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Nano-Ni catalyst packed by resorcinarenes and preparation method thereof

A technology of calixarene and nano-nickel is applied in the field of meta-calixarene cladding nano-nickel particle catalyst and its preparation field, which can solve the problems of irregular shape of nano-particles, poor particle dispersibility, complicated catalytic process and the like, and achieve good dispersion performance. , good solubility and high cracking efficiency

Inactive Publication Date: 2011-11-23
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Because the liquid-phase chemical reduction method has the characteristics of simple equipment and convenient operation, it is mostly prepared by this method, but the nanoparticles obtained by the liquid-phase chemical reduction method are often irregular in shape, large in particle size distribution, and relatively serious in agglomeration. bad sex
When it is used in the field of heterogeneous catalysis, the catalytic process is more complicated, which limits its application in some specific research fields, such as advanced

Method used

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  • Nano-Ni catalyst packed by resorcinarenes and preparation method thereof
  • Nano-Ni catalyst packed by resorcinarenes and preparation method thereof
  • Nano-Ni catalyst packed by resorcinarenes and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Dissolve 12.8g resorcinol and 21.4g laurylaldehyde in 115ml ethanol solution under stirring condition, add concentrated hydrochloric acid 18.5ml at 0 ℃, N 2 Under protection, the temperature was raised to 70 ° C for 10 hours, and then cooled to room temperature to obtain a yellow precipitate, which was filtered and washed with a large amount of water. After drying, methanol was recrystallized twice, and then recrystallized twice with n-hexane / acetone, and vacuum-dried to obtain Product 2,8,14,20-Tetrakis(undecyl)calix[4]resorcinolarene.

[0037] Take 2mmol nickel chloride (NiCl 2 ·6H 2 O) Dissolve in ethanol solution, ultrasonically disperse for 5min, prepare ethanol solution with nickel chloride concentration of 0.1mol / L, add a certain amount of 2,8,14,20-tetra (Undecyl) calix [4] resorcinol arene, stir and be heated to 50 ℃ and make it dissolve completely, add the sodium hydroxide aqueous solution of 0.8mol / L subsequently and adjust the solution pH to reach 10, add ...

Embodiment 2

[0042] 2,8,14,20-Tetrakis(undecyl)calix[4]resorcinolarene was prepared in the same manner as in Example 1.

[0043] Take 2mmol nickel nitrate (Ni(NO 3 ) 2 ·6H 2 O) be dissolved in ethanol solution, ultrasonic dispersion 5min, preparation nickel nitrate concentration is the ethanol solution of 0.1mol / L, add a certain amount of 2,8,14,20-tetra( Undecyl)calix[4]resorcinol aromatics, heated to 60°C while stirring to make it dissolve completely, then added 0.8mol / L aqueous sodium hydroxide solution to adjust the pH of the solution to 11, added 5ml 85wt% hydrazine hydrate Reduction was carried out, and the reaction was stopped after 0.5 hours. The obtained nano-nickel particles were centrifuged, washed three times with 30 ml of distilled water, washed three times with 30 ml of absolute ethanol, and vacuum-dried at 40° C. to obtain a metacalixarene inclusion nano-nickel catalyst. The particle size of the product is 30nm, and the crystal system is the same as that of Example 1. Th...

Embodiment 3

[0045] 2,8,14,20-Tetrakis(undecyl)calix[4]resorcinolarene was prepared in the same manner as in Example 1.

[0046] Take 2mmol nickel chloride (NiCl 2 ·6H 2 O) Dissolve in ethanol solution, ultrasonically disperse for 5min, prepare ethanol solution with nickel chloride concentration of 0.1mol / L, add a certain amount of 2,8,14,20-tetra (Undecyl)calix[4]resorcinol aromatics, heated to 60°C while stirring to make it dissolve completely, then added 1.0mol / L aqueous sodium hydroxide solution to adjust the pH of the solution to 10, added 5ml of 85wt% hydrated Hydrazine was reduced, and the reaction was stopped after 0.5 hours. The obtained nano-nickel particles were centrifuged, washed three times with 30 ml of distilled water, washed three times with 30 ml of absolute ethanol, and vacuum-dried at 40° C. to obtain a metacalixarene clathrate nano-nickel catalyst. The product sample also has high catalytic activity to the cracking reaction of JP-10.

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Abstract

The invention provides a nano-Ni catalyst packed by resorcinarenes and a preparation method thereof, wherein resorcinarenes is used as main body, soluble nickel salt is used as nickel source, hydrazine hydrate is used as reductant, and the liquid phase reduction method is adopted to prepare nano-Ni particles packed by resorcinarenes. The catalyst can be dispersed in decahydronaphthalene, JP-10 and other cyclane uniformly to realize a catalytic cracking reaction under the pseudo-homogeneous condition; and in the range of the experimental temperature, the cracking conversion ratio can be increased by up to 50%. The catalyst has the advantages of high catalytic activity, low cost and the like and particularly has market application prospect.

Description

technical field [0001] The invention belongs to the field of nanometer catalysis, and in particular relates to a metacalixarene clathrate nano-nickel particle catalyst for catalyzing the dehydrogenation and cracking of naphthenes and a preparation method thereof. Background technique [0002] In recent years, as a new type of catalytic material with high activity and high selectivity, metal nanoparticles have been widely used in catalytic oxidation, reduction, cracking reactions and photocatalysis. Due to their high catalytic activity, selectivity and stability, nanoscale precious metal catalysts are widely used in hydrogenation, dehydrogenation, oxidation, reduction and other reactions, and play an important role in chemical industry, petroleum refining, petrochemical and other fields. However, due to the scarcity and high price of precious metal resources, people began to study and develop non-precious metal catalysts. [0003] Compared with expensive nano-noble metal cat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/28B01J37/16C07C5/367C07C4/06
Inventor 郭永胜杨凤军魏会张玲玲
Owner ZHEJIANG UNIV
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