Hydrogen peroxide working solution regenerant used in preparation of hydrogen peroxide process according to anthraquinone method and preparation method of hydrogen peroxide working solution regenerant

A technology of hydrogen peroxide and anthraquinone method, applied in peroxide/peroxy hydrate/peroxyacid/superoxide/ozonide, chemical instruments and methods, chemical recovery, etc. High requirements, impact and other issues, to achieve the effect of improving activity and selectivity, simple process steps, and good economic effects

Inactive Publication Date: 2015-12-16
XIANGTAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The deactivated alumina ball should be replaced in time, if it is used for a long time, it will have a bad impact on the system
To sum up, there are many deficiencies in activated alumina balls as a regeneration agent: 1. Activated alumina balls can only regenerate part of the degraded products, and the regeneration of the degraded products is not thorough enough
2. Due to the insufficient mechanical strength of activated alumina balls, it is easy to pulverize in alkaline working fluid, which will increase the burden of alkali separation in the post-treatment process
3. When activated alumina balls are used for regeneration, the system often has the phenomenon of water and alkali, which will have a certain impact on production
However, when recycling waste alumina balls, the organic matter in the channels of the alumina ball is volatilized in a gaseous state, and these organic matter cannot be recycled, causing great pollution to the environment
[0013] Chinese patent CN101554996A proposes the use of a mixe

Method used

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  • Hydrogen peroxide working solution regenerant used in preparation of hydrogen peroxide process according to anthraquinone method and preparation method of hydrogen peroxide working solution regenerant
  • Hydrogen peroxide working solution regenerant used in preparation of hydrogen peroxide process according to anthraquinone method and preparation method of hydrogen peroxide working solution regenerant
  • Hydrogen peroxide working solution regenerant used in preparation of hydrogen peroxide process according to anthraquinone method and preparation method of hydrogen peroxide working solution regenerant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Take 1mL of the three-water working solution containing anthraquinone degradation products (provided by the hydrogen peroxide unit of Baling Branch of China Petroleum and Chemical Corporation), dilute it 100 times with n-hexane, and use Shimadzu LC-20A high performance liquid chromatography (Japan, Japan, Shimadzu Corporation) analyzes the composition of main substances and degradation products in the working solution (Agilent ZORBAXSIL column; mobile phase: n-hexane-dichloromethane-ethyl acetate (volume ratio is 80: 19: 0.5); flow rate: 1.0mL / min; Column temperature: 30°C; detection wavelength: 280nm; injection volume: 20μL). The analysis method adopts the area normalization method.

[0036] Such as figure 2 Shown, in the trihydrate working liquid normal phase chromatogram, the retention time of heavy aromatics is 3.649min and 3.945min, H 4 The retention times of EAQ and EAQ are 13.286min and 15.187min respectively, and the rest of the small impurity peaks are degrad...

Embodiment 2

[0041] Weigh 24.00g gamma crystalline alumina powder, 6.00g cubic crystal magnesia powder, 15g deionized water and 1.5g scallop powder, mix well, and then make strip-shaped regeneration with a diameter of 3mm through catalyst molding extrusion device After being dried in the shade at 25°C for 24h, it was dried at 125°C for 10h to obtain the regenerant.

[0042] Take 10g of the regenerant sample prepared above and 50mL of the three-water working solution containing anthraquinone degradation products and put them in a conical flask, put the conical flask in a constant temperature water bath shaker at 60°C for 6 hours, and take the working solution after the regeneration reaction 1mL, analyze the H in the working solution according to the method in Example 1 4 Changes in EAQ and EAQ content.

[0043] Check the regeneration performance of the regenerated catalyst in the anthraquinone working solution according to the above method, as image 3 As shown in the normal phase chromat...

Embodiment 3

[0048] Weigh 21.00g gamma crystalline alumina powder, 9.00g cubic crystal magnesia powder, 15g deionized water and 1.5g scallop powder, mix well, and then make strip-shaped regeneration with a diameter of 3mm through catalyst molding extrusion device After drying in the shade at 25°C for 24h, dry it at 125°C for 10h.

[0049] According to the method examination of embodiment 2, the regeneration performance of this regenerated catalyst in the anthraquinone working solution, as Figure 4 As shown in the normal phase chromatogram after the regeneration of hydrogen peroxide working solution, the results of the area normalization method of each component are shown in the table below, and the effective anthraquinone (H 4 EAQ+EAQ) content increased by 3.0511%.

[0050] Composition of main substances and degradation products in the working fluid after embodiment 3 regeneration

[0051]

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Abstract

The invention discloses a hydrogen peroxide working solution regenerant used in preparation of a hydrogen peroxide process according to an anthraquinone method and a preparation method of the hydrogen peroxide working solution regenerant. The regeneration effect of the hydrogen peroxide working solution regenerant is better than that of the conventional activated aluminum oxide anthraquinone degradation product regenerant used in the industry. Compared with the conventional regenerant, after regeneration, the quantity of effective anthraquinone is increased by 0.8 to 2.1 percent. During the preparation process, the reaction between magnesium oxide and water is very slow, the reaction product magnesium hydroxide is hard to dissolve in water, covers magnesium oxide to inhibit further reaction between magnesium oxide and water, and can properly improve the alkalinity of a working solution, while slight alkalinity provides convenience for improving the activity and the selectivity of a palladium catalyst, accelerating the speed of the hydrogenation, and avoiding a great amount of degradation. Meanwhile, the regenerant provided by the invention has favorable stability, is less susceptible to pulverization in the working solution, and low in adsorption of effective anthraquinone in the working solution; the preparation method is simple in process step, can be suitable for large-scale industrial production, and has a relatively high economical effect.

Description

technical field [0001] The invention relates to a working fluid regenerant in the process of preparing hydrogen peroxide by anthraquinone method and a preparation method thereof. Background technique [0002] Hydrogen peroxide is an important inorganic green chemical product, widely used in chemical industry, textile, papermaking, food, medicine, metallurgy, electronics, agriculture, military and environmental protection and other fields. With the rapid development of the global economy, the application fields of hydrogen peroxide continue to expand, the demand for hydrogen peroxide is increasing, and the quality requirements are also getting higher and higher. At present, the anthraquinone method has become the main production method of hydrogen peroxide in the world today with its relatively mature technology. The process uses 2-ethylanthraquinone as a carrier, dissolves it in a mixed solvent of heavy aromatic hydrocarbons and trioctyl phosphate, and prepares it as a work...

Claims

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Application Information

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IPC IPC(8): C01B15/023
CPCY02P20/584
Inventor 段正康张涛姚媛媛
Owner XIANGTAN UNIV
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