Thermoplastic fluorine-containing fully aromatic polyimide powder and preparation method thereof

A polyimide powder, thermoplastic technology, applied in the field of thermoplastic fluorine-containing peraromatic polyimide powder and its preparation, can solve problems such as unpublished literature or patent reports, and achieve good application prospects and environmental friendliness , the effect of mild reaction conditions

Inactive Publication Date: 2009-10-21
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The molecular structure and preparation method of the thermoplastic fluorine-containing peraromatic polyimide powder disclosed by the present invention have not yet been published in the literature or patent reports

Method used

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  • Thermoplastic fluorine-containing fully aromatic polyimide powder and preparation method thereof
  • Thermoplastic fluorine-containing fully aromatic polyimide powder and preparation method thereof
  • Thermoplastic fluorine-containing fully aromatic polyimide powder and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0072] 65.4 grams (0.1 moles) of 2,2-bis[4-(2-trifluoromethyl-4-aminophenoxy)phenyl]hexafluoropropane (BAPFP-2TF), 52.0 grams (0.1 moles) of 2 , 2-bis[4-(3,4-dicarboxyphenoxy) phenyl] propane dianhydride (BPADA), 0.005 mole isoquinoline and 1308 gram o-cresol are put into reactor, stir, heat up to Within the temperature range of 100°C-180°C, after maintaining the reaction for 5 hours, pour it into 13080 grams of ethanol precipitant under high-speed stirring state while it is hot, and precipitate solid powder, filter, wash with ethanol 2-3 times, soak in acetone 5 hours, filter, wash with deionized water 2-3 times, dry, obtain 111.5 grams of BAPFP-2TF / BPADA-PI thermoplastic fluorine-containing fully aromatic polyimide white powder (theoretical amount 113.8 grams), yield is 98% , the glass transition temperature is 189.5°C, and its Fourier transform infrared spectrum (FTIR) is as follows figure 2 shown.

[0073] The molecular structural formula of BAPFP-2TF / BPADA-PI thermopla...

Embodiment 2

[0076] 54.7 grams (0.1 moles) of 2,2-bis[4-(2-trifluoromethyl-4-aminophenoxy)phenyl]propane (BAPP-2TF), 52.0 grams (0.1 moles) of 2,2 -Bis[4-(3,4-dicarboxyphenoxy)phenyl]propanedianhydride (BPADA), 0.001 mole of isoquinoline and 274 grams of o-cresol were put into the reaction kettle, stirred, and heated to 100°C Within the temperature range of -180°C, after maintaining the reaction for 10 hours, pour it into 1370 grams of methanol precipitant under high-speed stirring state while it is hot, and precipitate solid powder, filter, wash with isopropanol 2-3 times, soak in acetone 5 hours, filter, wash 2-3 times with deionized water, dry, obtain 102.1 grams of BAPP-2TF / BPADA-PI thermoplastic fluorine-containing fully aromatic polyimide white powder (theoretical amount 103.1 grams), yield is 99% , the glass transition temperature is 192.2°C, and its Fourier transform infrared spectrum (FTIR) is as follows image 3 shown.

[0077] The molecular structural formula of BAPP-2TF / BPADA...

Embodiment 3

[0080] 50.4 grams (0.1 moles) of 4,4'-bis(2-trifluoromethyl-4-aminophenoxy)biphenyl (DABP-2TF), 52.0 grams (0.1 moles) of 2,2-bis[4 -(3,4-dicarboxyphenoxy)phenyl]propane dianhydride (BPADA), 0.001 mole of isoquinoline, 0.009 mole of pyridine and 600 grams of o-cresol were put into the reaction kettle, stirred, and heated to 100°C In the temperature range of -180°C, after maintaining the reaction for 8 hours, pour it into 30,000 grams of isopropanol precipitant under high-speed stirring state while it is hot, and precipitate solid powder, filter, wash with isopropanol for 2-3 times, acetone soaked in medium for 5 hours, filtered, washed with deionized water for 2-3 times, and dried to obtain 93.8 grams of DABP-2TF / BPADA-PI thermoplastic fluorine-containing fully aromatic polyimide white powder (theoretical amount 98.8 grams), the yield is 95%, the glass transition temperature is 219.7 ° C, and its Fourier transform infrared spectrum (FTIR) is as follows Figure 4 shown.

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Abstract

The invention relates to thermoplastic fluorine-containing fully aromatic polyimide powder, which has a general molecular structural formula shown above, wherein -R1 is a divalent linking group of fluorine-containing aromatic primary diamine; and -R2 is a divalent linking group of a molecule of aromatic acid dianhydride. The method comprises the following steps: reacting the fluorine-containing aromatic primary diamine with the aromatic acid dianhydride in a phenol solvent in the presence of a catalyst for 5 to 10 hours; pouring the hot solution in a precipitator with high-speed stirring to precipitate solid powder; and obtaining the thermoplastic fluorine-containing fully aromatic polyimide powder after filtration, washing, soaking, filtration and drying. The thermoplastic fluorine-containing fully aromatic polyimide powder has good solubility, is a high-performance heat-resistance toughness modifier for epoxy resin, unsaturated polyimide resin, unsaturated polyester resin and other thermosetting resins, and is good in application prospect, simple in operation, low in cost, environmentally-friendly, and suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of fluorine-containing polyimide and its preparation, and in particular relates to a thermoplastic fluorine-containing fully aromatic polyimide powder and a preparation method thereof. Background technique [0002] Polyimide is a kind of polymer material with excellent comprehensive properties. It has particularly excellent heat resistance, low temperature resistance, flame retardancy, electrical properties and mechanical properties. It is widely used in electronic microelectronics, aerospace, High-tech fields such as lasers and optoelectronics. [0003] Polyimide itself can not only prepare films, fibers, engineering plastics, adhesives, coatings, etc., but also can be used as thermosetting resins (such as epoxy resins, bismaleimide resins, unsaturated polyesters, etc.) or containing High temperature toughening modifier for polymer system of thermosetting resin. [0004] Chinese invention patent CN1927908A disclose...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10
Inventor 虞鑫海
Owner DONGHUA UNIV
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