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High-activity nickel phosphide catalyst as well as preparation method and application thereof

A catalyst, nickel phosphide technology, applied in the field of catalysis, can solve the problems of expensive organic compounds, unsuitable for large-scale synthesis of metal phosphide, complex and other problems, and achieve the effects of overcoming unstable crystal phase, increasing quantity, and overcoming poor quality

Inactive Publication Date: 2018-07-13
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the liquid synthesis method is complex and generally requires the use of expensive organic compounds, so it is not suitable for large-scale synthesis of metal phosphides

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) 29.7g Ni(NO 3 ) 2 ·6H 2 O, 23g TiCl 4 -Ethanol (0.3g / g) solution was dissolved in 100ml deionized water to form Ni(NO 3 ) 2 and TiCl 4 - mixed solution of ethanol;

[0036] (2) 5.2g Na 2 SiO 3 9H 2 O and 18.2 g anhydrous Na 2 CO 3 Dissolve in 100ml deionized water to form a mixed solution of sodium silicate and sodium carbonate;

[0037] (3) Slowly drop the above two solutions into 200ml deionized water at the same time in a water bath at 80°C, and stir vigorously for 1 hour to form a green precipitate;

[0038] (4) Suction filter the precipitate obtained in step (3), the pH value of the obtained filtrate after suction filtration is 8-9, fully wash the precipitate with deionized water to neutrality and thoroughly wash away the chloride ions in the solution, add the precipitate to into 200ml of n-butanol, evaporated in a water bath at 80°C for 12h, and then dried in an oven at 120°C for 12h to obtain Ni / SiO 2 -TiO 2 (n Si / n Ti =0.5) the precursor of...

Embodiment 2

[0041] (1) 29.7g Ni(NO 3 ) 2 ·6H 2 O, 18.1g TiCl 4 -Ethanol (0.3g / g) solution was dissolved in 100ml deionized water to form Ni(NO 3 ) 2 and TiCl 4 - mixed solution of ethanol;

[0042] (2) 8.1g Na 2 SiO 3 9H 2 O and 15.3 g anhydrous Na 2 CO 3 Dissolve in 100ml deionized water to form a mixed solution of sodium silicate and sodium carbonate;

[0043] (3) Slowly drop the above two solutions into 200ml deionized water at the same time in a water bath at 80°C, and stir vigorously for 1 hour to form a green precipitate;

[0044] (4) Suction filter the precipitate obtained in step (3), the pH value of the obtained filtrate after suction filtration is 8-9, fully wash the precipitate with deionized water to neutrality and thoroughly wash away the chloride ions in the solution, add the precipitate to into 200ml of n-butanol, evaporated in a water bath at 80°C for 12h, and then dried in an oven at 120°C for 12h to obtain Ni / SiO 2 -TiO 2 (n Si / n Ti =1) the precursor of...

Embodiment 3

[0047] (1) 29.7g Ni(NO 3 ) 2 ·6H 2 O, 13g TiCl 4 -Ethanol (0.3g / g) solution was dissolved in 100ml deionized water to form Ni(NO 3 ) 2 and TiCl 4 - mixed solution of ethanol;

[0048] (2) 11.4g Na 2 SiO 3 9H 2 O and 11.9 g anhydrous Na 2 CO 3 Dissolve in 100ml deionized water to form a mixed solution of sodium silicate and sodium carbonate;

[0049] (3) The above two solutions were slowly added dropwise to 200ml deionized water at the same time in a water bath at 80°C, and stirred vigorously for 1 hour to form a green precipitate.

[0050] (4) Suction filter the precipitate obtained in step (3), the pH value of the obtained filtrate after suction filtration is 8-9, fully wash the precipitate with deionized water to neutrality and thoroughly wash away the chloride ions in the solution, add the precipitate to into 200ml of n-butanol, evaporated in a water bath at 80°C for 12h, and then dried in an oven at 120°C for 12h to obtain Ni / SiO 2 -TiO 2 (n Si / n Ti =2) th...

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Abstract

The invention provides a high-activity nickel phosphide as well as a preparation method and application thereof. The preparation method is characterized in that a high-load-capacity Ni / SiO2-TiO2 catalyst adopting an SiO2-TiO2 compound oxide as a catalyst carrier is prepared according to a coprecipitation method; then a high-activity Ni2P / SiO2-TiO2 catalyst is prepared according to a triphenylphosphine liquid phase phosphating method; nickel phosphide is used as the active component. According to the method, the Ni / SiO2-TiO2 catalyst is pre-reduced to form highly-dispersed nano nickel particlesbefore being phosphatized, so that Ni / SiO2-TiO2 is easily phosphatized by PPh3 in the liquid phase under low temperature, and as a result, the highly-dispersed Ni2P particles can be produced. Test results show that the catalyst is high in activity for o-methoxyphenol and high in selectivity to cyclohexane.

Description

technical field [0001] The invention belongs to the technical field of catalysis, and in particular relates to the preparation of a catalyst for catalyzing the selective hydrodeoxygenation of o-methoxyphenol. Background technique [0002] Fossil energy reserves are limited and non-renewable. At the same time, a large amount of greenhouse gases and polluting smoke will be released while consuming fossil energy, which has triggered environmental and ecological crises on a global scale. In order to get rid of the excessive dependence on fossil energy, alternative energy must be sought to alleviate the energy crisis. Biomass energy has become the first choice to replace fossil energy because of its wide range of raw materials, easy availability, and direct conversion into liquid fuels. However, due to the complex structure of biomass and the arbitrariness of breaking bonds in the degradation process, there are many kinds of oxygenated compounds in biomass oil, so the oxygen con...

Claims

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Application Information

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IPC IPC(8): B01J27/185B01J37/02B01J37/03B01J37/28C07C1/20C07C13/18
CPCC07C1/20B01J27/1853B01J37/0236B01J37/03B01J37/28B01J35/393C07C13/18
Inventor 鲁墨弘孙雨吉新李明时
Owner CHANGZHOU UNIV
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