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Electrochemical method for synthesizing 2,2'-dichlorohydrazobenzene by use of supported catalyst ionic membrane

A dichlorohydroazobenzene and dichlorohydroazo technology, which is applied in the field of organic electrochemical synthesis, can solve the problems of long reaction time, short working life of nickel foam, and increased power consumption.

Inactive Publication Date: 2013-08-28
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Finally, the product DHB is separated. The production of DHB by this method is relatively mature, and the processing is relatively simple, but the problem is that the reaction time is long and the labor intensity is high; then the use of cheap iron powder instead of zinc powder has been developed. The process is widely used, the technology is mature, and the raw materials are cheap and easy to obtain
The use of pump circulation instead of mechanical agitation has little effect on the product yield; and the choice of nickel foam for the cathode plate has a short working life, which is difficult for industrialization; the current density is high during the reaction process, which increases power consumption , which increases the cost of production

Method used

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  • Electrochemical method for synthesizing 2,2'-dichlorohydrazobenzene by use of supported catalyst ionic membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Preparation of perfluorosulfonic acid ion exchange membrane:

[0016] First, ultrasonically mix 5 g of perfluorosulfonic acid resin with a mass ratio of 5:1 and N,N-dimethylformamide until there are no more bubbles in the solution. Put a polytetrafluoroethylene (PTFE) mesh cloth with a size of 8 cm × 10 cm in a water bath at 80 ° C, and first use 3% H 2 o 2 Soak in the solution for 30min, then use 0.5mol / L H 2 SO 4 The solution was soaked for 30 minutes, and finally put into a drying oven for drying treatment. Secondly, the casting method is used to scrape the film, and the pretreated PTFE mesh is spread on the glass plate, and the prepared mixed solution is used to scrape the film. Finally, a perfluorosulfonic acid ion exchange membrane is prepared.

[0017] The perfluorosulfonic acid ion-exchange membrane is applied to the electrochemical synthesis of 2,2'-dichlorohydroazobenzene. The ion-exchange membrane is closely attached to the anode plate and separated from...

Embodiment 2

[0019] Modification of perfluorosulfonic acid ion exchange membrane:

[0020] First prepare graphite into graphene oxide (Graphene), then reduce the mixed solution of graphene oxide and chloroplatinic acid with sodium ascorbate (VC), and prepare Pt / Graphene with a mass ratio of Pt to graphene of 3:10 The catalyst has a particle size of 1.99nm; 5g of a mixed solution of perfluorosulfonic acid resin and N,N-dimethylformamide with a mass ratio of 5:1 and 0.1g of the prepared Pt / Graphene catalyst are ultrasonically mixed, until there are no more bubbles in the solution. Secondly, the casting method is used to scrape the film. Spread the polytetrafluoroethylene mesh cloth after impurity removal on the glass plate, and use the prepared mixed solution to scrape the film. Finally, a graphene-supported platinum ion exchange membrane with a metal platinum loading of 30% was prepared.

[0021] The graphene-supported platinum ion exchange membrane is applied to the electrochemical synt...

Embodiment 3

[0023] Modification of perfluorosulfonic acid ion exchange membrane:

[0024] First prepare graphite into graphene oxide (Graphene), then reduce the mixed solution of graphene oxide and chloroplatinic acid with sodium ascorbate (VC), and prepare Pt / Graphene with a mass ratio of Pt to graphene of 2:10 The catalyst has a particle size of 4.58nm; 5g of a mixed solution of perfluorosulfonic acid resin and N,N-dimethylformamide with a mass ratio of 5:1 and 0.1g of the prepared Pt / Graphene catalyst are ultrasonically mixed, until there are no more bubbles in the solution. Secondly, the casting method is used to scrape the film. Spread the polytetrafluoroethylene mesh cloth after impurity removal on the glass plate, and use the prepared mixed solution to scrape the film. Finally, a graphene-supported platinum ion exchange membrane with a metal platinum loading of 20% was prepared. The graphene-supported platinum ion exchange membrane was applied to the electrochemical synthesis of...

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Abstract

The invention relates to an electrochemical method for synthesizing 2,2'-dichlorohydrazobenzene by use of a supported catalyst ionic membrane. The method is used for preparing a catalyst which is supported on an ionic exchange membrane, so that the membrane has a higher hydrogen generation rate, the ionic exchange capacity is increased, and the electrochemical performance of the ionic exchange membrane is optimized. The ionic exchange membrane is applied to a reaction of electrochemical synthesis of 2,2'-dichlorohydrazobenzene from o-chloronitrobenzene; an electrolytic tank is separated into a cathode chamber and an anode chamber by the supported catalyst ionic exchange membrane; a sodium hydroxide solution is added into the cathode chamber and the anode chamber; the raw material o-chloronitrobenzene generates a reduction reaction in the cathode chamber; the supported catalyst ionic membrane realizes a great effect on promoting the increase of the hydrogen generation rate in the reducing process, and the reaction efficiency is improved; and the method provided by the invention has the characteristics of short technological process and high product yield.

Description

technical field [0001] The invention relates to an electrochemical method for synthesizing 2,2'-dichlorohydroazobenzene by using a loaded catalyst ion membrane, which belongs to the field of organic electrochemical synthesis, and specifically relates to the electrolytic reduction of o-chloronitrobenzene by using a loaded catalyst ion exchange membrane to generate Electrochemical approach to 2,2'-dichlorohydroazobenzene. Background technique [0002] 2,2′-Dichlorohydroazobenzene (DHB) undergoes intramolecular rearrangement in strongly acidic medium to generate 3,3′-dichlorobenzidine (DCB), which is permanent yellow HR, benzidine yellow And benzidine yellow G and other series of yellow dye intermediates, this series of organic dyes account for about 25% of the total organic dyes, because of its wide application and moderate price, so the development prospect is very broad. The synthesis route of 3,3'-dichlorobenzidine has been relatively clear, and 2,2'-dichlorohydroazobenzen...

Claims

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Application Information

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IPC IPC(8): C25B3/04C25B3/25
Inventor 孟庆函曹兵武近冬
Owner BEIJING UNIV OF CHEM TECH
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