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Method for non-membrane electrochemical synthesis of 2,2,6,6-tetramethyl-piperidinol

A non-diaphragm, piperidinol technology, applied in the field of electrochemical synthesis, can solve the problems of difficult to realize industrialization, short service life, high equipment requirements, and achieve the effects of easy availability of equipment, short service life and low investment cost.

Inactive Publication Date: 2010-11-17
HEBEI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The more commonly used method in industry is to adopt catalytic hydrogenation method, the reaction yield of this method is as high as 96.5%, but it needs catalytic hydrogenation under high temperature and high pressure conditions, which requires high equipment and has certain dangers in the process; electrochemical synthesis The method has the characteristics of good selectivity, single product, easy separation, and recyclable electrolyte, which overcomes the defects of the catalytic hydrogenation method
However, ion exchange membranes are used in this method, and the current technology of ion exchange membranes in my country is not yet qualified. Although the price is cheap, the quality is poor and the service life is short. It is difficult to realize industrialization in China by using cation exchange membrane electrolyzers.

Method used

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  • Method for non-membrane electrochemical synthesis of 2,2,6,6-tetramethyl-piperidinol
  • Method for non-membrane electrochemical synthesis of 2,2,6,6-tetramethyl-piperidinol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Make a simple electrolytic cell without a diaphragm, use a Pb plate as an anode, and a Zn plate as a cathode;

[0020] (2) Configure the electrolyte solution:

[0021] The composition and content of the electrolyte solution are: sodium hydroxide 0.50mol / L, anhydrous sodium sulfate 0.35mol / L, piperidone 1.0mol / L, co-solvent is methanol or ethanol, and the mass fraction of co-solvent is 10%-40 %;

[0022] (3) Electrolysis: Under normal temperature and pressure, use a potentiostat to control the electric quantity to 1.0F / mol and the current density to 100A / m 2 , calculate the amount of time for electrolyzing the electrolyte in the electrolytic cell;

[0023] (4) Extraction of the product

[0024] a. Extraction: Take out the electrolyte in the diaphragmless electrolytic cell, neutralize it to pH=7 with sulfuric acid (50% by mass fraction, the same as in the following examples), extract with chloroform three times, discard the upper layer, and keep the lower layer . ...

Embodiment 2

[0027] (1) Make a simple electrolytic cell without a diaphragm, use a Pb plate as an anode, and a Zn plate as a cathode;

[0028] (2) Configure the electrolyte solution:

[0029] The composition and content of the electrolyte solution are: sodium hydroxide 0.50mol / L, anhydrous sodium sulfate 0.35mol / L, piperidone 1.0mol / L, co-solvent is methanol or ethanol, and the mass fraction of co-solvent is 10%-40 %;

[0030] (3) Electrolysis: under normal temperature and pressure, use a potentiostat to control the electric quantity to 1.5F / mol and the current density to 300A / m 2 , calculate the amount of time for electrolyzing the electrolyte in the electrolytic cell;

[0031] (4) Extraction of the product

[0032] a. Extraction: Take out the electrolyte solution in the electrolytic cell without diaphragm, neutralize it with sulfuric acid (50%) to pH=7, extract it three times with chloroform, discard the upper layer, and keep the lower layer. The solvent was distilled off under reduc...

Embodiment 3

[0035] (1) Make a simple electrolytic cell without a diaphragm, use a Pb plate as an anode, and a Zn plate as a cathode;

[0036] (2) Configure the electrolyte solution:

[0037] The composition and content of the electrolyte solution are: sodium hydroxide 0.50mol / L, anhydrous sodium sulfate 0.35mol / L, piperidone 1.0mol / L, co-solvent is methanol or ethanol, and the mass fraction of co-solvent is 10%-40 %;

[0038] (3) Electrolysis: under normal temperature and pressure, use a potentiostat to control the electric quantity to 1.1F / mol and the current density to 200A / m 2 , calculate the amount of time for electrolyzing the electrolyte in the electrolytic cell;

[0039] (4) Extraction of the product

[0040] a. Extraction: Take out the electrolyte solution in the diaphragmless electrolytic cell, neutralize it with sulfuric acid (50% by mass) to pH=7, extract it three times with chloroform, discard the upper layer, and keep the lower layer. The solvent was distilled off under r...

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Abstract

The invention discloses a method for non-membrane electrochemical synthesis of 2,2,6,6-tetramethyl-piperidinol. A non-membrane electrolytic cell is adopted, a Pb plate is taken as an anode, a Zn plate is taken as a cathode, sodium sulfate is taken as supporting electrolyte, a certain amount of sodium hydroxide and raw material of piperidone are added, two different organic latent solvents of methanol and ethanol are respectively added, and distilled water is added for preparing electrolyte. The electrochemical synthesis of piperidinol is carried out under a certain current density and electric quantity. The results show that the 2,2,6,6-tetramethyl-piperidinol can be directly obtained by taking 2,2,6,6-tetramethyl-4-piperidone as the raw material and carrying out the electrochemical synthesis under the condition of not using a membrane. The method can solve the technical defects of short service life of the membrane, high cost, difficult industrialization and the like caused by using the membrane. On the whole, the method is characterized by simple operation, easy obtainment of equipment, simple process flow, low investment cost and the like, and can carry out industrial production.

Description

technical field [0001] The present invention relates to a method for preparing 2,2,6,6-tetramethyl-4-piperidinol, in particular to a method for synthesizing 2,2,6,6-tetramethyl-4-piperidinol using a membrane-free electrochemical synthesis method. The method for 4-piperidinol belongs to the technical field of electrochemical synthesis. Background technique [0002] In the field of chemical synthesis technology, the methods for synthesizing piperidinol with 2,2,6,6-tetramethyl-4-piperidone (piperidone for short) include electrochemical synthesis, catalytic hydrogenation, and chemical reduction. Law. The more commonly used method in industry is to adopt catalytic hydrogenation method, the reaction yield of this method is as high as 96.5%, but it needs catalytic hydrogenation under high temperature and high pressure conditions, which requires high equipment and has certain dangers in the process; electrochemical synthesis The method has the characteristics of good selectivity,...

Claims

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Application Information

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IPC IPC(8): C25B3/04C25B3/25
Inventor 丁克强杨国凯田乐王庆飞
Owner HEBEI NORMAL UNIV
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