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Modified poly(p-phenylenebenzobisoxazole) and preparation thereof

A technology of benzobisoxazole and poly-p-phenylene is applied in the field of modified PBO polymer and its preparation, which can solve the problems of application limitation, weak fiber interaction force, etc., so as to increase the interaction force and improve the surface activity. , the effect of excellent mechanical properties and thermal stability

Inactive Publication Date: 2008-10-08
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, PBO fiber is a rigid rod-shaped polymer with a smooth surface and weak interaction between fibers, which greatly limits its application in composite materials.

Method used

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  • Modified poly(p-phenylenebenzobisoxazole) and preparation thereof
  • Modified poly(p-phenylenebenzobisoxazole) and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] When equipped with stirring device, N 2 Import and export, the capacity is 1L in the reactor, first pass high-purity N 2 Displacing the air, at N 2 Under protection, 30g 4,6-diaminoresorcinol hydrochloride (DAR), 22.2112g terephthalic acid (TPA), 1.3944g 2,5-dihydroxyterephthalic acid (DHTA), 172.9530g more Polyphosphoric acid (P 2 o 5 Concentration is 80wt%) and 96.9777g P 2 o 5 , Seal the reactor.

[0019] Raise the temperature of the reaction materials in the reactor to 50°C and keep for 1 hour to make the materials mix initially, then slowly raise the temperature to 65°C and keep for 1 hour to further dissolve the materials;

[0020] Fill the reaction kettle with dry inert gas to make the pressure in the reaction kettle reach 0.4MPa, raise the temperature to 110°C at the same time, keep it for 7 hours, open the pressure relief valve, and remove the pressure in the reaction kettle.

[0021] Then the reaction material is heated up to 150°C and evacuated to 20Pa...

Embodiment 2

[0027] Adopt the method described in Example 1 to carry out polymerization and spinning, the difference is that the addition of material is: 30g 4,6-diaminoresorcinol hydrochloride (DAR), 21.0423g terephthalic acid (TPA), 2.78873g2,5-dihydroxyterephthalic acid (DHTA), 178.1595g polyphosphoric acid (P 2 o 5 Concentration is 80wt%) and 103.2793g P 2 o 5 .

[0028] [η] of the polymerization product = 27 dL / g. FTIR analysis results (KBr pellet method, cm -1 ): 3096, 2922, 2852, 1620, 1557, 1494, 1410, 1363, 1306, 1274, 1231, 1193, 1140, 1111, 1053, 1008, 913, 852, 821, 752, 704, 500. Elemental analysis results: The theoretical values ​​of each element content are: C: 70.83%, H: 2.53%, N: 11.80%; the experimental values ​​are C: 64.85%, H: 2.79%, N: 10.70%.

[0029] Wherein: m=12, n=104, number average molecular weight is 27433;

[0030] The polymer solution is prepared into fibers with a fineness of 2.4dtex through a screw extruder using a dry jet wet spinning process, the ...

Embodiment 3

[0032] Adopt the method described in Example 1 to carry out polymerization and spinning, the difference is that the addition of material is: 30g 4,6-diaminoresorcinol hydrochloride (DAR), 11.6901g terephthalic acid (TPA), 13.9437g2,5-dihydroxyterephthalic acid (DHTA), 137.8115g polyphosphoric acid (P 2 o 5 Concentration is 80wt%) and 87.6923gP 2 o 5 .

[0033] [η] of the polymerization product = 21.9 dL / g. FTIR analysis results (KBr pellet method, cm -1 ): 3440, 2922, 1628, 1572, 1494, 1412, 1366, 1230, 1193, 1112, 1059, 1012, 918, 867, 805, 755, 705, 514. Elemental analysis results: The theoretical values ​​of each element content are: C: 67.20%, H: 2.40%, N: 11.20%; the experimental values ​​are C: 51.62%, H: 2.90%, N: 8.56%.

[0034] Wherein: m=49, n=49, number average molecular weight is 24421;

[0035] The polymer solution is prepared into fibers with a fineness of 2.3dtex through a screw extruder using a dry jet wet spinning process, the tensile strength is 25.0cN...

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Abstract

The invention provides a modified poly(p-phenylenebenzobisoxazole) and the preparation method. The preparation method is characterized in that the method comprises the following steps: 4,6-diaminoresorcinol dihydrochloride, terephthalic acid, 2,5-dihydroxyterephthalic acid are heated and dissolved in poly-phosphate (PPA) and then reacted for 5 to 7 hours in 0.2-1.0MPa at 110-120 DEG C; then after the reaction pressure is removed and the HCL generated in the reaction is removed, the mixture in the reactor is reacted for 6 to 7 hours in vacuum at 140-150 DEG C and in 20-100Pa so as to get the serum of the polymer. The serum can be directly used as spinning serum and can be extruded by a single or twin-screw extruder; the fibers prepared through dry-jet wet spinning technology has high surfactivity and strong interface adhesive force between resin matrix so as to improve the interface shear strength between the resin. See the molecular structure.

Description

technical field [0001] The invention relates to a modified PBO polymer with significantly improved interfacial adhesion performance and a preparation method thereof. Background technique [0002] In the 1960s, the successful development of poly-p-phenylene terephthalate (PPTA) fibers set off a research boom in high-performance fibers. Through molecular design and liquid crystal spinning technology, various high-performance fibers with excellent properties have been continuously developed. High-performance fibers prepared from aromatic heterocyclic polymers represented by poly-p-phenylenebenzobisoxazole (PBO) It is the best among them. [0003] Based on the research of the U.S. Air Force Materials Laboratory and Dow Chemical Company, Japan Toyobo successfully realized the industrial production of PBO fiber in the 1990s, and its trade name was "Zylon". Zylon has a tensile strength of 5.8GPa and a tensile modulus of 300GPa, twice that of PPTA fibers, respectively. In additio...

Claims

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Application Information

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IPC IPC(8): C08G73/22D01F6/78
Inventor 金俊弘杨胜林江建明张涛李光
Owner DONGHUA UNIV