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Process for synthesizing iron-nickel alloy nano particle catalyst for selective hydrogenation

A nanoparticle, iron-nickel alloy technology, applied in the field of synthesis of iron-nickel alloy nanoparticle catalysts for selective hydrogenation, can solve the problems of low decomposition temperature, toxic nickel carbonyl, inconvenient storage and transportation, etc.

Inactive Publication Date: 2009-01-28
BC P INC CHINA NAT PETROLEUM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There are following defects in the preparation method with iron carbonyl and nickel carbonyl as raw materials: (1) iron carbonyl and nickel carbonyl are poisonous, and the decomposition temperature is low, so storage and transportation are very inconvenient
The use of superparamagnetic monodisperse iron-nickel alloy nanoparticles as a catalyst for selective hydrogenation reactions has not been reported yet

Method used

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  • Process for synthesizing iron-nickel alloy nano particle catalyst for selective hydrogenation
  • Process for synthesizing iron-nickel alloy nano particle catalyst for selective hydrogenation
  • Process for synthesizing iron-nickel alloy nano particle catalyst for selective hydrogenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Put 2mmol of iron acetylacetonate, 2mmol of nickel acetylacetonate, 4ml of trioctylphosphine, 6ml of oleylamine, 3mmol of 1,2-hexadecanoyl alcohol, and 40ml of liquid paraffin into a 100ml stainless steel autoclave reactor, and pass it into a high-purity Nitrogen deoxygenation. Pass hydrogen gas (purity 99.9%) into the autoclave, fill the pressure to 4.0MPa, adjust the stirring speed to 500rpm, then raise the temperature to 300°C, and react for 3 hours. After the reaction was completed, the reactor was opened, and the reaction solution was taken out and placed in a 250 ml beaker. Add 40 milliliters of ethanol and 10 milliliters of petroleum ether (60-90° C.) into the beaker, stir well and place it on the surface of the permanent magnet. The liquid in the beaker will separate into two layers, remove the supernatant. Repeat the above steps 3-5 times, the black nanoparticles will be enriched at the bottom of the beaker. The obtained nanoparticles are vacuum-dried at 100...

Embodiment 2

[0032] 10 ml of p-chloronitrobenzene was dissolved in 30 ml of ethanol, the solution was added into an autoclave reactor, and then 0.2 g of iron-nickel alloy nanoparticles was added into the autoclave. Nitrogen was introduced into the reactor to replace it to remove oxygen, and then hydrogen was introduced. The initial hydrogen pressure is 4.0MPa.

[0033] The temperature of the reactor was raised to 100°C, and the temperature was kept constant for one hour. After the reaction is over, after the reactor body is cooled, hydrogen gas is released to open the reactor, and the black liquid is taken out into a beaker. The beaker is placed on the surface of the permanent magnet, and after a few minutes, the magnetic nano-catalyst particles are concentrated at the bottom of the beaker. The clear solution was removed for chromatographic analysis.

[0034]

[0035] The results of chromatographic analysis showed that p-chloronitrobenzene was converted into p-chloroaniline with a co...

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Abstract

The invention relates to a method for preparing and separating monodisperse superparamagnetism iron-nickel alloy nano-particle catalyst used for selective hydrogenation. In the method, Ferric acetylacetonate and Nickel acetylacetonate are taken as raw materials, liquid paraffin is taken as reaction medium, trioctyl-phosphine and oleyl amine are taken as stabilizer (also called protecting agent or surface modifier) and polyol is taken as morphology modifier. The product obtained is iron-nickel alloy nano-particle. The method adding magnetic field to assist solvent extraction can separate the iron-nickel alloy nano-particle from the reaction system. The iron-nickel alloy nano-particle can be dispersed into organic solvents again such as chloroform, petroleum ether, and the like, without the generation of precipitation. The nano-particle is used as the catalyst for the selectively hydrogenation of chloro-nitrobenzene, the convention rate of reactants can reach 70 percent and the selectivity thereof is 98 percent.

Description

technical field [0001] The invention relates to a synthesis method of an iron-nickel alloy nanoparticle catalyst for selective hydrogenation, which belongs to the improvement and innovation of the preparation and separation methods of magnetic nanoscale materials. The prepared monodisperse superparamagnetic iron-nickel alloy nanoparticles can be completely dissolved in polar and non-polar organic solvents, Background technique [0002] The application fields of magnetic nanomaterials are very extensive. Magnetic nanoparticles are an important part of nanoscale materials. At present, the methods for preparing ultrafine metal powder mainly include: grinding method, solid phase reaction method, vapor phase deposition method, aqueous solution electrolysis method, aqueous solution co-precipitation method, microemulsion method, sol-gel method, carbonyl compound thermal decomposition method, etc. The purity of the iron-nickel alloy powder prepared by the first seven methods is no...

Claims

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Application Information

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IPC IPC(8): B01J23/74C07B31/00
Inventor 张宏玉张永宁刘峰奎阙国和邓文安沐宝泉金环年李庶峰文萍于建宁
Owner BC P INC CHINA NAT PETROLEUM CORP
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