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Electrolytic synthesis method for 1,5-diamino-4,8-dihydroxyanthraquinone by one-step method

A technology of dihydroxyanthraquinone and electrolytic synthesis, which is applied in electrolytic process, electrolytic components, electrolytic organic production, etc., can solve the problems of high production cost, environmental pollution, large equipment investment, etc., and achieves low production cost, short process route, The effect of less pollution from the three wastes

Inactive Publication Date: 2007-10-17
ZHEJIANG UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Obviously, there are many problems in chemical production, such as many synthesis steps, long process flow, more pollution of three wastes, large equipment investment and high production cost. very serious
[0004] The catalytic hydrogenation method is more reported now, but this method needs to consume high-purity noble metal catalysts, and needs to be operated at high temperature and high pressure, the cost is high, and it still needs multiple steps to synthesize 1,5-diamino- 4,8-dihydroxyanthraquinone, so there are still problems such as many synthesis steps, long process flow, high investment cost and environmental pollution

Method used

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  • Electrolytic synthesis method for 1,5-diamino-4,8-dihydroxyanthraquinone by one-step method
  • Electrolytic synthesis method for 1,5-diamino-4,8-dihydroxyanthraquinone by one-step method
  • Electrolytic synthesis method for 1,5-diamino-4,8-dihydroxyanthraquinone by one-step method

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Effect test

Embodiment 1

[0030] At first do blank test, adopt the device shown in accompanying drawing 1, amalgam copper electrode (Cu / Hg) is cathode, platinum plate is anode, the same solution dynamic hydrogen electrode is reference electrode, negative, anode liquid is 12.75mol / L sulfuric acid solution at a temperature of 140°C, using a Potentistat / galvanostat Model 273A from Princeton, USA, at a scan rate of 100mv / s for cyclic voltammetry scanning. The result is curve B in FIG. 2 .

[0031] The amalgamated copper electrode is used as the cathode, the platinum sheet is used as the anode, the same solution dynamic hydrogen electrode is used as the reference electrode, and 12.75mol / L sulfuric acid+0.00671mol / L 1,5-dinitroanthraquinone is used as the catholyte (ie, catholyte The final concentration of sulfuric acid in the medium is 12.75mol / L, and the final concentration of 1,5-dinitroanthraquinone is 0.00671mol / L, and other identical expressions have the same meaning), 12.75mol / L sulfuric acid solutio...

Embodiment 2～5

[0035]Embodiments 2-5 use Cu / Hg, Cu, Zn-Ni-Cu and Zn electrodes as cathodes respectively, platinum sheets as anodes, the same solution dynamic hydrogen electrode as reference electrode, catholyte is 12.75mol / L sulfuric acid+0.00671mol / L 1,5-dinitroanthraquinone, the anolyte is 12.75mol / L sulfuric acid solution, and the temperature is 140°C. Use the Potentistat / galvanostatModel 273A of Princeton, USA to perform steady-state polarization scanning. The results are shown in Figure 3 Curve 1, Curve 2, Curve 3, Curve 4 in.

Embodiment 6～9

[0037] With Cu / Hg as cathode, platinum sheet is as anode, and the same solution dynamic hydrogen electrode is reference electrode, and in the catholyte of embodiment 6~9, the final concentration of 1,5-dinitroanthraquinone is 0.00671mol / L, The final concentrations of sulfuric acid are 10.20mol / L, 11.90mol / L, 13.60mol / L, and 14.45mol / L, respectively, and the anolyte corresponds to sulfuric acid solutions of the same concentration, and the temperature is 140°C. / galvanostatModel 273A, respectively for steady-state polarization curves, the results are curve 1, curve 2, curve 3, curve 4 in Figure 4.

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Abstract

The present invention relates to a one-step method for electrolytic synthesis of 1,5-diamino-4,8-dihydroxyanthraquinone. Principally, according to the method, by adopting a cathode rotation cellular-type electrolytic tank, adopting sulfuric acid of 7.5-14.2 mol / L as electrolysing solution, adopting 1,5-dinitroanthraquinone as raw material, adopting a phase transfer catalyst, controlling the temperature at 100-160 DEG C, controlling the cathode electric potential of -0.1--0.4 V, controlling the electric current density at 200-2000A, an electroanalysis is performed to prepare said 1,5-diamino-4,8-dihydroxyanthraquinone final product, with one one step. Said phase transfer catalyst is SnCl2, BiCl3, cetyl trimethyl ammonium bromide or octadecyl trimethyl ammonium bromide. Said electrolytic synthesis method in accordance with the present invention is characterized by its short process route, high selectivity, low cost of manufacture, few environment pollution, high total outcome yield, and the like. Especially, the method is capable of one-step preparing 1,5-diamino-4,8-dihydroxyanthraquinone product. At the same time, said method can be extensively used for electrolytic synthesis of other aromatics aminophenol compounds.

Description

(1) Technical field [0001] The invention relates to a method for electrolytically synthesizing 1,5-diamino-4,8-dihydroxyanthraquinone, especially a method for preparing 1,5-diamino-4,8-dihydroxyanthraquinone in one step. (2) Background technology [0002] Aromatic aminophenol compounds are important organic chemical raw materials and intermediates, widely used in pharmaceuticals, pesticides, dyes, rubber and other industrial fields. 1,5-diamino-4,8-dihydroxyanthraquinone and its mixture are a kind of dye itself, and also an important intermediate in the dye field. As early as 1909, J. Deient applied 1,5-diamino-4,8-dihydroxyanthraquinone to prepare dyes and used them as vat dyes (C.I vat violet). Since 1971, this variety has been used as a disperse dye. Anthraquinone disperse dyes occupy a very important position in the field of dyes because of their bright color (especially blue and red), excellent light fastness, and good uniformity. In recent years, the export volume o...

Claims

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Application Information

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IPC IPC(8): C25B3/04C25B3/25
Inventor 马淳安张诚褚有群盛江峰
Owner ZHEJIANG UNIV OF TECH
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