Synthetic method of polymetaphenylene diamine nanoparticle

A technology of poly-m-phenylenediamine and synthesis method, which is applied in the field of synthesis of poly-m-phenylenediamine nanoparticles with high monomer conversion rate, can solve the problem of improving the effectiveness and economy of polyarylamine synthesis reaction and affecting the industrialization of technology Application prospects, large secondary pollution and other problems, to achieve broad industrial application prospects, reduce secondary pollution problems, and improve effectiveness

Inactive Publication Date: 2013-01-16
CENT SOUTH UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Low monomer conversion rate is not conducive to improving the effectiveness and economy of polyarylamine synthesis reaction, and affects the application prospects of t...

Method used

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  • Synthetic method of polymetaphenylene diamine nanoparticle
  • Synthetic method of polymetaphenylene diamine nanoparticle
  • Synthetic method of polymetaphenylene diamine nanoparticle

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Accurately weigh 5.0 g of m-phenylenediamine and add to a 250 mL round bottom flask. Add 100ml of distilled water and stir until dissolved, keep the temperature of the monomer solution in a water bath to 30°C; accurately weigh 0.40g of copper chloride dihydrate and dissolve it in 10mL of distilled water, keep the temperature of the copper ion solution in a water bath to 30°C, and quickly Add it to the m-phenylenediamine solution for pre-reaction, and the solution turns from clear and colorless to dark yellow-brown rapidly. Accurately weigh 11g of sodium persulfate and dissolve it in 37ml of distilled water to fully dissolve it, and keep the temperature of the sodium persulfate solution in a water bath to 30°C. Accurately weigh 8g of sodium hydroxide and dissolve it in 100mL of distilled water to make it fully dissolved, and take 37mL for use. Within about 30 minutes, the sodium persulfate oxidant and sodium hydroxide solution were simultaneously dropped into the soluti...

Embodiment 2~4

[0025] Repeat Example 1, change the concentration of sodium hydroxide solution, respectively 1.5, 2.25 and 2.5mol / L. The obtained product is a black solid powder, all of which are nano-scale poly-m-phenylenediamine. The corresponding conversion rates are as high as 90.1%, 92.6% and 91.2% respectively.

Embodiment 5

[0027] Repeat Example 1, changing the water bath insulation temperature to 0, 15, and 60 degrees. The obtained product is a black solid powder, all of which are nano-scale poly-m-phenylenediamine. The corresponding conversion rates are as high as 94.5%, 96% and 97% respectively.

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Abstract

The invention discloses a synthetic method of polymetaphenylene diamine nanoparticles, and the method is divided into two stages of prepolymerization and oxidation polymerization. The method comprises the following steps: firstly adding a divalent copper ion solution into an aqueous solution of metaphenylene diamine, stirring and reacting for 10-30 min to perform a prepolymerization reaction; then, gradually adding a persulfate aqueous solution and alkali liquor simultaneously within 30-60 min, initiating oxidation polymerization, and continuing stirring and reacting for 5-8 hours; filtering, and washing to obtain the polymetaphenylene diamine nanoparticles. The conversion rate of metaphenylene diamine monomer is up to 90%-98%, and the generation amounts of metaphenylene diamine monomer and its oligomer are effectively reduced. The method of the invention can prepare nanoscale polymetaphenylene diamine with high efficiency, is economical, effective, and simple in operation, and has a greatly improved monomer conversion rate.

Description

technical field [0001] The invention relates to a method for synthesizing poly-m-phenylenediamine nanoparticles with high monomer conversion rate. Background technique [0002] Polyarylamine nanomaterials have excellent properties such as special oxidation-reduction properties, catalytic properties, photoelectric conversion properties, and adsorption properties, and are widely used in the fields of optics and electronics. Since the 1970s and 1980s, the research on the preparation of polyarylamines by chemical oxidative polymerization has been highly concerned, which mainly activates the monomers into cationic radicals by uniformly adding oxidants to initiate polymerization. But so far, chemical oxidative polymerization still has the problem of generally low monomer conversion rate (or yield) in the synthesis reaction. For example, Li [Li Xin-Gui, etc. Chemistry A European Journal, 2008, 14, 10309-10317] etc. used persulfate to synthesize polyaniline, and the conversion rate...

Claims

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Application Information

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IPC IPC(8): C08G73/02
Inventor 王海鹰柴立元张理源苏珍杨志辉彭兵闵小波杨卫春
Owner CENT SOUTH UNIV
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