2,2'-dichlorohydrazobenzene preparation method and special electrolytic tank thereof

A dichlorohydrogen azo, electrolytic cell technology, applied in 2 fields, can solve the problems of poor proton permeability, increase production cost, increase power consumption, etc. Effect

Active Publication Date: 2009-12-09
HANERGY TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The electrodes of the electrolytic cell used are stainless steel plates and hard lead plates, and the diaphragm material is corundum, so the proton permeability is poor
Due to the high hydrogen evolution potential of stai

Method used

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  • 2,2'-dichlorohydrazobenzene preparation method and special electrolytic tank thereof
  • 2,2'-dichlorohydrazobenzene preparation method and special electrolytic tank thereof
  • 2,2'-dichlorohydrazobenzene preparation method and special electrolytic tank thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Step A Activate Porous Cathode Plate and Porous Anode Plate

[0038] Pour 4550ml of cathodic lye NaOH solution with a concentration of 5wt% into cathode tank 1, and pour 7000ml of anolyte lye NaOH solution with a concentration of 30wt% into anode tank 2. Preheat the cathode lye in the cathode tank 1 at 50°C for 30 minutes, and at the same time pass the current density of 1A / dm 2 The current activates the porous cathode plate 5 and the porous anode plate 4, and the activation time is the same as the preheating time;

[0039] Preparation of 2,2'-dichlorohydroazobenzene by electrolytic reduction in step B

[0040] Add 450g of o-chloronitrobenzene, 1500ml of toluene, and 3.5g of cocatalyst sodium dodecylbenzenesulfonate into the cathode tank 1 in sequence, start the stirrer 9, and after the solution is mixed evenly, the porous anode plate 4 and the power supply anode Connection, the porous cathode plate 5 is connected to the cathode of the power supply, the hole 6 on the ...

Embodiment 2

[0046] Step A Activate Porous Cathode Plate and Porous Anode Plate

[0047]Pour 4550ml of cathodic lye KOH solution with a concentration of 10wt% into the cathode tank 1, and pour 7000ml of anolyte lye KOH solution with a concentration of 20wt% into the anode tank 2. Preheat the cathode lye in the cathode tank 1 at 60°C for 15 minutes, and at the same time pass the current density to 1.5A / dm 2 The current activates the porous cathode plate 5 and the porous anode plate 4, and the activation time is the same as the preheating time.

[0048] Preparation of 2,2'-dichlorohydroazobenzene by electrolytic reduction in step B

[0049] Add 450g of o-chloronitrobenzene, 1500ml of xylene, and 3.5g of cocatalyst sodium dodecylbenzenesulfonate into the cathode tank 1 in turn, start the stirrer 9, and after the solution is mixed evenly, the porous anode plate 4 and the power supply The anode is connected, the porous cathode plate 5 is connected to the cathode of the power supply, the hole ...

Embodiment 3

[0055] Step A Activate Porous Cathode Plate and Porous Anode Plate

[0056] Pour 4550ml of cathodic lye KOH solution with a concentration of 1wt% into cathode tank 1, and pour 7000ml of anode lye NaOH solution with a concentration of 40wt% into anode tank 2. Preheat the cathode lye in the cathode tank 1 at 30°C for 35 minutes, and at the same time pass the current density to 2.5A / dm 2 The current activates the porous cathode plate 5 and the porous anode plate 4, and the activation time is the same as the preheating time.

[0057] Preparation of 2,2'-dichlorohydroazobenzene by electrolytic reduction in step B

[0058] Add 450g of o-chloronitrobenzene, 1500ml of toluene, and 3.5g of cocatalyst sodium dodecylbenzenesulfonate into the cathode tank 1 in sequence, start the agitator 9, and after the solution is evenly mixed, the porous anode plate 4 and the power supply anode Connection, the porous cathode plate 5 is connected to the cathode of the power supply, the hole 6 on the ...

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Abstract

The invention discloses a 2,2'-dichlorohydrazobenzene preparation method and a special electrolytic tank thereof; the preparation method comprises the following steps: separately placing cathode alkali liquor and anode alkali liquor in the cathode tank and the anode tank of the electrolytic tank, preheating the cathode alkali liquor in the cathode tank at 30-60 DEG C for 15-35min while introducing an electric current activation porous negative plate 5 and a porous positive plate 4 with a current density of 1-2.5A/dm2; then adding the reactants containing o-chloronitrobenzene, toluene and promoter into the cathode tank 1 in turn, mixing and stirring the mixture evenly, and connecting a power supply with a voltage of 1.42-2.65V, an electrolytic current density of 1-5A and an electrolytic temperature of 50-80 DEG C. The preparation method of the invention has the advantages of simple process, mild technology condition, low electricity consumption and low cost.

Description

technical field [0001] The invention relates to a preparation method of 2,2'-dichlorohydroazobenzene, and also relates to a special electrolytic cell for preparing 2,2'-dichlorohydroazobenzene. Background technique [0002] 2,2'-dichlorohydroazobenzene is an intermediate for the production of 3,3'-dichlorobenzidine, and 3,3'-dichlorobenzidine is a very important pigment intermediate. Currently, 3 , The main methods of 3′-dichlorobenzidine include zinc powder method, formaldehyde hydrazine hydrate method, and catalytic hydrogenation method. At present, my country's industrial production mainly adopts the catalytic hydrogenation method, which uses noble metals such as Pd / C and Pt / C as catalysts and 1,4-naphthoquinone, 2,3-dichloro-1,4-naphthoquinone, etc. Catalyst and adding an appropriate amount of surfactants such as sodium dodecylbenzenesulfonate, etc., in benzene, toluene and other aromatic solvents and alkaline media, one-step hydrogenation reduction of o-chloronitrobenze...

Claims

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Application Information

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IPC IPC(8): C25B3/04C25B9/00C25B3/25
Inventor 张超肖钢侯晓峰
Owner HANERGY TECH
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