Process for hydrogen peroxide production including step for regeneration of working solution

A technology of hydrogen peroxide and manufacturing method, applied in the direction of chemical instruments and methods, peroxide/peroxyhydrate/peroxyacid/superoxide/ozonide, physical/chemical process catalyst, etc., can solve the problem of no convenience Methods for removing inert substances, problems with handling liquid carbon dioxide, etc.

Active Publication Date: 2009-04-29
MITSUBISHI GAS CHEM CO INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the problem with this method is that a high-pressure reactor is necessary because liquid carbon dioxide is used, and there are also problems in the treatment of separated liquid carbon dioxide.
[0018] As mentioned above, there is no simple and effective method for removing inert substances in the prior art, and it is hoped to develop a method to control the inert substances in the working solution at a low concentration

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] The first distillation step of the present invention is carried out in a compact apparatus. 1000 g of a working solution for producing hydrogen peroxide was extracted from the hydrogen peroxide producing device and used for the experiment. The solvent recovery in the first stage is carried out by adding about 200 g of the working solution in advance to a 500 ml flask installed in the distillation pot, adjusting the vacuum degree to 13 kPa, and raising the temperature from room temperature. After the start of distillation, the amount of liquid in the flask gradually decreased, so the working solution was gradually added, and when the total amount added reached 1000 g, the addition was stopped. After the addition of the working solution was stopped, the distillation was continued until the temperature in the distillation pot reached 200° C., and the solvent was recovered in about 2 hours. The solvent component in the anthraquinones remaining in the flask of the distillat...

Embodiment 2

[0041] The second distillation step of the present invention is carried out in a small apparatus. Distillation of anthraquinones is carried out at a pressure lower than that of the first distillation step. Continuing from Example 1, 300 g of anthraquinone-containing solid remained in the flask placed in the distillation pot, and distillation was performed with it. Heating was performed by reducing the pressure to 100 Pa with a vacuum pump. At this time, a small amount of residual solvent components are distilled off, thereby affecting the degree of vacuum. The temperature was raised slowly until it reached 250° C.·100 Pa, and distillation was carried out over 3 hours to obtain 238 g of distillate. In addition, the solvent·water accumulated in the return pipe (trap) was 2 g, which contradicts the result of Example 1, indicating that it was generated during distillation. On the contrary, the result of analyzing the anthraquinones in the residue remaining in the still by LC wa...

Embodiment 3

[0043] The regenerated catalyst contacting process of the present invention is carried out in a small apparatus. In order to confirm the distillation effect, first, a working solution was prepared by using the anthraquinones distilled in Example 2 and the solvent recovered in Example 1. The concentration of the working solution is adjusted to the concentration of the original working solution, and a fixed bed of alumina is used for regeneration. 280 g of KHD-12 manufactured by Sumitomo Chemical Co., Ltd. was used as the activated alumina, and liquid flow was performed at 80°C. The prepared working solution was circulated for 12 hours at a flow rate of 300ml / h (the contact time with the catalyst was 1 hour), and the target working solution was obtained by blowing oxygen into the buffer tank. Each composition to be analyzed by LC is shown below.

[0044] Table 1: Composition of each working solution of embodiment 3 (the weight % in the solid is in parentheses)

[0045] ...

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Abstract

A process for producing hydrogen peroxide which comprises a step in which a working solution comprising an organic solvent, anthraquinone having an alkyl substituent, and tetrahydroanthraquinone having an alkyl substituent is reduced and then oxidized to thereby produce hydrogen peroxide and a working solution regeneration step in which the inert substance generated as a by-product in the hydrogen peroxide production is removed from the working solution and the resultant working solution from which the inert substance has been removed is circulated again to the hydrogen peroxide production step. It is characterized in that the working solution regeneration step comprises i) a first distillation step in which the organic solvent is recovered by distillation at atmospheric pressure or a pressure lower than that and ii) a second distillation step in which the anthraquinone and tetrahydroanthraquinone are subsequently recovered by conducting distillation at a lower pressure and 200 DEG C or higher so as to result in a residence time of 1 hour or longer.

Description

technical field [0001] The present invention relates to an anthraquinone comprising anthraquinone with an alkyl substituent (hereinafter, sometimes simply referred to as "anthraquinone") and 5,6,7,8-tetrahydroanthraquinone with an alkyl substituent as anthraquinones (hereinafter, sometimes simply referred to as "tetrahydroanthraquinone") working solution repeated reduction, oxidation, thereby producing a method of hydrogen peroxide. More specifically, it relates to a method for producing hydrogen peroxide capable of efficiently removing inert substances by-produced along with the production of hydrogen peroxide from the working solution. Background technique [0002] <Outline of the production method of hydrogen peroxide by the anthraquinone method> [0003] Generally, anthraquinone or tetrahydroanthraquinone (hereinafter, sometimes referred to as "anthraquinones") is used by dissolving in a suitable organic solvent. As the organic solvent, a simple solvent or a mixe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B15/023B01J21/04
CPCB01J21/04B01J21/12C01B15/023
Inventor H·堺谷井浦克弘萩原猪佐夫松井勉北田大介
Owner MITSUBISHI GAS CHEM CO INC
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