A low-viscosity high-heat-resistant polyimide fiber sizing agent and its preparation method

A technology of polyimide fiber and setting agent, which is applied in the direction of carbon fiber, fiber treatment, heating/cooling fabric, etc., can solve the problem of unclear specific composition of foaming powder, insufficient fluidity and heat resistance, and reduced material heat resistance. and other problems, to achieve the effect of improving operability and efficiency, low viscosity, and simple preparation method

Active Publication Date: 2021-03-26
AVIC BEIJING INST OF AERONAUTICAL MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN201110376947.9 discloses a method for setting the shape of fiber-reinforced composite materials. The invention uses polyimide foaming powder composed of polytetraacid diester diammonium salt or polyamic acid as the setting agent, but does not specify the setting method. The specific composition of the foaming powder, in addition, this kind of foaming powder is also thermoplastic polyimide after imidization, also has the problem of insufficient fluidity and heat resistance, which is easy to cause defects inside the composite material and reduce the material overall heat resistance

Method used

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  • A low-viscosity high-heat-resistant polyimide fiber sizing agent and its preparation method
  • A low-viscosity high-heat-resistant polyimide fiber sizing agent and its preparation method
  • A low-viscosity high-heat-resistant polyimide fiber sizing agent and its preparation method

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Experimental program
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Effect test

Embodiment 1

[0040]At room temperature, 23.11g (78.55mmol) of 2,3,3',4'-biphenyltetralic dianhydride and 53.37g (215mmol) of 4-phenylethynylphthalic anhydride were added to a 500mL single-necked bottle, and 85g of Methanol. The above mixed solution was heated to reflux, and after the solution was clarified, it was kept under reflux for 2.5h. Cool the solution to room temperature, add 12.07g (111.63mmol) of m-phenylenediamine and 14.90g (74.42mmol) of 3,4'-diaminodiphenyl ether, and add 18g of methanol to adjust the solid content of the solution to 50wt %. React at room temperature for 6 hours to obtain a fixative solution. The solution was distilled under reduced pressure at 40° C. to obtain a concentrated fixative solution. Molecular weight: 900 g / mol.

[0041] The concentrated fixative solution was placed in a vacuum oven at 80°C (pressure lower than -0.095MPa) for 6 hours, and solid fixative lumps were obtained after cooling down.

[0042] Crush the above-mentioned sizing agent blo...

Embodiment 2

[0044] At room temperature, add 12.03g (40.88mmol) of 2,3,3',4'-biphenyltetralic dianhydride and 124.12g (500mmol) of 4-phenylethynylphthalic anhydride in a 500mL one-necked bottle, and add 224g of ethanol. The above mixed solution was heated to reflux, and after the solution was clarified, it was kept under reflux for 3h. The solution was cooled to room temperature, and 46.58 g (145.44 mmol) of 2,2'-bistrifluoromethyl-4,4'-diaminobiphenyl and 42.5 g (145.44 mmol) of 1,3-bis(4-amino phenoxy)benzene, and add 51g of ethanol to adjust the solid content of the solution to 45wt%. React at room temperature for 8 hours to obtain a fixative solution. The solution was distilled under reduced pressure at 40° C. to obtain a concentrated fixative solution. Molecular weight: 859 g / mol.

[0045] The concentrated fixative solution was placed in a 90°C vacuum oven (pressure lower than -0.095MPa) for 4 hours, and a solid fixative block was obtained after cooling down.

[0046] The above-m...

Embodiment 3

[0048] At room temperature, 136.53 g (550 mmol) of 4-phenylethynylphthalic anhydride and 190 g of ethanol were added to a 500 mL single-necked bottle. The above mixed solution was heated to reflux, and after the solution was clarified, it was kept under reflux for 3h. The solution is down to room temperature, add 17.84g (165.00mmol) of m-phenylenediamine and 32.16g (110mmol) of 1,3-bis(4-aminophenoxy)benzene, and add 12g of methanol, the solution solid content Adjusted to 50wt%. React at room temperature for 6 hours to obtain a fixative solution. Molecular weight: 642 g / mol.

[0049] The solution was distilled under reduced pressure at 40° C. to obtain a concentrated fixative solution. The concentrated fixative solution was placed in a vacuum oven at 80°C (pressure lower than -0.095MPa) for 6 hours, and solid fixative lumps were obtained after cooling down.

[0050] Crush the above-mentioned sizing agent block to 200 mesh, sprinkle it evenly on the surface of the carbon fi...

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Abstract

The invention belongs to the field of composite material fiber shaping agent materials and relates to a low-viscosity high-thermal resistant polyimide fiber shaping agent and a preparation method thereof. The shaping agent is of a structure with amido acid, monoester carboxylic acid ammonium salt and imide, 4-phenylacetylene phthalic anhydride is adopted as an end sealing agent, nonlinear mixed diamine and 2,3,3',4'-biphenyl dianhydride are adopted as monomers, and the molecular weight is optimized. The shaping agent is prepared through two steps of shaping agent solution synthesis and thermaltreatment, the preparation method is simple and high in preparation efficiency, has a good fiber shaping effect, fiber viscosity, manufacturability and thermal resistance and can be applied to shaping processes such as high-temperature resistant polyimide resin-based composite material resin transfer molding (RTM).

Description

technical field [0001] The invention belongs to the field of composite fiber sizing agent materials, and relates to a low-viscosity, high-heat-resistant polyimide sizing agent and a preparation method thereof. Background technique [0002] The heat resistance of polyimide resin-based composite materials can reach more than 280°C, which is the highest temperature-resistant composite material at present, so it has great application value in high-tech fields such as aerospace. As an alternative or supplementary process to the hot pressing process, liquid molding processes such as polyimide composite resin transfer molding (RTM) have the advantages of relatively simple process, low production cost, complex components, high component integrity and short process cycle. Etc. The liquid molding process includes key links such as preform preparation, resin injection and composite material curing. For laminated composite components, the prefabricated body is usually laid by dry fibe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D06M15/59C08G73/10D06C7/02D06M101/40
CPCC08G73/1007C08G73/1039C08G73/1071D06C7/02D06M15/59D06M2101/40
Inventor 倪洪江邢宇戴霄翔刘燕峰李军张代军陈祥宝
Owner AVIC BEIJING INST OF AERONAUTICAL MATERIALS
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