A kind of microspherical hollow structure nickel-based hydrogenation catalyst and preparation method thereof

A hydrogenation catalyst, spherical technology, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, preparation of organic compounds, etc., can solve destructive, environmental pollution, reduce material integrity and mechanical Strength and other issues, to achieve the effect of large internal cavity, simple preparation technology, and low raw material cost

Inactive Publication Date: 2016-05-11
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is highly manipulable, and the final shape of the product inherits the shape of the hard template, and a variety of different materials can be prepared; however, the template will be destructive to the assembled structure during the removal process, reducing the integrity and mechanical strength of the material. , and the process of processing templates will use some organic solvents or acid-base solutions, which will easily cause certain environmental pollution
Soft templating agents generally form micelles through some organic surfactants such as cetyltrimethylammonium bromide, sodium dodecylsulfonate, etc. to control the morphology to obtain a hollow spherical structure. easy to cause environmental pollution

Method used

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  • A kind of microspherical hollow structure nickel-based hydrogenation catalyst and preparation method thereof
  • A kind of microspherical hollow structure nickel-based hydrogenation catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Weigh 1.2716g of Al(H 2 PO 4 ) 3 Dissolve in 40mL deionized water, then sonicate to completely dissolve into a clear and clear solution, reflux and stir in an oil bath at 90°C for 6 hours to obtain a white turbid colloidal solution, then pour it into the polytetrafluoroethylene liner of the high-pressure hydrothermal reactor; Weigh 0.9608g urea and 2.1028g NiSO 4 ·6H 2 O was dissolved in 40mL of deionized water, then sonicated to completely dissolve into a clear solution, poured into the PTFE liner of the above high-pressure hydrothermal reactor, stirred evenly and sealed, moved to a constant temperature oven at 100℃, reacted for 12h Take it out and cool it to room temperature; wash with deionized water and absolute ethanol to neutrality, and place the resulting product in a 70°C constant temperature drying oven for 48 hours to obtain a micron-sized hollow spherical nickel-aluminum hydrotalcite assembly material.

Embodiment 2

[0017] Weigh 0.9853g aluminum sec-butoxide and dissolve it in 40mL deionized water, sonicate it to completely dissolve into a transparent clear solution, reflux and stir in an oil bath at 100°C for 4h to obtain a white turbid colloidal solution, then pour it into a high-pressure hydrothermal reactor for polymerization In the tetrafluoroethylene liner; weigh 1.9216g urea and 3.1542g NiSO 4 ·6H 2 O was dissolved in 40mL deionized water, and ultrasonic washer was sonicated until it was completely dissolved to obtain a green transparent solution. This solution was transferred to the aforementioned inner tank and stirred until it was evenly mixed. The high-pressure hydrothermal kettle was sealed and moved to 150℃. In a constant temperature oven, after reacting for 12 hours, take it out and cool to room temperature; wash with deionized water and absolute ethanol to neutrality, and place the product in a constant temperature drying oven at 70°C for 48 hours to obtain a micron-sized holl...

Embodiment 3

[0019] Weigh 2.6657g of Al 2 (SO 4 ) 3 ·18H 2 O was dissolved in 40mL deionized water, sonicated to completely dissolve into a clear and clear solution, refluxed in an oil bath at 70°C and stirred for 4h. After the reaction, it was cooled to room temperature and transferred to a 100mL high-pressure hydrothermal reactor polytetrafluoroethylene liner Medium for use; then weigh out 2.2430g hexamethylenetetramine and 4.2056g NiSO 4 ·6H 2 Dissolve O in 40mL deionized water, sonicate it in an ultrasonic scrubber until it is completely dissolved, and obtain a green clear solution. Move it to the inner tank described before and stir it evenly; seal the high-pressure hydrothermal kettle and place it in a 140℃ constant temperature oven Reaction for 24h; after the reaction, take out the reaction kettle and cool it to room temperature, wash with deionized water and absolute ethanol until the pH of the system is about 7, and then dry the obtained precipitate in a constant temperature drying o...

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Abstract

The invention discloses a micro spherical hollow structure nickel-based hydrogenation catalyst as well as a preparation method thereof in the technical field of catalyst preparation. The method comprises the following steps: controlling the morphology of an aluminum raw material serving as a mold plate which is consumed gradually along with the reaction, inducing hydrotalcite assembly to obtain a micro spherical hollow hydrotalcite assembly body, and carrying out in-situ reduction to obtain the micro spherical hollow nickel-based catalyst. The catalyst material obtained by preparation has high specific surface area, and the internal empty cavity structure and the abundant open-framework structures have great actual application value. The catalyst has relatively high hydrogenation activity and selectivity when being used for catalyzing dimethyl terephthalate (DMT) benzene ring hydrogenation in the reaction for preparing dimethyl 1, 4-cyclohexanedicarboxylate.

Description

Technical field [0001] The invention belongs to the technical field of nickel-based hydrogenation catalyst preparation, and particularly relates to a microspherical hollow structure nickel-based hydrogenation catalyst and a preparation method thereof. Background technique [0002] Hydrotalcite is a multifunctional anionic layered material, also known as bis-hydroxyl composite metal hydroxide. Its general chemical formula can be expressed as [M 1-x 2+ M x 3+ (OH) 2 ] x+ (A n- ) x / n ·MH 2 O, where A n- Represents exchangeable anions between layers, n is the number of charges, M 3+ , M 2+ It represents trivalent and divalent metal cations, and x refers to the content of metal elements. Hydrotalcite has a layered structure, the exchangeability of interlayer ions, and the tunability of layer elements. It has a wide range of applications in catalysis, adsorption, biosensing, photoelectric materials, etc. The performance of hydrotalcite flakes is limited by its irregular accumulation an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/755B01J35/08C07C67/303C07C69/75
Inventor 张法智张悦张荣岳彩利
Owner BEIJING UNIV OF CHEM TECH
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