Method for preparing nano nickel by taking nano spherical polyelectrolyte brush as reactor and application of nano nickel

A polyelectrolyte brush and polyelectrolyte technology, applied in chemical instruments and methods, nanotechnology, nanotechnology, etc., can solve problems such as easy agglomeration, difficulty in controlling the size and distribution of nano-nickel, and achieve good catalytic activity and excellent dispersion Effect

Inactive Publication Date: 2013-05-22
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main obstacle affecting its application at present is that the size and distribution of nano-nickel are not easy to control and easy to agglomerate

Method used

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  • Method for preparing nano nickel by taking nano spherical polyelectrolyte brush as reactor and application of nano nickel
  • Method for preparing nano nickel by taking nano spherical polyelectrolyte brush as reactor and application of nano nickel
  • Method for preparing nano nickel by taking nano spherical polyelectrolyte brush as reactor and application of nano nickel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Preparation of Photoinitiator HMEM by Schotten-Baumann Reaction

[0034] Pour 30.0g of photoinitiator 2-hydroxy-4'-hydroxyethoxy-2-methylphenyl ethyl ketone (HMP) into a 500ml single-necked flask, add 150ml of acetone, stir until HMP is completely dissolved, then add 10g of newly purified pyridine, continue to stir at low temperature, then dissolve 13.6g of methacryloyl chloride (MC) in 50ml of acetone, and slowly add it dropwise into the reaction flask, after the dropwise addition, react at room temperature for 12 hours to obtain Orange liquid, the beige precipitate at the bottom is removed by filtration, and the chromatographic separation method is used to obtain pure HMEM photoinitiator, and its proton nuclear magnetic resonance spectrogram is as follows image 3 shown.

Embodiment 2

[0036] Nanospherical Polyelectrolyte Brushes Prepared by Photoemulsion Polymerization

[0037]Put 230 ml of deionized water, 0.24 g of sodium dodecylsulfonate (or sodium dodecylbenzenesulfonate), and 0.74 g of potassium persulfate (or hydrogen peroxide) into a 500 ml three-neck flask. After fully dissolved, add 10.0 g of styrene (or methyl methacrylate). Pump nitrogen 3 to 5 times, and control the speed at 300 rpm. After the temperature rose to 35 °C, 0.15 g of sodium bisulfite was dissolved in 20 ml of deionized water, and quickly dropped into the three-necked flask. During the reaction, keep the temperature and rotating speed constant, and after 2 hours, the polymerization reaction reaches the final stage. At this time, 1.0 gram of the photoinitiator HMEM obtained in Example 1 is slowly added dropwise to the reaction system, and the rate of addition is controlled at 7 seconds. / drop; continue to react for 3 hours after the drop is completed; the polymer microemulsion ball...

Embodiment 3

[0039] Preparation of nanospherical polyelectrolyte brushes adsorbed with nickel ions

[0040] Get 50 milliliters of the spherical polyelectrolyte brush emulsion that embodiment 2 obtains, add 0.024 gram of sodium hydroxide solids, after fully stirring for 10 hours, place this emulsion in an ultrafiltration device, adopt 3 liters of concentration to be 0.001 mol / liter of nickel chloride The aqueous solution (nickel chloride hexahydrate or nickel acetate tetrahydrate can be used) is subjected to ultrafiltration, so that nickel ions and sodium ions undergo ion exchange, enter the interior of the nano-spherical polyelectrolyte brush, and then use 3 liters of deionized water for ultrafiltration washing to remove free nickel ions, and the nano-spherical polyelectrolyte brushes adsorbed with nickel ions are obtained.

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Abstract

The invention discloses a method for preparing nano nickel by taking a nano spherical polyelectrolyte brush as a microreactor and an application of the nano nickel. The method comprises the following steps of: preparing polymer microspheres with the particle size of 80-140nm by adopting emulsion polymerization initiated by an oxidation-reduction system; adding a photoinitiator in the terminal stage of the emulsion polymerization, coating the photoinitiator on the surfaces of the polymer microspheres to form a photoinitiator layer, then utilizing an ultraviolet lamp to initiate polyelectrolytemonomers to be polymerized so as to obtain a spherical electrolyte brush with the particle size of 10-400nm; then adding sodium hydroxide to dissociate carboxyl on an electrolyte chain; treating the dissociated spherical polyelectrolyte brush by use of a nickel chloride aqueous solution, thus nickel ions exchange sodium ions and enters into the polyelectrolyte brush; and adding sodium borohydrideto reduce the nickel ions into nano nickel in situ, thus finally obtaining controllable nano nickel which are uniformly distributed inside the nano spherical polyelectrolyte brush and have the particle size of 1-14nm. The nano nickel loaded on the spherical polyelectrolyte brush is an ideal efficient nano catalyst.

Description

technical field [0001] The present invention relates to the preparation method and application of nano-nickel. Specifically, the spherical polyelectrolyte brush is prepared by using the emulsion polymerization and photoemulsion polymerization method initiated by the oxidation-reduction system, and then the spherical polyelectrolyte brush is used as a nanoreactor to reduce the nano-nickel in situ. Divalent nickel ions are used to prepare nano-nickel composite particles, and the obtained nano-composite particles are used as high-efficiency catalysts. Background technique [0002] When one end of the charged linear polymer chain is fixed on the surface of the spherical substrate and arranged densely, due to the volume repulsion effect and electrostatic repulsion, their free ends will be stretched outwards to form a brush-like structure, These are so-called spherical polyelectrolyte brushes. The special structure of spherical polyelectrolyte brushes greatly strengthens the Donn...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/24B82Y40/00B82Y30/00B01J31/28C07C215/76C07C213/02
Inventor 郭旭虹朱忠明吴爽李莉房鼎业
Owner EAST CHINA UNIV OF SCI & TECH
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