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A kind of hydrogenation catalyst and its preparation method and application

A hydrogenation catalyst and catalyst technology, which are applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve the problems of less application in the field of hydrogenation catalysis, and are beneficial to deep hydrogenation, reducing agglomeration, increasing Active and selective effects

Active Publication Date: 2020-08-11
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since graphene was first prepared by the GEIM group in 2014 by mechanical exfoliation, it has been widely used in photocatalysis, electrochemical catalysis, fuel cells and other fields due to its excellent performance, but it has less application in the field of hydrogenation catalysis.

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  • A kind of hydrogenation catalyst and its preparation method and application
  • A kind of hydrogenation catalyst and its preparation method and application

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preparation example Construction

[0023] The technical purpose of the first aspect of the present invention provides a kind of preparation method of hydrogenation catalyst, comprises the following steps:

[0024] The first step, preparation of composite oxide: dissolve copper salt and manganese salt in water, add TiO 2 , ultrasonication, stirring, and evaporating the mixture to dryness in a water bath, drying, and roasting to obtain a composite oxide; the molar ratio of each substance in Cu, Mn and Ti is 1:0.2~1:6~20;

[0025] The second step, graphene oxide-loaded composite oxide: ultrasonically disperse graphene oxide into the alcohol solution, stir, then add the composite oxide in the first step, transfer to a closed reaction kettle, and conduct hydrothermal treatment at 150~250°C. Cool, filter, wash and dry to obtain the catalyst.

[0026] In the above preparation method, as a preferred technical solution, the copper salt and manganese salt described in the first step are water-soluble salts that do not c...

Embodiment 1

[0046] Catalyst preparation:

[0047] (1) The first step, the preparation of composite oxide: 20.1g Cu(NO 3 ) 2 ·3H 2 O and 12.5g Mn(NO 3 ) 2 4H 2 O mixed, dissolved in 200mL water to form a solution, to which 80.0g TiO 2 , sonicated for 0.5h, stirred to obtain a homogeneous slurry, evaporated to dryness in a constant temperature water bath, then dried in an oven at 100°C, and finally placed in a muffle furnace at 350°C for 8h to obtain Cu, Mn and Ti composite oxide Y1.

[0048] (2) The second step, graphene oxide-loaded composite oxide: use natural graphite as raw material to prepare graphene oxide by Hummers' method, take 1.0g of graphene oxide and disperse it in 1L of absolute ethanol by ultrasonication for 0.5h, and then take 70g of graphene oxide The composite oxide prepared in one step was added to the above suspension, transferred to a polytetrafluoroethylene-sealed autoclave, placed in a 180°C oven for hydrothermal treatment for 8 hours, cooled, filtered and was...

Embodiment 2

[0049] Embodiment 2 (preparation of catalyst C2)

[0050] (1) The first step, the preparation of composite oxide: 24.2g Cu(NO 3 ) 2 ·3H 2 O and 7.53g Mn(NO 3 ) 2 4H 2 O mixed, dissolved in 200mL water to form a solution, to which 80.0g TiO 2 , sonicated for 0.5h, stirred to obtain a homogeneous slurry, evaporated to dryness in a constant temperature water bath, then dried in an oven at 100°C, and finally placed in a muffle furnace at 450°C for 6h to obtain Cu, Mn and Ti composite oxide Y2.

[0051] (2) The second step, graphene oxide-loaded composite oxide: use natural graphite as raw material to prepare graphene oxide by Hummers' method, take 2.1g of graphene oxide and disperse it in 1L of absolute ethanol by ultrasonication for 0.5h, and then take 70g of graphene oxide Add the composite oxide prepared in one step to the above suspension, transfer to a polytetrafluoroethylene sealed autoclave, place the autoclave in a 180°C oven for hydrothermal treatment for 8 hours, ...

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Abstract

The invention relates to a hydrogenation catalyst, and a preparation method and application thereof. The catalyst is prepared by the following steps: uniformly mixing a copper salt, a manganese salt and TiO2, carrying out drying by distillation with a water bath, carrying out drying and roasting to obtain a composite oxide, ultrasonically dispersing graphene oxide into an alcohol solution, addinga composite oxide, and carrying out water heat treatment, cooling, filtering, washing and drying to obtain the catalyst. The catalyst can be used for catalyzing the reaction for preparing 1,4-butanediol by using maleic anhydride or an ester of the maleic anhydride. Graphene exists in the catalyst provided by the invention, so that the dispersion degree and the particle size of an active componentCu<0>, and the temperature and pressure required by the action of the catalyst are effectively reduced. Through the synergistic effect of the graphene, the TiO2 and the active component, the deep hydrogenation of the maleic anhydride or the ester of the maleic anhydride can be catalyzed, and the selectivity of the 1,4-butanediol is improved. The conversion rate of the maleic anhydride or the esterof the maleic anhydride can reach 98.7%, the selectivity of the 1,4-butanediol can be up to 87.2%, and compared with the selectivity without supported graphene, the selectivity is increased by 24.3%.

Description

technical field [0001] The invention relates to a hydrogenation catalyst and its preparation method and application, in particular to a catalyst for catalyzing the hydrogenation of maleic anhydride or its ester to prepare 1,4-butanediol. Background technique [0002] 1,4-Butanediol (1,4-BDO) is an important basic organic chemical and fine chemical raw material, mainly used in the fields of chemical industry, medicine, textile and daily chemical industry. -With the increasing demand for polyurethane and polybutylene terephthalate (PBT) fibers and engineering plastics synthesized from BDO, the demand for 1,4-BDO is also gradually increasing. Maleic anhydride or its ester (MA) is hydrogenated to 1,4-BDO in the liquid phase. The reaction conditions are mild, relatively easy to control, and low in investment. Tetrahydrofuran (THF) and gamma - Butyrolactone (GBL). However, the process of preparing 1,4-BDO requires a catalyst capable of deep hydrogenation. The commonly used coppe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/889C07C29/154C07C31/20
CPCB01J23/002B01J23/8892B01J2523/00C07C29/154B01J2523/17B01J2523/47B01J2523/72C07C31/207Y02P20/52
Inventor 孙启梅王崇辉王领民高大成张霖樊亚超姚新武
Owner CHINA PETROLEUM & CHEM CORP