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Preparation and application of hydroxyl modified poly-p-phenylene benzo imidazolinyl resin

A technology of benzodiimidazole and hydroxyterephthalic acid, which is applied in the preparation and application field of a class of hydroxyl-modified poly-p-phenylene benzodiimidazole resins, can solve the problems that the mechanical properties are not as good as PBO, etc., and achieve improved compression Strength and surface polarity, good adhesion, excellent heat resistance and flame resistance

Active Publication Date: 2012-07-04
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the addition of some N-H...N hydrogen bonds between PBI molecular chains, the compressive performance is better than PBO, but the mechanical properties are still not as good as PBO

Method used

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  • Preparation and application of hydroxyl modified poly-p-phenylene benzo imidazolinyl resin
  • Preparation and application of hydroxyl modified poly-p-phenylene benzo imidazolinyl resin
  • Preparation and application of hydroxyl modified poly-p-phenylene benzo imidazolinyl resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Embodiment 1: Poly 1,4-(2,5-dihydroxy)phenylene-2,6-benzodiimidazole new resin (PDBI) prepares (1,2,4,5-tetraaminobenzene hydrochloride Mixed polycondensation with 2,5-dihydroxyterephthalic acid)

[0057] Add P sequentially into the glass polymerization reactor 2 o 5 6.0g and P 2 o 5 18.0g (PPA) of polyphosphoric acid with a mass concentration of 80% was heated up to 100°C and stirred for 1 hour until it became clear and transparent to form a polyphosphoric acid containing 85.0% PPA. 2 o 5 Add 1.57 g (0.0055 mol) of 1,2,4,5-tetraaminobenzene hydrochloride (TAB 4HCl) after passing through nitrogen for a little cooling, heat up to 100°C, stir to remove HCl gas for 5 hours, and turn pink Opaque solution, add 1.1g (0.0055mol) of 2,5-dihydroxyterephthalic acid (2,5-DHTA) at this time, the mass percentage concentration (ω) of two monomers TAB 4HCl and 2,5-DHTA 10.0% (corresponding to the molar concentration of monomer 0.023mol / 100g PPA), it turns into a yellow turbid li...

Embodiment 2

[0058] PDBI resin infrared see figure 1 , the relevant characteristic peaks and their attribution analysis are: 1623.4 (s) imidazole C=N peak, 1575.8 (s) benzene ring C=C peak, 197.2 (s) heterocycle absorption, 1429.0, 1248.1, 1086.7 (s) benzene ring C-C Skeleton peak, 1346.1 (s) C-N peak of imidazole, 877.5, 736.7 (s) C-H on benzene ring. In addition, in this batch there is also free state OH-. Due to the effect of intramolecular hydrogen bonds, the stretching vibration peak of -OH moves to a lower wave number and becomes wider, which is 3189.9 (s). According to thermogravimetric analysis, the temperature at 10% weight loss is 550°C, and the temperature corresponding to the maximum decomposition rate is 665.12°C. Embodiment 2PDBI as-spun fiber (the application of resin-the direct wire-drawing method of the PPA liquid crystal stock solution of new resin PDBI)

[0059] The same as the operation of preparing PDBI by polycondensation reaction in Example 1, the PDBI resin liquid...

Embodiment 3

[0061] The condition scope of embodiment 3PDBI new resin preparation and application

[0062] On the basis that the molar ratio of TAB 4HCl and DHTA is 1:1, change the monomer molar concentration C (mol / 100g PPA), reaction temperature T (℃) and reaction time t (h) in Example 1, according to the example The operation steps of 1 were used to prepare new PDBI resins under different process conditions. First, the method of obtaining primary fibers in Example 2 was used to take out part of the PDBI monofilament fibers and measure their tensile strength, and then the remaining PDBI resin liquid crystal stock solution was prepared according to Example 1. The PDBI resin was obtained by water washing, post-neutralization treatment and drying, and its intrinsic viscosity was measured. The results are shown in Table 1.

[0063] Table 1 Properties of PDBI resin and PDBI monofilament fiber

[0064]

[0065] *Total yield including removal of PDBI monofilament fibers

[0066] **The concen...

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Abstract

The invention provides a preparation method of hydroxyl modified poly-p-phenylene benzo imidazolinyl resin and application of the resin in high performance fiber preparation. 1,2,4,5-tetraaminobenzene hydrochloride and two hydroxy terephthalic acid are utilized as raw materials, hydrogen chloride is desorbed from polyphosphoric acid, and the hydroxyl modified resin is prepared by temperature programming mixed with polycondensation. The resin can be applied to spinning processing and made into high performance fiber, particularly poly-1, 4-(2, 5-dyhydroxy) phenylene-2, 6-benzo diimidazole resin can directly utilize poly phosphoric acid liquid crystal basic solution when polymerization is finished to conduct manual wire drawing or dry-jet wet spinning to obtain poly-1, 4-(2, 5-dyhydroxy) phenylene-2, 6-benzo diimidazole fiber, compression and composite adhesive performance of the fiber are improved, and production cost is reduced. The preparation method and the application provide a new way for replacing PBO and M5 fiber to implement commercialization production of the high-performance fiber and developing research direction of high-technology materials.

Description

(1) Technical field [0001] The invention relates to the preparation of a class of hydroxyl-modified poly-p-phenylene benzodiimidazole resin and its application in high-performance fibers. (2) Background technology [0002] PBO is the abbreviation of cis-poly(p-phenylene-2,6-benzobis-oxazole), and its fiber is a kind of organic fiber with high strength, high modulus and low density. , has excellent thermal stability and flame retardant properties. Zylon-HM fiber, its comprehensive performance (5.8GPa tensile strength, 270GPa modulus, 68 limiting oxygen index and 650 ° C decomposition temperature) has fully exceeded Kevlar-49, so As a new material in the fields of aerospace, national defense and military and its special civil use, it has also attracted much attention from research departments and industries. PBO fiber is originally composed of AA-type monomer 4,6-diaminoresorcinol hydrochloride (DAR·2HCl) and BB monomer terephthalic acid (TPA) first contain 85% P 2 o 5 Poly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/18D01F6/74C08J5/04
Inventor 金宁人张建庭赵德明何彪侯晓华
Owner ZHEJIANG UNIV OF TECH
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