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Micro-nano copper and ruthenium composite phosphide catalyst, and preparation method and application thereof

A phosphide and catalyst technology, which is applied in the field of micro-nano copper ruthenium composite phosphide catalyst and its preparation, can solve the problems of complex preparation process, low loading amount, unstable structure in the reaction process and the like, and achieves simple preparation method and high activity. Single component, the effect of promoting synergistic effect

Inactive Publication Date: 2020-02-25
SHANGHAI NAT ENG RES CENT FORNANOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of the shortcomings of current single-atom / monodisperse catalysts, such as relatively low loading capacity, complicated preparation process, or insufficiently stable structure in the reaction process, the purpose of the present invention is to provide a micro-nano monodisperse copper-ruthenium composite phosphide catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A micro-nano copper ruthenium composite phosphide catalyst, by adjusting the pH of the solution, controlling the electronegativity of the carrier surface, and forming a weak repulsion with the target copper ruthenium ions; the weak repulsion ensures that all the copper ruthenium enters into the ion exchange process. In the carrier lattice, and achieve uniform monodispersion; ultrasonic treatment removes possible weakly adsorbed copper ruthenium ions on the surface; then under specific conditions, the monodisperse copper ruthenium composite phosphide catalyst is formed in situ through the temperature-programmed reduction method; optimize the ratio of copper ruthenium to promote The synergistic effect between the two is prepared according to the following steps:

[0025] Preparation of hydroxyapatite carrier: Weigh 0.05mol of calcium nitrate and 0.03mol of diammonium hydrogen phosphate and dissolve them in 100mL and 100mL of deionized water respectively; Mixing; under the...

Embodiment 2

[0028] A kind of micronano copper ruthenium composite phosphide catalyst, prepared according to the following steps:

[0029] Preparation of hydroxyapatite carrier: Weigh 0.05mol of calcium nitrate and 0.03mol of diammonium hydrogen phosphate and dissolve them in 150mL and 150mL of deionized water respectively; Mixing; under the condition of stirring, ammonia water condition pH=12, react in water bath at 90°C for 4 hours, stand and age for 18 hours; filter, wash with deionized water, and freeze-dry to obtain hydroxyapatite carrier;

[0030] Preparation of micronano copper ruthenium composite phosphide catalyst: prepare 70 mL of a mixed solution with a copper chloride concentration of 10 mmol / L and a ruthenium chloride concentration of 5 mmol / L, and adjust the mixed solution with a ruthenium-copper molar ratio of 1:2 to pH =7 or so; add 1.5g of hydroxyapatite for ion exchange, stir at room temperature for 3 hours; re-disperse in aqueous solution after centrifugation and sonicat...

Embodiment 3

[0032] A kind of micronano copper ruthenium composite phosphide catalyst, prepared according to the following steps:

[0033] Preparation of hydroxyapatite carrier: Weigh 0.05mol of calcium nitrate and 0.03mol of diammonium hydrogen phosphate and dissolve them in 100mL and 150mL of deionized water respectively; Mixing; pH=10 in ammonia water under stirring condition, reacting in a water bath at 60°C for 6 hours, standing and aging for 18 hours; filtering, washing with deionized water, and freeze-drying to obtain hydroxyapatite carrier.

[0034] Preparation of micro-nano copper ruthenium composite phosphide catalyst: prepare 70mL of mixed solution with copper chloride concentration of 10mmol / L and ruthenium chloride concentration of 10mmol / L, adjust the ruthenium copper molar ratio to 1:1 mixed solution with ammonia water to pH = 7 or so; add 1.5g of hydroxyapatite for ion exchange, stir at room temperature for 5 hours; redisperse in aqueous solution after centrifugation and ul...

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Abstract

The invention discloses a micro-nano copper and ruthenium composite phosphide catalyst, and a preparation method and an application thereof. The micro-nano copper and ruthenium composite phosphide catalyst takes hydroxyapatite as a carrier and copper and ruthenium composite phosphide as an active component, and the copper and ruthenium composite phosphide is highly dispersed on the surface of thehydroxyapatite. The electronegativity of the surface of the carrier is controlled by adjusting the pH value of a solution in order to make the carrier and target copper and ruthenium ions form weak repulsive action; copper and ruthenium completely enter crystal lattices of the carrier in the ion exchange process, and uniform and single dispersion is achieved; possible copper and ruthenium ions weakly adsorbed on the surface are removed through ultrasonic treatment; and then the monodisperse copper and ruthenium composite phosphide catalyst is formed in situ through a programmed heating reduction technology under specific conditions. The obtained micro-nano copper and ruthenium composite phosphide catalyst has the characteristics of high loading capacity, uniform dispersion, single active component and the like. The preparation method has the advantages of simplicity, easiness in large-scale production, and excellent application prospect.

Description

technical field [0001] The invention relates to a micro-nano preparation method of a monodisperse catalyst, in particular to a micro-nano copper-ruthenium composite phosphide catalyst and its preparation method and application. Background technique [0002] Nanocatalysts can expose more low-coordination highly active sites on the surface, and exhibit excellent catalytic performance different from conventional materials. However, nanocatalysts prepared by traditional methods are usually difficult to obtain uniform active components, which are specifically manifested in: the particle size of the active components is mixed from a dozen nanometers to several nanometers, or even sub-nanometer clusters; A variety of mixed valence exists, etc. This not only leads to unfavorable results such as poor controllability of the catalyst, low selectivity of the target reaction, and excessive side reactions, but also reduces the utilization rate of the active components. [0003] The unif...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/185C07C273/18C07C275/06
CPCB01J27/1856C07C273/1809C07C275/06
Inventor 崔大祥赵昆峰童琴蔡婷袁静金彩虹
Owner SHANGHAI NAT ENG RES CENT FORNANOTECH
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