A hydrogen peroxide working fluid regenerant in the process of preparing hydrogen peroxide by anthraquinone method and its preparation method

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, easy pulverization and other problems, to achieve the effect of improving activity and selectivity, simple process steps and good stability

Inactive Publication Date: 2018-03-09
XIANGTAN UNIV
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  • Abstract
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  • 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 CN 101554996A proposes the use of a mixed regenerant of calcium oxide and silicon dioxide. The regenerant has a certain regeneration effect on the degraded product, but since the two substances are not mixed and formed, they are easily dispersed in the working fluid, causing the physical properties of the working fluid to deteriorate. change, detrimental to recycling
The content of alumina in the prepared regenerant is about 93% to 97%, the content of macropores above 75nm is more than 5%, the pore volume is more than 0.42ml / g, and the micro-diameter pore diameter is mainly concentrated in The process requires too much equipment, which increases the production cost
[0015] Chinese patent CN 103878021A proposes the use of alkylaniline as a catalyst for regeneration of anthraquinone degradation products. The catalyst mainly regenerates the degradation products produced in the partial hydrogenation stage, but this catalyst has fewer types of renewable degradation products and lower regeneration efficiency , and difficult to separate and recycle

Method used

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  • A hydrogen peroxide working fluid regenerant in the process of preparing hydrogen peroxide by anthraquinone method and its preparation method
  • A hydrogen peroxide working fluid regenerant in the process of preparing hydrogen peroxide by anthraquinone method and its preparation method
  • A hydrogen peroxide working fluid regenerant in the process of preparing hydrogen peroxide by anthraquinone method and its preparation method

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) to analyze the composition of main substances and degradation products in the working solution (Agilent ZORBAX SIL 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] like 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 degrada...

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 liquid regeneration agent in the process of preparing hydrogen peroxide by anthraquinone method and a preparation method thereof. The regeneration effect of the regeneration agent is better than that of the active alumina anthraquinone degradation product regeneration agent used in the traditional industry. After regeneration, compared with the existing regeneration agent, the effective anthraquinone increases by 0.8% to 2.1%. During the preparation process, the reaction between magnesium oxide and water proceeds very slowly, and the magnesium hydroxide produced by the reaction between the two is a substance that is insoluble in water, and it wraps on the surface of magnesium oxide, inhibiting the further reaction between magnesium oxide and water . The generated magnesium hydroxide can appropriately increase the alkalinity of the working fluid, and the slight alkalinity is conducive to improving the activity and selectivity of the palladium catalyst, increasing the speed of the hydrogenation reaction, and avoiding a large amount of degradation. At the same time, the regenerant has good stability, is not easy to pulverize in the working fluid, and reduces the adsorption of effective anthraquinone in the working fluid, and the preparation method has simple process steps, and is applicable to large-scale industrial production. economic 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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Patent Type & Authority Patents(China)
IPC IPC(8): C01B15/023
CPCY02P20/584
Inventor 段正康张涛姚媛媛
Owner XIANGTAN UNIV
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