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Programmed heating type melt polymerization method for polybenzimidazole

A polybenzimidazole and temperature-programmed technology, applied in the field of polymer materials, can solve the problems of poor controllability of polybenzimidazole reaction degree and the like

Inactive Publication Date: 2014-04-09
BEIJING ZHONGJU TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to overcome the shortcomings of the poor controllability of the reaction degree of polybenzimidazole prepared by the traditional method, the present invention selects 3,3'-diaminobenzidine (DAB) and diphenyl isophthalate (DPIP) as polymerized monomers. Temperature rise method to control the melt polymerization process of polybenzimidazole, and determine the optimal reaction conditions by changing the reaction temperature of the second step

Method used

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  • Programmed heating type melt polymerization method for polybenzimidazole
  • Programmed heating type melt polymerization method for polybenzimidazole
  • Programmed heating type melt polymerization method for polybenzimidazole

Examples

Experimental program
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Effect test

Embodiment 1

[0023] The first step: the reaction monomer 3,3'-diaminobenzidine (DAB) 0.01-0.2mol (preferably 0.02mol) and diphenyl isophthalate (DPIP) 0.01-0.2mol ( Preferably 0.02mol) was added into a 1000mL three-neck flask equipped with a stirrer, nitrogen inlet and outlet, and the reaction flask was placed in an oil bath. The oil bath is heated and controlled at 160-180°C (preferably 180°C). Stir mechanically for 1-2h (preferably 2h) to melt the reaction mixture completely, and stop stirring when it is difficult to stir. Then the reaction mixture will slowly expand to a full bottle, and the reaction temperature will be maintained at 270-275°C (preferably 270°C) for 1-3h (preferably 3h), until no more phenol is discharged from the tail gas port, and the heating will be stopped. After cooling down to room temperature, the feeding of nitrogen gas was stopped, and the reaction mixture was taken out and ground to obtain a powdery prepolymer.

[0024] Step 2: Add the prepolymer powder into...

Embodiment 2

[0027] As described in the first step of Example 1, a powdery prepolymer was obtained.

[0028]Step 2: Add the prepolymer powder into a three-necked flask with a stirrer, nitrogen inlet and outlet, and heat it with an oil bath. Directly heated to 350°C for 3 hours, and after cooling down, the PBIb polymer can be obtained. The polymer was washed with absolute ethanol to remove residual phenol, and dried in a vacuum oven at 150°C for 24h.

[0029] The logarithmic reduced viscosity of the PBIb measured by the method described in Example 1 is 0.6675g.dl -1 , the thermal stability has been significantly improved, T d5％ and T d10％ They are 660°C and 715°C, respectively.

Embodiment 3

[0031] As described in the first step of Example 1, a powdery prepolymer was obtained.

[0032] In the second step, the prepolymer powder is added to a three-neck flask with a stirrer, nitrogen inlet and outlet, and the oil bath is still used for heating. Directly heat to 350°C for 3 hours, and after cooling down, the PBI polymer can be obtained. The polymer was washed with absolute ethanol to remove residual phenol, and dried in a vacuum oven at 150°C for 24h.

[0033] The logarithmic reduced viscosity of the PBIc measured by the method described in Example 1 is 0.7774g.dl -1 , the thermal stability has been significantly improved, T d5％ and T d10％ They are 670°C and 736°C, respectively.

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Abstract

The invention belongs to the field of polymer materials and specifically relates to a programmed heating type melt polymerization preparation method of polybenzimidazole. The polybenzimidazole is prepared by taking 3, 3'-diaminobenzidine (DAB) and diphenyl isophthalate (DPIP) as polymerization monomers and performing programmed heating type melt polymerization. The whole polymerization process is controlled by programmed heating and adjustment of reaction temperature in the second step, the polybenzimidazole with a controllable reaction degree is prepared, optimal polymerization conditions are further obtained, and a foundation is laid for preparing polybenzimidazole polymer materials with excellent performances.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to a temperature-programmed melting polymerization preparation method of polybenzimidazole. Background technique [0002] Polybenzimidazole (PBI) is a class of ladder-type polymers whose main chain contains repeated benzimidazole rings. Because the main chain of PBI contains benzimidazole, a conjugated aromatic heterocyclic structure, it has excellent thermal stability, mechanical properties and chemical stability, and it still has very good mechanical and electrical properties at 400 ° C. One of the most ideal matrix resins for high temperature composite materials. In addition, phosphoric acid doped polybenzimidazole is also one of the preferred materials for proton exchange membrane (PEM), especially in the study of medium and high temperature PEM, which shows unique advantages. The main reason is that in addition to its strong stability, the imidazole ring is an amp...

Claims

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Application Information

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IPC IPC(8): C08G73/18
Inventor 瞿翔宇漆奇
Owner BEIJING ZHONGJU TECH
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