Method for paired electrolysis during synthesis of benzaldehyde, sorbitol and mannitol

A paired electrolysis and benzaldehyde technology, applied in electrolysis process, electrolysis components, electrolysis organic production, etc., can solve the problems of low current efficiency and space-time efficiency, harsh paired electrosynthesis process conditions, high production cost and energy consumption

Inactive Publication Date: 2014-03-12
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
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  • Claims
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AI Technical Summary

Problems solved by technology

[0007] Judging from the existing literature, whether it is the synthesis of benzaldehyde, or the preparation of mannitol and sorbitol, it is mainly based on the unipolar electrosynthesis method. Compared with the paired electrosynthesis technology, this method is not only The efficiency and space-time efficiency are relatively low, and the production cost and energy consumption are relatively high; the process conditions of paired electrosynthesis are also relatively harsh, and its yield or conversion rate is not high enough

Method used

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Examples

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Effect test

preparation example Construction

[0026] Step 2. Electrode preparation and pretreatment

[0027] Anode: Cut the nickel foam into a 2×2.5cm rectangle, wash it with alcohol and dilute hydrochloric acid in turn, and finally wash it with pure water for use; the nickel foam is used as the working electrode, the saturated calomel electrode is used as the reference electrode, and the nickel plate is Auxiliary electrode, the electrolysis current is 0.3A, and the electrolyte composition is 0.1mol / L NiSO 4 +0.1mol / L CH 3 COONa+0.5mol / L NaOH, carry out constant current electrolysis until black NiOOH is formed on the surface of the electrode, which is the NiOOH electrode and is ready for use.

[0028] Cathode: Cut the lead plate with a purity of 99.9% into a 3×3.5cm rectangle, polish it with sandpaper, wash it with alcohol, then wash it with dilute hydrochloric acid, and finally wash it with water for use.

[0029] Step 3: paired electrosynthesis of benzaldehyde, sorbitol, and mannitol

[0030] Install the H-type diaph...

Embodiment 1

[0037] Place the treated cation exchange membrane in an H-type diaphragm electrolyzer, use Pd plate as the cathode, and NiOOH as the anode, add 40mL pure water and 2.0g of sodium sulfate, and solid NaOH 0.1 g (cathode pool) and 1.2g (anode pool), start the electromagnetic stirrer to dissolve it completely, then add 5.41g of glucose to the cathode pool, add 5.40g of benzyl alcohol to the anode pool, stir for 5 minutes, and put Adjust the temperature of the reaction solution to 25°C, set the electrolysis current to 0.1A, and conduct constant current electrolysis for 19320s; after the electrolysis reaction is completed, add H to the anolyte 2 SO 4 The solution was neutralized to a pH of 2-3, then transferred to a 100mL separatory funnel, extracted with ethyl acetate, separated, and then extracted twice with water, combined with ethyl acetate, washed with water three times (10mL each time), and washed with It is dried and dehydrated with anhydrous sodium sulfate, and then separat...

Embodiment 2

[0041] The experimental process only changed the add-on of solid NaOH in the cathode cell, increased from 0.1g to 0.2g, and the rest were the same as in Example 1. The analysis results show that the yield of benzaldehyde is 85.35%, while the conversion rate of sorbitol and mannitol is 91.63%, and the total current efficiency of the whole electrolysis reaction is 176.98%. It can be seen that, by increasing the amount of alkali in the catholyte to accelerate the glucose The hydrolysis reaction improves the yield of the product, but its effect is not obvious. It shows that the addition of 0.1g of NaOH in the cathode cell can satisfy the hydrolysis reaction of glucose, and at the same time, OH will also be generated due to the hydrogen evolution side reaction of the cathode - , which is conducive to the hydrolysis of glucose.

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Abstract

A method for aired electrolysis during synthesis of benzaldehyde, sorbitol and mannitol comprises the followings: a cationic membrane is processed firstly, then electrode preparation and pretreatment are performed, and finally paired electrosynthesis is carried out, wherein paired electrosynthesis refers to that an H-type diaphragm electrolytic cell is provided with a cationic exchange membrane, both a cathode electrolytic bath and an anode electrolytic bath use a sodium sulfate solution as supporting electrolyte, sodium hydroxide is used for adjusting the alkalinity of the solution, then benzyl alcohol is added into an anode pool, glucose is added into a cathode pool, after stirring, the reaction temperature is adjusted through thermostatic waterbath, constant-current electrolysis is performed through setting electrolytic current, the benzyl alcohol is selectively oxidized to be benzaldehyde at the anode, and the glucose is reduced to be the sorbitol and the mannitol at the cathode. According to the method, in the same electrolytic process, two compounds of the benzyl alcohol and the glucose are both taken as raw materials, so that the benzaldehyde, the sorbitol and the mannitol are obtained simultaneously, the current efficiency and the time and space efficiency are improved greatly, the manufacturing cost and the energy consumption are reduced, the cathode product conversion rate is increased by more than 10 percent, and the economic benefit is very obvious.

Description

technical field [0001] The invention relates to a method for preparing benzaldehyde, sorbitol and mannitol, in particular to a paired electrosynthesis method for simultaneously preparing benzaldehyde, sorbitol and mannitol by using paired electrosynthesis technology. technical background [0002] Benzaldehyde, sorbitol, and mannitol are all important fine chemical intermediates and raw materials, widely used in medicine, food, pesticide dyes and other fields. [0003] Due to the mild conditions, simple operation and no pollution to the environment, the electrochemical method is a green synthesis technology, especially the paired electrosynthesis technology. In addition to the general advantages of electrosynthesis, it also has high current efficiency, high space-time efficiency, The advantages of low production cost, saving electric energy, and high electric energy efficiency have attracted people's attention. [0004] The electrosynthesis of existing benzaldehyde is mainly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/00
Inventor 李彦威王丽丽刘强张照昱李兴常宏宏魏文珑
Owner TAIYUAN UNIV OF TECH
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