High-strength and high-modulus polypyrrolone fiber and preparation method thereof

A high-strength, high-modulus, polypyrrolidone technology, applied in the fields of fiber chemical characteristics, single-component synthetic polymer rayon, chemical post-processing of synthetic polymer rayon, etc., can solve the limitations of processability, high boiling point, environmental pollution, etc.

Inactive Publication Date: 2021-11-23
JIANGXI NORMAL UNIV
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  • 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.
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. If it is removed from the membrane material, it is easy to cause environmental pollution

Method used

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  • High-strength and high-modulus polypyrrolone fiber and preparation method thereof
  • High-strength and high-modulus polypyrrolone fiber and preparation method thereof
  • High-strength and high-modulus polypyrrolone fiber and preparation method thereof

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preparation example Construction

[0029] A second aspect of the present invention provides a method for preparing the above-mentioned high-strength and high-modulus polypyrrole fiber, which includes the following steps:

[0030] (1) Preparation of raw material monomer: acetic anhydride is dissolved in organic solvent A to obtain reaction material A, then said reaction material A is added in the organic solvent B solution of substituted biphenyl diamine, and Reacting at a reaction temperature of °C for 2 to 6 hours to obtain an intermediate crude product; adding calcium oxide to the intermediate crude product for precipitation, filtering, and concentrating to obtain a crude product; then recrystallizing the crude product to obtain the raw material monomer;

[0031] (2) Synthesis of the intermediate polyacetamidoamic acid: adding the raw material monomers into the reactor to carry out condensation reaction with the dibasic acid anhydride in the spinning solvent to obtain the polyacetamidoamic acid solution;

[0...

Embodiment 1

[0063] (1) Preparation of raw materials: 100 grams (466.7 mmol) of 3,3'-diaminobenzidine was placed in a reactor and dissolved in 567 grams of THF to prepare a solution with a concentration of 15%, and then in the above 3,3'- In the THF solution of diaminobenzidine (M=214.27), 952.9 grams (2*466.7mmol acetic anhydride (M=102.09), weight 95.29 grams) of 10% acetic anhydride THF solution was added dropwise at a speed of 3-5g / min, Control the reaction temperature in the range of -5~0°C for 4 hours, then add 22.6g (466.7mmol) of dry calcium oxide (M=56.077) to react with acetic acid to form calcium acetate precipitate, which is precipitated from the THF solution; Calcium acetate, and the filtrate was concentrated by rotary evaporation to obtain 136 grams of crude product (theoretical yield is 139.2 grams) of 3,3'-diamino-4,4'-diacetamidobiphenyl (M=298.27); ,3'-diamino-4,4'-diacetylaminobiphenyl crude product was added ethanol / THF solvent with a volume ratio of 1 / 1, and recrystall...

Embodiment 2

[0067] (1) Preparation of raw materials: 100 grams (466.7 mmol) of 3,3'-diaminobenzidine was placed in a reactor and dissolved in 567 grams of THF to prepare a solution with a concentration of 15%, and then in the above 3,3'- In the THF solution of diaminobenzidine (M=214.27), 952.9 grams (2*466.7mmol acetic anhydride (M=102.09), weight 95.29 grams) of 10% acetic anhydride THF solution was added dropwise at a speed of 3-5g / min, Control the reaction temperature in the range of -5~0°C for 4 hours, then add 22.6g (466.7mmol) of dry calcium oxide (M=56.077) to react with acetic acid to form calcium acetate precipitate, which is precipitated from the THF solution; Calcium acetate, and the filtrate was concentrated by rotary evaporation to obtain 136 grams of crude product (theoretical yield is 139.2 grams) of 3,3'-diamino-4,4'-diacetamidobiphenyl (M=298.27); ,3'-diamino-4,4'-diacetylaminobiphenyl crude product was added ethanol / THF solvent with a volume ratio of 1 / 1, and recrystall...

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Abstract

The invention relates to the technical field of polypyrrolone materials, in particular to high-strength and high-modulus polypyrrolone fiber and a preparation method thereof. The diameter of the polypyrrolone nanofiber is 8 to 15 microns. According to scheme, tetraaminobiphenyl (4,4'-diacetamido-3,3'-diaminobiphenyl) containing two invisible amino groups (acetamido) is adopted as a monomer to firstly synthesize a polyimide prepolymer (poly acetamido amic acid), then the polyimide prepolymer is used for preparing a nascent filament in a wet spinning manner, imidization (at a high temperature of 300-350 DEG C) is performed in an air atmosphere to form poly acetamido imide (a polypyrrolone prepolymer), and high-temperature pyrrolone treatment ( at a high temperature of 450-500 DEG C) is performed in the air atmosphere to form a high-performance polypyrrolone polymer. Besides, the problems that free amino group in polyaminoamic acid is active, so that the prepolymer is not stable enough, gel is easy to generate, the flowability of a solution is seriously influenced, and spinning cannot be smoothly carried out are effectively avoided.

Description

technical field [0001] The present application relates to the technical field of polypyrrole materials, in particular to a high-strength and high-modulus polypyrrole fiber 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 application development ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/74D01F11/08
Inventor 侯豪情王科遇黄强朱咏梅
Owner JIANGXI NORMAL UNIV
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