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Method for regenerating working solution used for production of hydrogen peroxide and method for producing hydrogen peroxide using regenerated working solution

A working solution, hydrogen peroxide technology, applied in the direction of peroxide/peroxyhydrate/peroxyacid/superoxide/ozonide, metal/metal oxide/metal hydroxide catalyst, organic chemistry method, etc. , which can solve the problems of reducing the production efficiency of hydrogen peroxide, and achieve the effect of reducing the amount of solvent used, reducing the risk, and realizing the process.

Inactive Publication Date: 2016-08-31
MITSUBISHI GAS CHEM CO INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These by-products change various physical and chemical properties such as the specific gravity, viscosity, and surface tension of the working solution, and thus cause the production efficiency of hydrogen peroxide to decrease through the reduction, oxidation, and extraction steps of the working solution.

Method used

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  • Method for regenerating working solution used for production of hydrogen peroxide and method for producing hydrogen peroxide using regenerated working solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0058] Hereinafter, the present invention will be described in more detail by way of examples, but the present invention is not limited to these examples. Among them, in the present invention, pseudocumene (PSC) is used as the aromatic hydrocarbon as the nonpolar solvent in the working solution, and diisobutylcarbinol (DIBC) is used as the higher alcohol as the polar solvent. The ketone body derived from diisobutyl carbinol is diisobutyl ketone (DIBK), and each organic solvent component was measured by gas chromatography (GC). Among the organic solvent components, dimethylbenzoic acid, alkylphthalic anhydride, aliphatic carboxylic acids, trimethylphenol and 2 , 6-Dimethyl-4-heptanediol, etc.

[0059]

[0060] The acid value measurement of a solvent was performed based on JIS-K0070. The details are as follows. First, 40 mL of a solvent sample and 20 mL of an N / 10 sodium carbonate aqueous solution were weighed in a flask, and extracted at 50° C. for 15 minutes. Leave the e...

reference example 1

[0068]

[0069] As the working solution used in the first distillation step of the present invention, a working solution that has been used for many years in an actual hydrogen peroxide production device is used. Take out 2000ml of working solution from the hydrogen peroxide production device. The reaction medium in the working solution is amyl anthraquinone and amyl tetrahydroanthraquinone. In the recovery of the organic solvent component in the first stage, 400 ml of the working solution was placed in advance in a 1000 ml flask equipped with a distillation device, the degree of vacuum was controlled to 13 kPa, and the temperature was raised from room temperature. Distillation began when the temperature of the kettle reached 130°C. Since the liquid volume in the flask gradually decreased, the remaining working solution was gradually added, and the addition was stopped when the total amount added reached 2000ml. After the addition of the working solution was stopped, the di...

Embodiment 1

[0077]

[0078] 900 g of the solvent recovered by distillation and 9 g of N203SD (Cu-Cr based catalyst) manufactured by Nikki Kasei Co., Ltd. as a catalyst (1% by mass relative to the solvent recovered by distillation) were added to the autoclave, and a hydrogenation reaction was performed for 7 hours. The reaction temperature is controlled at 200° C., and the reaction pressure is controlled at 2.0 MPa. After completion of the hydrogenation reaction, the catalyst was left to stand at room temperature, and then, the catalyst was separated by filtration with a filter No. 1 made by ADVANTEC. The solvent obtained by performing hydrogenation reaction on the recovered solvent by distillation is called a hydrogenated solvent. As a result of analyzing this hydrogenation solvent component by GC, pseudocumene / diisobutylmethanol / diisobutyl ketone=62.4 mass % / 30.8 mass % / 6.4 mass %. Table 1 shows the GC analysis results of the hydrogenation solvent components accompanying the passage o...

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Abstract

In the production of hydrogen peroxide, a higher alcohol component in an organic solvent changes into a ketone body and increase in the ketone bodies reduces water content of a working solution and causes deterioration of catalytic activity. In addition, increase in the ketone bodies may obstruct stable and safe operation during the production of hydrogen peroxide due to decrease in the solubility of anthrahydroquinones, crystallization, precipitation, etc. The objective of the present invention is to provide a method for improving hydrogen peroxide production efficiency by regenerating an altered substance (ketone body) derived from a polar solvent in the working solution used for the production of hydrogen peroxide by the anthraquinone method to the original alcohol component. Hydrogen peroxide can be produced more efficiently by distilling off the organic solvent component including the ketone body from the working solution which has been used over time and hydrogenating the same under the presence of a metal catalyst to regenerate to the original alcohol component.

Description

technical field [0001] The present invention relates to the regeneration method of the working solution used when producing hydrogen peroxide by anthraquinone method. In more detail, it relates to a regeneration method of a working solution that regenerates an original polar solvent component by hydrogenating a modified product derived from a polar solvent in the working solution under a metal catalyst, and the use of Method for producing hydrogen peroxide from the working solution. Background technique [0002] The main production method of hydrogen peroxide currently carried out industrially uses a method using anthraquinones as a reaction medium, which is generally called an anthraquinone method. Anthraquinones are used dissolved in an appropriate organic solvent. The organic solvent is used alone or in the form of a mixture, and a mixture of two types, a polar solvent and a nonpolar solvent, is usually used. The solution prepared by dissolving anthraquinones in an org...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B15/023B01J23/86C07C37/07C07C39/12C07B61/00
CPCB01J23/868B01J29/00C01B15/023C07C29/143Y02P20/50Y02P20/584C07C31/125B01J23/26B01J23/40B01J23/72
Inventor 长谷川浩和田祐加子竹内基晴
Owner MITSUBISHI GAS CHEM CO INC
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