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High-strength and high-modulus electrospun polypyrrolone nanofiber and preparation method thereof

A nanofiber, high-strength and high-modulus technology, applied in the fields of fiber chemical characteristics, textiles and papermaking, single-component synthetic polymer rayon, etc., can solve problems such as processability limitations, high boiling point, and environmental pollution

Inactive Publication Date: 2021-11-26
JIANGXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since polypyrroline is neither molten nor soluble in common organic solvents, its processability is greatly limited, and at the same time, it greatly hinders the development of its applications.
Moreover, its insoluble and infusible properties make it impossible to prepare nanoscale fibers of this type of polymer by melt electrospinning or solution electrospinning
In addition, the traditional preparation of polypyrrone crude fibers or films is processed by dissolving them in super-strong protonic acids such as methanesulfonic acid and chlorosulfonic acid. These solvents are highly toxic and have high boiling points. The membrane material is removed cleanly, and it is easy to cause environmental pollution

Method used

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  • High-strength and high-modulus electrospun polypyrrolone nanofiber and preparation method thereof
  • High-strength and high-modulus electrospun polypyrrolone nanofiber and preparation method thereof
  • High-strength and high-modulus electrospun polypyrrolone nanofiber and preparation method thereof

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preparation example Construction

[0034] A second aspect of the present invention provides a method for preparing the above-mentioned high-strength and high-modulus electrospun polypyrrole nanofibers, which includes the following steps:

[0035] (1) Preparation of raw material monomers: acetic anhydride is dissolved in organic solvent A to obtain reaction material A, then the reaction material A is added to the organic solvent B solution of substituted benzphenyl diamine, and the temperature is not higher than 5 Reacting at a reaction temperature of °C for 2 to 6 hours to obtain an intermediate crude product; adding calcium oxide precipitation to the intermediate crude product, filtering, and concentrating to obtain a crude product; then recrystallizing the crude product to obtain the raw material monomer;

[0036] (2) Synthesis of the intermediate polyacetamidoamic acid: adding the raw material monomers into the reactor to perform condensation reaction with the dibasic acid anhydride in a solvent to obtain a p...

Embodiment 1

[0055] (1) 10 grams (46.67mmol) of 3,3'-diaminobenzidine is placed in the reactor, and 56.7 grams of THF is added to dissolve and prepare a solution with a concentration of 15%, and then in the above-mentioned 3,3'-diaminobenzidine (M=214.27) THF solution 95.29 grams (2*46.67mmol acetic anhydride (M=102.09), weight 9.53 grams) of 10% acetic anhydride THF solution is added dropwise at the speed of 1-3g / min, controls reaction temperature at React in the range of -5 to 0°C for 4 hours, then add 2.26g (46.67mmol) of dry calcium oxide (M=56.077), react with acetic acid to form calcium acetate precipitate, and precipitate from the THF solution; filter to remove calcium acetate in the system, And the filtrate was concentrated by rotary evaporation to obtain 13.6 grams of crude product (theoretical yield was 13.92 grams) of 3,3'-diamino-4,4'-diacetamidobiphenyl (M=298.27); Add ethanol / THF solvent with a volume ratio of 1 / 1 to the crude product of diamino-4,4'-diacetylaminobiphenyl, an...

Embodiment 2

[0060](1) 10 grams (46.67mmol) of 3,3'-diaminobenzidine is placed in the reactor, and 56.7 grams of THF is added to dissolve and prepare a solution with a concentration of 15%, and then in the above-mentioned 3,3'-diaminobenzidine (M=214.27) THF solution 95.29 grams (2*46.67mmol acetic anhydride (M=102.09), weight 9.53 grams) of 10% acetic anhydride THF solution is added dropwise at the speed of 1-3g / min, controls reaction temperature at React in the range of -5 to 0°C for 4 hours, then add 2.26g (46.67mmol) of dry calcium oxide (M=56.077), react with acetic acid to form calcium acetate precipitate, and precipitate from the THF solution; filter to remove calcium acetate in the system, And the filtrate was concentrated by rotary evaporation to obtain 13.6 grams of crude product (theoretical yield was 13.92 grams) of 3,3'-diamino-4,4'-diacetamidobiphenyl (M=298.27); Add ethanol / THF solvent with a volume ratio of 1 / 1 to the crude product of diamino-4,4'-diacetylaminobiphenyl, and...

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Abstract

The invention relates to the technical field of polypyrrolone materials, in particular to a high-strength and high-modulus electrospun polypyrrolone nanofiber and a preparation method thereof. According to the invention, tetraaminobiphenyl (4, 4 '- diacetamido-3, 3'-diaminobiphenyl) containing two invisible amino (acetamido) groups is adopted as a monomer to synthesize a polyimide precursor (polyacetamido amic acid), polyacetamido amic acid is subjected to imidization (at a high temperature of 300-350 DEG C) in an air atmosphere to form polyacetamido imide (a polypyrrolone precursor), and high-temperature pyrrolone reaction (at a high temperature of 450-500 DEG C) is carried out in the air atmosphere, and the high-performance polypyrrolone nanofiber with the tensile strength up to 3.0 GPa, tensile film amount up to 200 GPa and above, high glass transition temperature, high decomposition temperature and the like is obtained. Compared with a method for directly synthesizing polypyrrolone by using 3, 3 ', 4, 4'-tetraaminobiphenyl as a monomer, the method has the advantages that the chemical structure of the polymer is not damaged by high-temperature imidization and pyrrolone reaction in an air atmosphere, and acetamido is more resistant to high temperature and air oxidation than amino.

Description

technical field [0001] The present application relates to the technical field of polypyrrole materials, in particular to a high-strength and high-modulus electrospun polypyrrole nanofiber and a preparation method thereof. Background technique [0002] Polypyrrole is a kind of rigid ladder-shaped or semi-ladder-shaped polyaromatic heterocyclic macromolecular polymer, which has good high temperature resistance and oxidation resistance, and the decomposition temperature of some polypyrrolone exceeds 700°C. This kind of polymer fiber is not only a kind of high temperature resistant flame retardant fiber, but also a kind of high-strength, high-modulus high-performance fiber. Since the 1960s, this type of polymer has been widely studied, and it is generally polymerized at high temperature in a high boiling point solvent such as polyphosphoric acid. Since polypyrroline is neither molten nor soluble in common organic solvents, its processability is greatly limited, and its applicat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/74C08G73/10
CPCD01F6/74C08G73/1067C08G73/1007
Inventor 侯豪情胡添赵永丽江昱轩彭慧珍
Owner JIANGXI NORMAL UNIV
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