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A kind of alkyl anthraquinone hydrogenation catalyst and preparation method thereof

A hydrogenation catalyst and alkyl anthraquinone technology, applied in the chemical industry, can solve the problems of affecting solubility, viscosity of working fluid, increase of degradation products, etc., so as to reduce the generation of degradation products, reduce the occurrence of degradation reactions, and improve catalyst activity. Effect

Active Publication Date: 2019-04-09
CHINA CATALYST HLDG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the activity and selectivity of the palladium catalyst used are a pair of contradictory factors. If the activity of the catalyst is too low, it will affect the production capacity of hydrogen peroxide in the production enterprise. If the activity of the catalyst used is too high, the actual production process will often be due to Excessive hydrogenation leads to deterioration of the working condition of the working fluid system and increased degradation products
These degradation products not only affect the hydrogenation efficiency of the working fluid (the yield of hydrogen peroxide), but also affect the solubility of anthraquinone and hydroanthraquinone in the working fluid, resulting in the viscosity of the working fluid or the precipitation of anthraquinone, which is not conducive to the separation and maintenance of catalysts. Reuse of working fluid

Method used

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  • A kind of alkyl anthraquinone hydrogenation catalyst and preparation method thereof
  • A kind of alkyl anthraquinone hydrogenation catalyst and preparation method thereof
  • A kind of alkyl anthraquinone hydrogenation catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] An alkyl anthraquinone hydrogenation catalyst is prepared by the following method:

[0031] (1) Preparation of CNTs-TiO by chemical vapor deposition 2 Complex:

[0032] A. Weigh 3g TiO 2 (0.0375mol) immersed in 15ml 2mol / L Ni(NO 3 ) 2 (0.03mol) aqueous solution, stirred at room temperature for 15h, and dried at 105°C for 12h to obtain the supported Ni(NO 3 ) 2 TiO 2 Precursor;

[0033] B, the precursor obtained in step A is placed in the constant temperature zone of the tube furnace, N 2 After heating to 450°C under protective atmosphere (flow rate 20ml / min), the atmosphere was switched to N 2 / H 2 (N 2 with H 2 The volume ratio is 2:1, and the total flow is 120ml / min); in N 2 / H 2 Reduction in mixed atmosphere for 50min, keeping the atmosphere unchanged and heating up to 800℃, then switching the atmosphere to N 2 / C 2 H 2 (N 2 with C 2 H 2 The volume ratio is 2:1, and the total flow is 120ml / min); in N 2 / C 2 H 2 After 20 min of reaction in a mixe...

Embodiment 2

[0039] An alkyl anthraquinone hydrogenation catalyst is prepared by the following method:

[0040] (1) Preparation of CNTs-TiO by chemical vapor deposition 2 Complex:

[0041] A. Weigh 5g TiO 2 (0.0626mol) immersed in 25ml 3mol / L Ni(NO 3 ) 2 (0.075mol) aqueous solution, stirred at room temperature for 12h, and dried at 105°C for 12h to obtain the supported Ni(NO 3 ) 2 TiO 2 Precursor;

[0042] B, the precursor obtained in step A is placed in the constant temperature zone of the tube furnace, N 2 Protective atmosphere (N 2 After heating to 450°C at a flow rate of 40ml / min), the atmosphere was switched to N 2 / H 2 (N 2 with H 2 The volume ratio is 2:1, and the total flow is 150ml / min); in N 2 / H 2 Reduction in a mixed atmosphere for 60 min, keeping the atmosphere unchanged and heating up to 800 °C, then switching the atmosphere to N 2 / C 2 H 2 (N 2 with C 2 H 2 The volume ratio is 2:1, and the total flow is 150ml / min); in N 2 / C 2 H 2 After 15 min of react...

Embodiment 3

[0048] An alkyl anthraquinone hydrogenation catalyst is prepared by the following method:

[0049] (1) Preparation of CNTs-TiO by chemical vapor deposition 2 Complex:

[0050] A. Weigh 10g TiO 2 (0.1252mol) immersed in 50ml 4mol / L Ni(NO 3 ) 2 (0.2mol) aqueous solution, stirred at room temperature for 20h, and dried at 105°C for 15h to obtain the supported Ni(NO 3 ) 2 TiO 2 Precursor;

[0051] B, the precursor obtained in step A is placed in the constant temperature zone of the tube furnace, N 2 Protective atmosphere (N 2 After heating to 500°C at a flow rate of 40ml / min), the atmosphere was switched to N 2 / H 2 (N 2 with H 2 The volume ratio is 3:1, and the total flow is 120ml / min); in N 2 / H 2 Reduction in mixed atmosphere for 40min, keeping the atmosphere unchanged and heating up to 650℃, then switching the atmosphere to N 2 / C 2 H 2 (N 2 with C 2 H 2 The volume ratio is 3:1, and the total flow is 120ml / min); in N 2 / C 2 H 2 After 10 min of reaction in ...

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Abstract

The invention discloses an alkyl anthraquinone hydrogenation catalyst and a preparation method thereof, which are used in the process of producing hydrogen peroxide by an anthraquinone method; the catalyst consists of a catalyst carrier (CNTs-TiO 2 Composite) and active components (palladium atoms) are prepared by an equal volume impregnation method, and the active components account for 0.1 to 5% of the total weight of the catalyst in terms of palladium atoms; CNTs‑TiO 2 Composite made of TiO 2 and Ni(NO 3 ) 2 Prepared by chemical vapor deposition in the presence of carbon source gas, TiO 2 with Ni(NO 3 ) 2 The molar ratio of 0.04~0.25:0.015~0.2, CNTs accounts for CNTs‑TiO 2 5-30% of the total weight of the compound. Catalyst of the present invention, carrier CNTs-TiO 2 The complex has a large external specific surface area, which can effectively reduce the occlusion of palladium atoms in the support, make full use of palladium atoms, and improve the catalyst activity; at the same time, CNTs‑TiO 2 The acidity ratio of the complex to Al 2 O 3 weak, and the TiO 2 Under the action, it can effectively reduce the occurrence of degradation reactions in the reaction process and reduce the generation of degradation products in the working fluid. The catalyst is used in the process of producing hydrogen peroxide by the anthraquinone method and has the characteristics of high hydrogenation efficiency, less degradation of anthraquinone, and the like.

Description

technical field [0001] The invention relates to an alkyl anthraquinone hydrogenation catalyst and a preparation method thereof, belonging to the technical field of chemical industry. Background technique [0002] Hydrogen peroxide is a green chemical product, which is widely used in textile, chemical, paper, military, environmental protection, electronics, medicine, food, mining, construction and other industries. Although the production methods of hydrogen peroxide include electrolysis method, anthraquinone method, isopropanol method and direct hydrogen-oxygen synthesis method, the anthraquinone method is still the main method for the production of hydrogen peroxide in the world at present. The process flow of the anthraquinone method mainly includes three processes of hydrogenation, oxidation and extraction, of which the hydrogenation process is the core of the whole process. The anthraquinone method mostly uses supported palladium catalysts, and one of the keys is the ch...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/44C01B15/023
Inventor 李进李永宾段江波王建青孙红影张恩锋
Owner CHINA CATALYST HLDG CO LTD
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