Thermosetting polyimide resin and preparation method thereof

A technology of polyimide resin and maleimide-based polyimide resin, applied in the direction of adhesives, etc., can solve the problems that have not yet been published in literature or patent reports, and achieve low cost, easy molecular weight, and good reaction conditions mild effect

Inactive Publication Date: 2010-12-22
DONGHUA UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The thermosetting polyimide resin disclosed by the present invention and

Method used

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  • Thermosetting polyimide resin and preparation method thereof
  • Thermosetting polyimide resin and preparation method thereof
  • Thermosetting polyimide resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Put 44.1 grams (0.1 moles) of 2,2-bis[4-(2,4-diaminophenoxy)phenyl] propane and 285.0 grams of N-methyl-2-pyrrolidone organic solvent into the reaction kettle, room temperature After stirring and dissolving completely, add 19.6 grams (0.2 moles) of maleic anhydride solid powder, stir at room temperature until completely dissolved, continue stirring for 0.5 hours, add 31.0 grams (0.1 moles) of 3,3',4,4' -Tetracarboxydiphenyl ether dianhydride, stirring and reacting at room temperature for 5-8 hours to obtain a homogeneous transparent viscous resin solution, adding 142.5 grams of toluene azeotropic dehydrating agent, azeotropic reflux, water separation and stirring for 6-8 hours , Separate the toluene azeotropic dehydrating agent to obtain a homogeneous transparent viscous maleimide-based polyimide resin liquid with a solid content of 25 wt%, namely component A.

[0058] 264.3 grams (0.6 moles) of 2,2-bis[4-(2,4-diaminophenoxy)phenyl]propane and 750.0 grams of N-methyl-2-...

Embodiment 2

[0064] 48.5 grams (0.11 moles) of 2,2-bis[4-(2,4-diaminophenoxy)phenyl]propane and 1004.0 grams of N,N-dimethylacetamide organic solvent are put into the reactor, At room temperature, after stirring and dissolving completely, add 21.6 grams (0.22 moles) of maleic anhydride solid powder, stir at room temperature until completely dissolved, continue stirring for 0.5 hours, then add 15.5 grams (0.05 moles) of 3,3', 4,4 '-Tetracarboxydiphenyl ether dianhydride and 26.0 grams (0.05 moles) of 2,2-bis[4-(3,4-dicarboxyphenoxy)phenyl]propane dianhydride, stirred at room temperature for 5-8 hours , to obtain a homogeneous transparent viscous resin solution, add 502.0 grams of toluene azeotropic dehydrating agent, azeotropic reflux, water separation and stirring reaction for 6-8 hours, separate the toluene azeotropic dehydrating agent to obtain a homogeneous transparent viscous The maleimide-based polyimide resin liquid has a solid content of 10wt%, that is, component A.

[0065] 264.3 ...

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Abstract

The invention relates to a thermosetting polyimide resin and a preparation method thereof. A homogeneous transparent sticky maleimide-based polyimide resin solution is taken as a component A, and a 4-maleimide-based bisphenol solution A is taken as a component B. The preparation method of the thermosetting polyimide resin comprises the following steps: (1) preparing the maleimide-based polyimide resin solution as the component A; (2) preparing the 4-maleimide-based bisphenol solution A as the component B; and (3) uniformly mixing the component A and the component B at room temperature to obtain the thermosetting polyimide resin. The thermosetting polyimide resin of the invention not only can be applied to the matrix resin of high temperature resistant adhesives and glass fiber reinforced composite materials but also can be applied to the matrix resin of high-performance fiber (carbon fiber, aramid fiber and the like) reinforced advanced composite materials, thus the thermosetting polyimide resin has wide application prospects; and the invention has simple preparation technology, low cost and environmental protection, can finish preparation processes in the general equipment, and is suitable for industrial production.

Description

technical field [0001] 本发明属于高分子新材料及其制备领域,特别是涉及一种热固性聚酰亚胺树脂及其制备方法。 Background technique [0002] 复合材料的应用被认为是飞机、火箭、导弹等飞行器减重的一个重要解决方案,因此,在航空航天领域中的应用相当广泛。随着飞行速度的提高,对复合材料的综合性能提出更高的要求,尤其是耐高温性。 [0003] 纤维增强树脂基复合材料具有比强度高、吸湿性小、尺寸稳定性好、介电性能优良、微波透过率高以及制品结构可设计性强等优点.。复合材料的耐高温性能主要取决于基体树脂,因此,开发耐高温的基体树脂极为关键。 [0004] 聚酰亚胺是一类综合性能非常优异的高分子材料,具有特别优异的耐热性、耐低温性、阻燃性、电气性能和力学性能,被广泛地应用于电子微电子、航空航天、激光、光电等高科技领域。 [0005] 有关聚酰亚胺树脂领域的研究开发工作已有不少报道: [0006] 中国发明专利CN1927908A公开了一种含酚羟基聚酰亚胺粉末的制备方法,其主要特征在于:(1)摩尔比为1∶1的含酚羟基芳香族二元胺化合物或含酚羟基芳香族二元胺与其它二元胺的混合物和芳香族二元酐在强极性非质子有机溶剂中,氮气保护下,于0℃~30℃下反应3~12小时后,得到透明粘稠的聚羟基酰胺酸溶液,其中,强极性非质子有机溶剂占整个反应体系的质量百分数为5%~30%;(2)氮气气氛中,加入共沸脱水剂,加热升温,于120℃~160℃的温度范围内,回流共沸脱水亚胺化反应5~18小时,冷却至室温,过滤,洗涤,真空干燥,得到含酚羟基聚酰亚胺粉末,其中,共沸脱水剂与强极性非质子有机溶剂的体积比为0.1~10∶1。 [0007] 虞鑫海等人【耐高温单组分环氧胶粘剂的研制,粘接,2008,29(12):16-19】公开了耐高温单组分环氧胶粘剂的制备方法,其主要特征在于:以马来酸酐(MA)为封端剂,以2,2-双(3-氨基-4-羟基苯基)六氟丙烷(BAHPFP)、2,2-双[4-(4-氨基苯氧基)苯基]丙烷(BAPOPP)、2,2-双[4-(3,4-二羧基苯氧基)苯基]丙烷二酐(BPADA)为主原料合成得到了含酚羟基的聚醚酰亚胺树脂(HPEI);以所合成得到的HPEI为耐高温增韧剂,与N,N,N′,N’-四缩水甘油...

Claims

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Application Information

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IPC IPC(8): C08L79/08C08K5/3415C08G73/12C09J179/08
Inventor 虞鑫海陈梅芳
Owner DONGHUA UNIV
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