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Method for preparing poly (1-amino-5-chloro anthraquinone) nanofiber through interface chemical oxidative polymerization

A technology of oxidative polymerization and interfacial chemistry, applied in the field of material chemistry, can solve the problems of low stability of nano-dispersion, reduced solubility, low molecular weight, etc., and achieve the effect of low synthesis cost, pure product, and high molecular weight of product

Inactive Publication Date: 2014-07-30
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

One of the main reasons for the low molecular weight may be that the addition of inorganic acid significantly reduces the solubility of monomer anthraquinone-1-amino-5-ammonium sulfonate in water, and also reduces the solubility of oligomers in the chain growth stage. Solubility, so that the oligomer precipitates out from the reaction system and the chain growth process cannot continue, so only low molecular weight oligomers can be obtained
Secondly, the stability of the nano-dispersion is not high, such as poly(1-aminoanthraquinone) nanofibers need to maintain the nano-dispersion state of the polymer by means of emulsifier DBSA
There are no reports about poly(1-amino-5-chloroanthraquinone) nanofibers and their interfacial chemical oxidative polymerization

Method used

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  • Method for preparing poly (1-amino-5-chloro anthraquinone) nanofiber through interface chemical oxidative polymerization
  • Method for preparing poly (1-amino-5-chloro anthraquinone) nanofiber through interface chemical oxidative polymerization
  • Method for preparing poly (1-amino-5-chloro anthraquinone) nanofiber through interface chemical oxidative polymerization

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Embodiment 1: The method for preparing poly(1-amino-5-chloroanthraquinone) nanofibers by interfacial chemical oxidative polymerization, the specific operation is as follows:

[0027] (1) Weigh 0.9 mmol (0.2319 g) of 1-amino-5-chloroanthraquinone monomer into a 100 mL Erlenmeyer flask, add 30 mL of nitrobenzene, and pipette 150 μL (1.75 mmol) perchloric acid was dropped into the Erlenmeyer flask, the concentration of perchloric acid in the whole reaction system was 50 mmol / L, another 1.8 mmol (0.1865 g) chromium trioxide was taken as an oxidant and dissolved in 5.0 mL of distilled water ;

[0028] (2) Put the chromium trioxide aqueous solution and the 1-amino-5-chloroanthraquinone acidic nitrobenzene solution in a constant temperature water bath at 30°C for about 30 minutes, and then add the oxidant solution to the 1-amino-5 -In acidic nitrobenzene solution of chloranthraquinone, magnetic stirring was carried out at the same time, constant temperature reaction was carri...

Embodiment 2

[0029] Embodiment 2: The method for preparing poly(1-amino-5-chloroanthraquinone) nanofibers by interfacial chemical oxidative polymerization, the specific operation is as follows:

[0030] The method is the same as in Example 1, except that the organic solvent for dissolving the 1-amino-5-chloroanthraquinone monomer is changed to o-dichlorobenzene, nitromethane or chloroform respectively, and the resulting poly(1-amino-5-chloroanthraquinone ) nanofiber yields were 12.8%, 34.7% and 10.3%, respectively. The electrical conductivity of poly(1-amino-5-chloroanthraquinone) nanofiber pellets measured by two-electrode method was 6.9×10 -6 S / cm, 4.3×10 -6 S / cm and 5.5×10 -7 S / cm.

[0031] The UV-Vis spectra of PACA and ACA monomers synthesized in different media are shown in figure 1 , the figure shows: the monomer has a strong absorption at 267 nm and a weak absorption at 481 nm, while the polymer produces a new strong and broad absorption peak at around 612 nm, and the absorp...

Embodiment 3

[0032] Embodiment 3: The method for preparing poly(1-amino-5-chloroanthraquinone) nanofibers by interfacial chemical oxidative polymerization, the specific operation is as follows:

[0033] (1) Weigh 0.9 mmol (0.2328 g) of 1-amino-5-chloroanthraquinone monomer into a 100 mL Erlenmeyer flask, add 30 mL of nitrobenzene, and pipette 150 μL (1.75 mmol) perchloric acid was dropped into the Erlenmeyer flask, the concentration of perchloric acid in the whole reaction system was 50 mmol / L, another 1.8 mmol NaClO (1.04 mL NaClO solution, the NaClO solution contained no less than 5.2 %, OH – content of 7.0–8.0%) as an oxidizing agent, with HClO 4 Adjust the pH value to close to 7.0, then dilute to 5.0 mL with distilled water;

[0034] (2) Put NaClO aqueous solution and 1-amino-5-chloroanthraquinone acidic nitrobenzene solution in a constant temperature water bath at 30°C for about 30 minutes, then add the oxidant solution to the monomer solution at one time, and perform magnetic Stir...

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Abstract

The invention discloses a method for preparing poly(1-amino-5-chloroanthraquinone) nanofibers through interfacial chemical oxidation polymerization. In this method, the oxidant is dissolved in water, and the monomer 1-amino-5-chloroanthraquinone is dissolved in water. Water-immiscible organic solvents are protonated by adding acid, and then the two are mixed. The monomer contacts the oxidizing agent at the two-phase interface to cause a polymerization reaction to produce poly(1-amino-5-chloroanthraquinone). The method of the present invention, There is no need to add any external stabilizer, just control the polymerization reaction conditions, and you can synthesize a self-stabilizing nanofiber bundle with a diameter of 10~70nm with multiple fibers intertwined with each other. This synthesis method is a one-pot synthesis and has The synthesis method and post-treatment procedures are simple, do not involve any stabilizers and surfactants, the product is pure, the molecular weight of the obtained product is large, the synthesis cost is low, and it can be universally applicable.

Description

technical field [0001] The invention relates to a method for preparing poly(1-amino-5-chloroanthraquinone) nanofibers through interface chemical oxidation polymerization, belonging to the field of material chemistry. Background technique [0002] In recent years, with the continuous advent of various new aromatic amine polymers, they have excellent performance in terms of conductivity, electroactivity, electrocatalysis, electrochromism, optical activity, and detection and adsorption of heavy metal ions. Similar to traditional conductive polymers, the above properties can be effectively controlled by controlling the polymerization conditions and doping mechanism. However, aromatic amine polymers are generally insoluble and infusible polymers that are difficult to process. Nanoizing it can not only solve this problem ingeniously, but also endow the polymer with new functionality. [0003] Among the many new aromatic amine conductive polymers, aminoanthraquinone polymers have...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/02
Inventor 黄绍军杜萍孙卉黄秋玲
Owner KUNMING UNIV OF SCI & TECH
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