Method for synthesizing pipradrol through electrocatalytic reduction on piperidone by Ti/Ce nano-TiO2 modified electrode

A technology for modifying electrodes and piperidone, which is applied in the direction of electrodes, electrolysis process, electrolysis components, etc., can solve the problems of poor electrode catalytic activity, poor electrode corrosion resistance, low electrolysis efficiency, etc., to achieve increased electrocatalytic sites and corrosion resistance Good, the effect of small surface particles

Inactive Publication Date: 2015-03-04
HUAINAN NORMAL UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

However, most of the existing technologies use traditional Pb plates as anodes, and Zn plates or Pb plates as cathodes, such as Chinese patent application number 201010230347.7, the application date is July 20, 2010, and the invention is named Electrochemical Synthesis without Diaphragm 2,2 , the method of 6,6-tetramethyl-4-piperidinol, most of these technical solutions have poor catalytic activity of the electrode, low electrolysis efficiency, easy deactivation of the electrode during the electrolysis process, poor corrosion resistance of the electrode, and poor selectivity. Good, which leads to the problem of many side effects

Method used

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  • Method for synthesizing pipradrol through electrocatalytic reduction on piperidone by Ti/Ce nano-TiO2 modified electrode
  • Method for synthesizing pipradrol through electrocatalytic reduction on piperidone by Ti/Ce nano-TiO2 modified electrode

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Embodiment 1

[0039] The present embodiment uses Ti / Ce nano-TiO 2 The method for synthesizing piperidinol by electrocatalytic reduction of piperidinone by modified electrode, the steps are:

[0040] Step 1. Preparation of Ti / Ce nano-TiO modified by rare earth Ce doping 2 Modified electrodes. The specific operation steps are:

[0041] 1) Using pure titanium metal as the substrate, the pure titanium metal mentioned here refers to titanium metal with a purity of 99.5-99.7%. Use 600-mesh emery paper to polish the titanium substrate. After the grinding is completed, wash it with acetone and absolute ethanol to remove oil. The volume ratio is 1:4. Finally, it was ultrasonically washed with secondary water and absolute ethanol for 15 minutes, and dried for later use.

[0042] 2) Preparation of rare earth Ce-doped composite nano-TiO 2 Sol, the process is as follows: A solution is a mixed solution composed of butyl titanate, absolute ethanol, acetylacetone, and distilled water. In this example...

Embodiment 2

[0052] The present embodiment uses Ti / Ce nano-TiO 2 The method for synthesizing piperidinol by electrocatalytic reduction of piperidinone by modified electrode, the steps are:

[0053] Step 1. Preparation of Ti / Ce nano-TiO modified by rare earth Ce doping 2 Modified electrodes. The specific operation steps are:

[0054] 1) Using pure titanium metal as the substrate, the pure titanium metal mentioned here refers to titanium metal with a purity of 99.5-99.7%. Use 1000-mesh emery paper to polish the titanium substrate. After the grinding is completed, wash with acetone and absolute ethanol to remove oil. The volume ratio is 1:4. Finally, it was ultrasonically washed with secondary water and absolute ethanol for 10 min, and dried for later use.

[0055] 2) Preparation of rare earth Ce-doped composite nano-TiO 2 Sol, the process is as follows: A solution is a mixed solution composed of butyl titanate, absolute ethanol, acetylacetone, and distilled water. In this example, the ...

Embodiment 3

[0065] The present embodiment uses Ti / Ce nano-TiO 2 The method for the synthesis of piperidinol by electrocatalytic reduction of piperidinone by modified electrode, its basic steps and effects are the same as in Example 1, except that:

[0066] Step 1. Preparation of Ti / Ce nano-TiO modified by rare earth Ce doping 2 In the process of modifying the electrode:

[0067] 1) Use 2000-mesh emery paper to polish the titanium substrate, put the degreased titanium substrate into a mixed solution of HF and ethylene glycol for 20 minutes, and use secondary water and absolute ethanol to ultrasonically wash it for 20 minutes. .

[0068] 2) Preparation of rare earth Ce-doped composite nano-TiO 2 Anhydrous ethanol in the sol process: distilled water: Ce(NO 3 ) 3 .6H 2 The molar ratio of O is 10:0.25:0.7, and the stirring speed of adding solution B to solution A is 600r / min.

[0069] 3) Coat the sol prepared in step 2) on the surface-clean titanium substrate obtained in step 1), dry it...

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Abstract

The invention discloses a method for synthesizing piperidinol by electrocatalytically reducing piperidinone by using a Ti / Ce nano-TiO2 modified electrode, which belongs to the technical field of electrocatalytic synthesis. The specific steps of the present invention are: Step 1, preparation of Ti / Cenano-TiO2 modified electrode modified by rare earth Ce doping; Step 2, electrolysis test, electrocatalytic reduction of piperidone to synthesize piperidinol, and Step 2 comprising assembling a diaphragm Electrolyzer, configuration of electrolyte, and electrolysis; step 3, extracting product: taking out the electrolyte that has been electrolyzed in step 2, performing extraction and purification to obtain piperidinol product. The present invention adopts self-made rare earth Ce doped and modified highly active Ti / Ce nano-TiO2 modified electrode as the cathode, the electrode should not be deactivated during the electrolysis process, the electrode has good corrosion resistance, the electrolysis process has good selectivity, and the electrolysis side reaction is less. The high electrolysis efficiency ensures a high yield of piperidinol.

Description

technical field [0001] The invention relates to the technical field of electrocatalytic synthesis, in particular to the use of Ti / Ce nano-TiO 2 The modified electrode is used as a cathodic electrocatalytic method for the synthesis of piperidinol. Background technique [0002] Piperidinol is an important intermediate in the synthesis of hindered amine light stabilizers (HALS). The emergence of HALS has brought about a revolution in the history of light stabilizer development. It is the main development of light stabilizers in the world today. In recent years, with the rapid development of my country's plastics industry, it has provided market protection and development space for light stabilizers, and at the same time put forward higher requirements for light stabilizers. According to the "China Chemical Industry News" report: With the increase of domestic agricultural film production, the demand for light stabilizers in my country will exceed 5000 tons in 2010. At present,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B3/04C25B11/06C25B11/10C25B3/25
Inventor 徐迈王凤武方文彦魏亦军朱传高李敏鲍霞洪萍魏琳金莹
Owner HUAINAN NORMAL UNIV
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