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Transition metal nanoparticle catalyst with dual confinement structure as well as application thereof to catalysis of selective hydrogenation reaction of dimethyl terephthalate

A technology of dimethyl phthalate and transition metals, which is applied in the field of transition metal nanoparticle catalysts, can solve the problems of reduced Ni metal reduction, large active metal nanoparticles, and difficult oxide reduction, so as to prevent sintering and Loss of transition metals, strong interaction, and outstanding reaction stability

Inactive Publication Date: 2016-09-28
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, on the basis of such materials, the active metal nanoparticles prepared by heat treatment in a reducing atmosphere are relatively large, the interaction force between the metal and the substrate is weak, and the reactivity is still limited.
And in the reduction process, the reduction of oxides is difficult, and the reduction degree of Ni metal will decrease

Method used

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  • Transition metal nanoparticle catalyst with dual confinement structure as well as application thereof to catalysis of selective hydrogenation reaction of dimethyl terephthalate
  • Transition metal nanoparticle catalyst with dual confinement structure as well as application thereof to catalysis of selective hydrogenation reaction of dimethyl terephthalate
  • Transition metal nanoparticle catalyst with dual confinement structure as well as application thereof to catalysis of selective hydrogenation reaction of dimethyl terephthalate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A. Add 19.2g of Ni(NO 3 ) 2 ·6H 2 O, 12.4g of Al(NO 3 ) 2 9H 2 O was added to 150mL deionized water, and ultrasonically dissolved to obtain a mixed salt solution; 6.3g of sodium hydroxide and 7.0g of sodium carbonate were added to 150mL of deionized water, and ultrasonically dissolved to obtain a mixed alkali solution; 150mL of deionized water was put into 500mL In the three-necked flask, then gradually drop the mixed alkali solution to pH 10, then drop the mixed salt solution simultaneously to keep the pH at 10; Crystallize at 130°C for 24h, filter, wash with deionized water and filter to pH 7, and finally dry at 70°C for 24h to obtain a highly dispersed hydrotalcite precursor, denoted as Ni 2 Al-LDHs (XRD, FT-IR, TG-DTA spectra and SEM images see figure 1 );

[0022] B. The highly dispersed hydrotalcite precursor Ni prepared in step A 2 Al-LDHs is placed in a high-temperature atmosphere furnace, and H with a purity of 99.999% is introduced 2 , the flow rate i...

Embodiment 2

[0026]Place the hydrotalcite precursor prepared in step A in Example 1 in a muffle furnace, air roast, raise the temperature in the furnace to 400°C, the heating rate is 5°C / min, keep it for 5h, and then naturally cool to room temperature; after taking it out Then place it in a high-temperature atmosphere furnace and feed H2 with a purity of 99.999%. 2 , the flow rate is 60mL / min, the temperature in the furnace is raised to 400°C and 600°C respectively, the heating rate is 5°C / min, keep for 5h, and then naturally cooled to room temperature, the transition metal nanoparticle catalysts with double confinement structure are obtained respectively denoted as Ni / NiAlO x / AlO x (C400R400) and Ni / NiAlO x / AlO x (C400R600) sample (XRD figure see figure 2 ).

[0027] The transition metal nanoparticle catalyst with a double confinement structure prepared above has a composition structure: nickel nanoparticles are confined in an aluminum-doped nickel oxide shell, and the outermost p...

Embodiment 3

[0032] A. Add 19.2g of Co(NO 3 ) 2 ·6H 2 O, 12.4g of Al(NO 3 ) 2 9H 2 O was added to 150mL deionized water, and ultrasonically dissolved to obtain a mixed salt solution; 6.3g of sodium hydroxide and 7.0g of sodium carbonate were added to 150mL of deionized water, and ultrasonically dissolved to obtain a mixed alkali solution; 150mL of deionized water was put into 500mL In the three-necked flask, then gradually drop the mixed alkali solution to pH 10, then drop the mixed salt solution simultaneously to keep the pH at 10; Crystallized at 130 °C for 24 h, filtered, washed with deionized water and filtered to pH 7, and finally dried at 70 °C for 24 h to obtain a highly dispersed hydrotalcite precursor, denoted as Co 2 Al-LDHs;

[0033] B. The highly dispersed hydrotalcite precursor Co prepared in step A 2 Al-LDHs is placed in a high-temperature atmosphere furnace, and H with a purity of 99.999% is introduced 2 , the flow rate is 60mL / min, the temperature in the furnace is ...

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Abstract

The invention discloses a method for preparing a transition metal nanoparticle catalyst with a dual confinement structure as well as an application thereof to catalysis of a selective hydrogenation reaction of dimethyl terephthalate. Firstly, a laminate of a hydrotalcite-like precursor containing transition metal and aluminium ions is synthesized, and then the transition metal nanoparticle catalyst with the dual confinement structure is prepared by reduction. The catalyst structure has the characteristics that transition metal nanoparticles are embedded in dual shells including an aluminium doped transition metal oxide shell and an amorphous aluminum oxide shell in order, and the dual confinement structure containing nanometer metal particles is formed. The structure with two oxide shells is used, so that transition metal is dispersed uniformly, mutual effects between the transition metal and a carrier are strong, sintering and loss of transition metal are prevented, and active sites of reaction are provided for reactants. The catalyst improves conversion rate of dimethyl terephthalate, and selectivity and reaction stability of dimethyl 1,4-cyclohexanedicarboxylate are substantially improved.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, and particularly relates to the controlled reduction of a hydrotalcite-like precursor to prepare a transition metal with metal nanoparticles embedded in a double shell of metal oxide and amorphous alumina in sequence to form a double confinement structure. Nanoparticle catalyst and its application in catalyzing the selective hydrogenation of dimethyl terephthalate. Background technique [0002] Industrially, the hydrogenation of dimethyl terephthalate to prepare dimethyl 1,4-cyclohexanedicarboxylate mainly uses supported noble metal Pd, Ru or Rh-based catalysts. However, noble metal catalysts have high hydrogenation activity and selectivity, but their process conditions are relatively harsh, and their prices are relatively expensive, which is not conducive to the further development of industrialization. Therefore, most of the current research focuses on the use of non-noble metals,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755B01J23/75B01J23/72B01J23/745B82Y30/00B82Y40/00C07C69/75C07C67/303
CPCB01J23/002B01J23/72B01J23/745B01J23/75B01J23/755B82Y30/00B82Y40/00C07C67/303B01J35/396B01J35/40C07C69/75
Inventor 张法智樊启宁李雪锋
Owner BEIJING UNIV OF CHEM TECH
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