Then, the reaction time was 338min, and the electricity was stopped, and the catholyte was ana...

Embodiment 2

[0072] An H-type electrolytic cell is used as the reactor, the anode plate 3 is an anode plated titanium mesh, the cathode plate 4 is a cathode copper plate, and the cation membrane 7 is a cation exchange membrane Nafion PFSA Membranes (N-324).

[0073] The concentration of 1.5mol·L was added to the cathode compartment and anode compartment respectively. -1 250ml of sulfuric acid solution, and 5g of raw material p-nitrophenyl-β-hydroxyethyl sulfone was added to the cathode chamber, that is, 20g L -1 , stirred and heated to 60°C with circulating water to maintain a constant temperature. After the raw materials were basically dissolved, electrolysis was started. Electrolysis was performed at a constant current of 1.23A, and the current density was 500A m -2 , when the incoming electricity reaches 6F·mol -1 After that, the reaction time was 282 min, the electricity was stopped, the catholyte was analyzed by high performance liquid chromatography, the current efficiency was 68.89...

Embodiment 3

[0075] An H-type electrolytic cell is used as the reactor, the anode plate 3 is an anode plated titanium mesh, the cathode plate 4 is a cathode lead plate, and the cation membrane 7 is a cation exchange membrane Nafion PFSA Membranes (N-324).

[0076] The concentration of 1.5mol·L was added to the cathode compartment and anode compartment respectively. -1 250ml of sulfuric acid solution, and 5g of raw material p-nitrophenyl-β-hydroxyethyl sulfone was added to the cathode chamber, that is, 20g L -1 , and 5g (2w%) of titanium sulfate, stirred and heated to 65°C with circulating water to maintain a constant temperature, after the raw materials were basically dissolved, electrolysis was started, and electrolysis was performed at a constant current of 0.74A, and the current density was 300A m -2 , when the incoming electricity reaches 6F·mol-1 After that, the reaction time was 282 min, the electricity was stopped, and the catholyte was analyzed by high performance liquid chromatogr...

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Abstract

The invention discloses an electrochemical preparation method of p-aminophenyl-beta-hydroxyethyl sulfone. The method comprises the following steps: using an electrolytic cell as a reactor, separatinga cathode chamber and an anode chamber by using a cationic diaphragm, respectively adding a sulfuric acid solution into the cathode chamber and the anode chamber, keeping the distance between electrode plates constant, adding p-nitrophenyl beta hydroxyethyl sulfone serving as a raw material into the cathode chamber, controlling the reaction temperature to be constant, performing electrifying for electrolysis, keeping the current density constant in the reaction process, and stopping electrifying when the introduced electric quantity reaches the target electric quantity so as to obtain an electrolyte containing p-aminophenyl beta hydroxyethyl sulfone sulfate; and neutralizing the catholyte with sodium hydroxide until the catholyte is alkaline, carrying out rotary evaporation to remove waterto obtain a solid, dissolving the solid with methanol, performing filtering to remove insoluble solids, and carrying out rotary evaporation on the filtrate to remove methanol to obtain a solid p-aminophenyl beta hydroxyethyl sulfone. The method provided by the invention is high in selectivity and yield, and the yield reaches 100% after sufficient electric quantity is introduced.

Description

technical field [0001] The invention belongs to the technical field of reactive dye intermediates and organic electrochemical synthesis, and in particular relates to an electrochemical preparation method of p-aminophenyl-β-hydroxyethyl sulfone. Background technique [0002] P-aminophenyl-β-hydroxyethyl sulfone is an important intermediate for the preparation of vinyl sulfone reactive dyes. It is generally prepared by reducing p-nitrophenyl-β-hydroxyethyl sulfone with iron powder. At present, the iron powder reduction method is widely used in China, and its biggest disadvantage is that a large amount of iron sludge and waste water containing aromatic amine compounds are produced after the reaction, which causes serious environmental pollution. In order to develop an environmentally friendly process, people try to replace the original iron powder reduction process with catalytic hydrogenation. The key to catalytic hydrogenation is to prepare a catalyst with excellent performa...

Claims

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Application Information

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IPC IPC(8): C25B3/25C25B3/07
Inventor 张新胜郭浩钮东方
Owner EAST CHINA UNIV OF SCI & TECH
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