Alkyl anthraquinone hydrogenation catalyst and preparation method thereof

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

CN106693958AActive Publication Date: 2017-05-24CHINA CATALYST HLDG CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Current Assignee / Owner
Publication Date
2017-05-24

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Abstract

The invention discloses an alkyl anthraquinone hydrogenation catalyst and a preparation method thereof. The alkyl anthraquinone hydrogenation catalyst is applied to a technology for producing hydrogen peroxide by an anthraquinone method. The alkyl anthraquinone hydrogenation catalyst is prepared from a catalyst carrier (a CNTs-TiO2 complex) and an active component (palladium atoms) by an equivalent-volume impregnation method, wherein in terms of the elementary palladium atoms, the active component accounts for 0.1-5% of the total weight of the alkyl anthraquinone hydrogenation catalyst; the CNTs-TiO2 complex is prepared from TiO2 and Ni(NO3)2 by a chemical vapor deposition method in the presence of a carbon source gas; the molar ratio of the TiO2 to the Ni(NO3)2 is (0.04-0.25): (0.015-0.2); CNTs accounts for 5-30% of the total weight of the CNTs-TiO2 complex. In the alkyl anthraquinone hydrogenation catalyst, the carrier CNTs-TiO2 complex has a relatively large external specific surface area, so that envelopment of the palladium atoms in the carrier can be effectively reduced, and thus the palladium atoms are fully utilized to improve the activity of the alkyl anthraquinone hydrogenation catalyst; meanwhile, the acidity of the CNTs-TiO2 complex is weaker than Al2O3, and under the action of the TiO2, occurrence of a degradation reaction in the reaction process can be effectively reduced, so that production of a degraded product in a working fluid is reduced. The alkyl anthraquinone hydrogenation catalyst has the characteristics of high hydrogenation efficiency, low anthraquinone degradation and the like in the process of producing the hydrogen peroxide by the anthraquinone method.
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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, anthraquinone method, isopropanol method and direct synthesis of hydrogen and oxygen, the anthraquinone method is still the main method of hydrogen peroxide production in the world. The technological process of the anthraquinone method mainly includes three processes of hydrogenation, oxidation and extraction, among 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 selection of the...

Examples

Embodiment 1

[0030] A kind of alkyl anthraquinone hydrogenation catalyst is prepared by following method:

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

[0032] A. Weigh 3g TiO 2 (0.0375mol) impregnated 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 supported Ni(NO 3 ) 2 TiO 2 Precursor;

[0033] B. Place the precursor obtained in step A in the constant temperature zone of the tube furnace, N 2 After the temperature rises to 450°C under the protective atmosphere (flow rate 20ml / min), the atmosphere is switched to N 2 / H 2 (N 2 with H 2 The volume ratio is 2:1, the total flow rate is 120ml / min); in N 2 / H 2 Restore in a mixed atmosphere for 50 minutes, keep the atmosphere unchanged and raise the temperature to 800°C, then switch the atmosphere to N 2 / C 2 h 2 (N 2 with C 2 h 2 The volume ratio is 2:1, the total flow rate is 120ml / min); in N 2 / C 2 h 2 After ...

Embodiment 2

[0039] A kind of alkyl anthraquinone hydrogenation catalyst is prepared by following method:

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

[0041] A. Weigh 5g TiO 2 (0.0626mol) impregnated 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 supported Ni(NO 3 ) 2 TiO 2 Precursor;

[0042] B. Place the precursor obtained in step A in the constant temperature zone of the tube furnace, N 2 Protective atmosphere (N 2 After the temperature rises to 450°C at a flow rate of 40ml / min), the atmosphere is switched to N 2 / H 2 (N 2 with H 2 The volume ratio is 2:1, the total flow rate is 150ml / min); in N 2 / H 2 Restore in a mixed atmosphere for 60 minutes, keep the atmosphere unchanged and raise the temperature to 800°C, then switch the atmosphere to N 2 / C 2 h 2 (N 2 with C 2 h 2 The volume ratio is 2:1, the total flow rate is 150ml / min); in N 2 / C 2 h 2 Af...

Embodiment 3

[0048] A kind of alkyl anthraquinone hydrogenation catalyst is prepared by following method:

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

[0050] A. Weigh 10g TiO 2 (0.1252mol) impregnated 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 supported Ni(NO 3 ) 2 TiO 2 Precursor;

[0051] B. Place the precursor obtained in step A in the constant temperature zone of the tube furnace, N 2 Protective atmosphere (N 2 After the temperature rises to 500°C at a flow rate of 40ml / min), the atmosphere is switched to N 2 / H 2 (N 2 with H 2 The volume ratio is 3:1, the total flow rate is 120ml / min); in N 2 / H 2 Restore in a mixed atmosphere for 40 minutes, keep the atmosphere unchanged and raise the temperature to 650°C, then switch the atmosphere to N 2 / C 2 h 2 (N 2 with C 2 h 2 The volume ratio is 3:1, the total flow rate is 120ml / min); in N 2 / C 2 h 2 Afte...