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Dispersion containing flame-resistant polymer, flame-resistant fiber, and carbon fiber

A polymer and dispersion technology, applied in the field of carbon fiber, can solve the problems of large viscosity changes over time, inability to use as a solution, difficult fiber shaping and forming, etc., to achieve the suppression of single fiber breakage or adhesion, and damage reduction , The effect of improving physical strength

Inactive Publication Date: 2012-12-12
TORAY IND INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since this method uses acrylonitrile-based polymer powder that has not undergone flame-resistant reaction, there is a problem that the viscosity of the solution changes greatly over time, and disconnection is often prone to occur.
In addition, since strong acidic solvents such as sulfuric acid and nitric acid, which tend to decompose general organic polymers, are used as solvents, it is necessary to use equipment made of special materials with corrosion resistance, which is also unrealistic in terms of cost.
[0007] In addition, a method of mixing heat-treated acrylonitrile-based polymer powder with non-heat-treated acrylonitrile-based polymer powder and dissolving them in an acidic solvent has also been proposed (see Patent Document 2). The aforementioned problem of imparting corrosion resistance to the device or instability of the solution
[0008] Further, a method of heat-treating polyacrylonitrile in dimethylformamide solution to convert polyacrylonitrile to a polymer having a cyclized structure has been proposed (refer to Non-Patent Document 1). In this scheme, due to polymerization A dilute solution with a concentration of 0.5% has too low viscosity, so it is basically difficult to shape and shape fibers, etc. When the concentration is increased, the polymer precipitates and cannot be used as a solution.

Method used

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  • Dispersion containing flame-resistant polymer, flame-resistant fiber, and carbon fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0121] 10.0 parts by weight of acrylonitrile homopolymer as a precursor polymer, 3.5 parts by weight of monoethanolamine as a cyclizing agent, 8.0 parts by weight of o-nitrotoluene as an oxidant, and 3.0 parts by weight of benzoic acid as an acid were dispersed in The resulting dispersion was stirred at 150°C for 8 hours in 75.5 parts by weight of dimethylsulfoxide as an organic solvent, and then cooled to a temperature of 30°C to obtain a dispersion in which a fire-resistant polymer was dispersed in dimethylsulfoxide. The average thickness of the film produced by the above-mentioned of the obtained dispersion containing the fire-resistant polymer was 141 μm, and the tensile strength per cross-sectional area was 3.15 MPa. In addition, the concentration of the refractory polymer in the obtained dispersion containing the refractory polymer was 12.1% by weight, and the refractory polymer isolated from the dispersion containing the refractory polymer was analyzed by 13C-NMR. Ther...

Embodiment 2

[0124] Except having used 3.0 weight part of p-hydroxybenzoic acids as an acid, it experimented similarly to Example 1. The average thickness of the film produced by the method of of the obtained dispersion containing the fire-resistant polymer was 141 μm, and the tensile strength per cross-sectional area was 2.86 MPa. Meanwhile, there was no single fiber breakage or clogging at the die opening site. In addition, the concentration of the refractory polymer in the dispersion containing the refractory polymer was 12.2% by weight, and the refractory polymer isolated from the dispersion containing the refractory polymer was analyzed by 13C-NMR. The peaks derived from the precursor polymer polyacrylonitrile or the flame-resistant polymer not confirmed in the organic solvent and the modifying agent are present. In addition, using IR for analysis, the result is at 1600cm -1 There are clear peaks. This flame-resistant polymer-containing dispersion was spun by the method of above....

Embodiment 3

[0126] Except using 2.5 parts by weight of monoethanolamine as a cyclizing agent, 7.0 parts by weight of o-nitrotoluene as an oxidant, 3.0 parts by weight of p-hydroxybenzoic acid as an acid, and 77.5 parts by weight of dimethyl sulfoxide as an organic solvent, the same as in Example 1 conduct experiments. The average thickness of the film produced by the method of of the obtained dispersion containing the refractory polymer was 130 μm, and the tensile strength per cross-sectional area was 2.46 MPa. Meanwhile, there was no single fiber breakage or clogging at the die opening site. In addition, the concentration of the refractory polymer in the dispersion containing the refractory polymer was 12.1% by weight, and the refractory polymer isolated from the dispersion containing the refractory polymer was analyzed by 13C-NMR. The peaks derived from the precursor polymer polyacrylonitrile or the flame-resistant polymer not confirmed in the organic solvent and the modifying agent a...

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Abstract

An object of the present invention is to provide a dispersion containing a flame-resistant polymer, which can improve shaping stability of the flame-resistant polymer during ejection from a die orifice, and physical stability of a shaped product in a washing step. The dispersion containing a flame-resistant polymer is a dispersion in which a flame-resistant polymer is dispersed in an organic solvent, an in-water tensile strength thereof per unit cross-sectional area is 1.0 MPa or more and 6.5 MPa or less, the flame-resistant polymer can be preferably obtained by heat-treating an acrylonitrile polymer in the presence of at least one kind of acid, acid anhydride or acid chloride in an organic solvent, and a suitable organic solvent is a polar organic solvent.

Description

technical field [0001] The present invention relates to a dispersion containing a refractory polymer, a refractory fiber obtained by shaping the refractory fiber, and a carbon fiber obtained by carbonizing the refractory fiber. Background technique [0002] Due to the excellent heat resistance and flame retardancy of the refractory fiber, it is used, for example, as a welding protection sheet to protect the human body from high-heat iron powder or welding sparks scattered during welding operations, etc., or as a fireproof and heat insulating material for aircraft, etc. Widely utilized, the demand for refractory fibers in these fields is increasing. [0003] In addition, refractory fibers are also important as intermediate raw materials for obtaining carbon fibers. Carbon fiber is widely used in various applications due to its excellent mechanical properties, chemical properties, and light weight, such as aviation and aerospace materials for aircraft or rockets, sporting goo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L33/20D01F6/18D01F9/22
CPCD01F9/22C09D133/18D01F6/18C08L2201/02C08K5/0066C08K5/0091C08K5/092C08K5/095C08K5/098C08L2203/12
Inventor 须藤真史川上大辅石田富弘
Owner TORAY IND INC