Interface preparation method for polynaphthalenediamine sub-micron particles

A polynaphthalene diamine submicron, naphthalene diamine technology is applied in the field of preparation of polynaphthalene diamine, which can solve the problems of restricting wide application and insolubility, and achieve the effects of surface purity, good yield and universal applicability.

Inactive Publication Date: 2009-06-24
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this type of polymer still has the chronic problem of being insoluble, which restricts its wide application.

Method used

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  • Interface preparation method for polynaphthalenediamine sub-micron particles
  • Interface preparation method for polynaphthalenediamine sub-micron particles
  • Interface preparation method for polynaphthalenediamine sub-micron particles

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Accurately weigh 0.158g of 1,5-naphthalene diamine and dissolve it in 20mL of propylene carbonate, then weigh 0.228g of ammonium persulfate and dissolve it in 20mL of 2mol / L nitric acid aqueous solution. After lowering the temperature of the two solutions to 0°C at the same time, slowly add the acid solution dissolved in the oxidizing agent on top of the organic phase, and let it stand still so that the monomer and the oxidizing agent react on the interface for 24 hours. After the reaction, the resulting poly-1,5-naphthalenediamine mixture was poured into a beaker to terminate the reaction with 1 L of deionized water, filtered, and dried to obtain a tan polymer powder with a yield of 35%. The obtained poly-1,5-naphthalene diamine particles have a particle size of 150nm to 300nm, and its transmission electron microscope photo is shown in figure 1 .

Embodiment 2

[0022] Accurately weigh 0.158g of 1,5-naphthalene diamine and dissolve it in 20mL of propylene carbonate, then weigh 0.228g of ammonium persulfate and dissolve it in 20mL of 2mol / L perchloric acid aqueous solution. After lowering the temperature of the two solutions to 0°C at the same time, slowly add the acid solution dissolved in the oxidizing agent on top of the organic phase, and let it stand still so that the monomer and the oxidizing agent react on the interface for 24 hours. After the reaction, the resulting poly-1,5-naphthalenediamine mixture was poured into a beaker to terminate the reaction with 1 L of deionized water, filtered, and dried to obtain a tan polymer powder with a yield of 42%. The prepared poly-1,5-naphthalene diamine particles are uniform in size, with particle diameters ranging from 300nm to 400nm. figure 2 .

Embodiment 3

[0024] Accurately weigh 0.158g of 1,8-naphthalene diamine and dissolve it in 20mL of propylene carbonate, then weigh 0.228g of ammonium persulfate and dissolve it in 20mL of 2mol / L perchloric acid aqueous solution. After lowering the temperature of the two solutions to 5° C., slowly add the acid solution dissolved in the oxidizing agent on top of the organic phase and let it stand still so that the monomer and the oxidizing agent react on the interface for 24 hours. After the reaction, the resulting poly-1,5-naphthalenediamine mixture was poured into a beaker to terminate the reaction with 200 mL of deionized water, filtered, and dried to obtain a tan polymer powder with a yield of 31%. Observation by TEM shows that the particle diameter of the prepared poly-1,5-naphthalene diamine particles is 300nm-400nm.

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Abstract

The invention discloses a preparation method of polynaphthalene diamine. The method for preparing the interface of polynaphthalene diamine submicron particles comprises the following steps: dissolving the naphthalene diamine monomer in propylene carbonate, dissolving the oxidizing agent in the acid aqueous solution, cooling the two to 0-5°C, and dissolving the oxidizing agent aqueous solution Pour it into the liquid surface of the organic solution of the monomer, wait for the reaction to be complete, and then process it. The method of the invention does not need any template and additives, utilizes the interface between the organic phase and the water phase to suppress the excessive growth of the polymer, so that the particle size of the polymer is maintained at the submicron level of 100-400nm. The surface of the prepared polymer nanoparticle is pure, no special method is needed for purification treatment, and the method has good yield and universal applicability.

Description

technical field [0001] The invention relates to the field of preparation methods of polynaphthalenediamine. Background technique [0002] Organic conductive polymers have developed into one of the very active research fields due to their unique properties and broad application prospects. Research on conductive polymers has been extended to the chemical oxidative polymerization and electrochemical oxidative polymerization of aromatic diamines in recent years [Huang Meirong, Li Xingui, Li Shengxian. Synthesis of polynaphthalene diamine and its efficient reactive adsorption of heavy metal ions. Chemistry Progress, 2005, 17(2): 299-309], the typical representative of which is polynaphthalenediamine. Since the naphthalene diamine monomer is very sensitive to oxidative polymerization, one or two amino groups in the monomer can be oxidized to obtain linear polyaminoaniline, linear polyaminonaphthylamine, ladder polyphenazine and polymers containing phenazine structures. Thereby o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/02
Inventor 李新贵章家立黄美荣
Owner TONGJI UNIV
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