Preparation method of polybenzimidazole polymer with high molecular weight and high solubility

A technology of polybenzimidazoles and polymers, which is applied in the field of preparation of polybenzimidazoles polymers, can solve the troublesome processing technology, the solubility problem of polybenzimidazoles polymers is not well solved, and affects the material Performance and other issues

Pending Publication Date: 2021-08-24
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are many methods for preparing polybenzimidazole polymers, but the solubility problem of high molecular weight polybenzimidazole polymers has not been solved well. Although, with the help of cosolvent (LiCl), It can be dissolved in strong polar solvents (such as DMAC, DMF, DMSO, etc.), but the existence of co-solvents will bring some troubles to the subsequent processing of materials. The co-solvents need to be removed in the subsequent processing processes, and need to be washed and dried. And other procedures, but also affect the performance of the material (the removal of LiCl will affect the compactness of the material, and the residual LiCl will also affect the performance of the material)

Method used

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  • Preparation method of polybenzimidazole polymer with high molecular weight and high solubility
  • Preparation method of polybenzimidazole polymer with high molecular weight and high solubility
  • Preparation method of polybenzimidazole polymer with high molecular weight and high solubility

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preparation example Construction

[0056] The present invention provides a kind of preparation method of polybenzimidazole polymer of high molecular weight and high solubility, specifically, the method of the present invention comprises: use tetramine compound A and dicarboxylate phenyl ester compound B, in catalyst C and In the presence of arylphenol D, polybenzimidazole polymers are prepared by two-step high-temperature condensation under the protection of nitrogen flow.

[0057] Wherein, the molar ratio of tetramine compound A to phenyl dicarboxylate compound B is 1:0.6-1.5 (preferably 1:1); the amount of catalyst C is the total mass of tetramine compound A and phenyl dicarboxylate compound B 0.01%-5%; the amount of arylphenol D is 1%-500% of the total mass of tetraamine compound A and dicarboxylate phenyl compound B.

[0058] In the stepwise polymerization, the reaction temperature of the first step is 180°C-300°C, and the reaction temperature of the second step is 240°C-450°C.

[0059] In a preferred embo...

Embodiment 1

[0085] Preparation of m-PBI:

[0086]

[0087] Add biphenyltetramine (21.43g, 100mmol), diphenyl isophthalate (31.83g, 100mmol), triphenyl phosphite (53.3mg), phenol (26.63g) then vacuumize, change nitrogen, repeat operation three times. Start heating, and start stirring when the solid turns into a solution state. At the same time, turn on the nitrogen flow (flow rate is 500mL / min), heat to 270°C for reaction, and when the viscosity of the system is very high (stirring is difficult), stop stirring and continue the reaction for 2 hours. , stop responding. After cooling to room temperature, the obtained solid prepolymer was pulverized into a fine powder. Add the pulverized prepolymer fine powder into the reaction kettle again, then evacuate, change nitrogen, and repeat the operation three times. Under the protection of nitrogen flow (flow rate of 500 mL / min), heating was started, heated to 380° C. for 2 hours to obtain m-PBI. The polymer’s Mw=243265, molecular weight dist...

Embodiment 2

[0089] Preparation of m-PBI:

[0090]

[0091] Add biphenyltetramine (21.43g, 100mmol), diphenyl isophthalate (31.83g, 100mmol), diphenyl phosphite (266.3mg), o- Cresol (53.26g) is then vacuumized, and nitrogen is changed, and the operation is repeated three times. Start heating, and start stirring when the solid turns into a solution state. At the same time, turn on the nitrogen flow (flow rate is 250mL / min), and heat to 260°C for reaction. When the viscosity of the system is very high (stirring is difficult), stop stirring and continue the reaction for 1.5 hours. , stop responding. After cooling to room temperature, the obtained solid prepolymer was pulverized into a fine powder. Add the pulverized prepolymer fine powder into the reaction kettle again, then evacuate, change nitrogen, and repeat the operation three times. Under the protection of nitrogen flow (flow rate of 250 mL / min), heating was started, heated to 360° C. and reacted for 2 hours to obtain m-PBI. The ...

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Abstract

The invention provides a preparation method of a polybenzimidazole polymer with high molecular weight and high solubility. The method comprises the following steps: in the presence of a catalyst and aryl phenol, adopting a tetramine compound and a phenyl dicarboxylate compound, and preparing the high-molecular-weight and high-solubility polybenzimidazole polymer in a two-step high-temperature condensation manner. The preparation method provided by the invention overcomes the problems of uncontrollable polymerization, harsh reaction conditions and the like in the existing polymerization method, and the obtained product has high molecular weight, high solubility and excellent processability, and is very suitable for wide processing and use.

Description

technical field [0001] The invention belongs to the field of engineering thermoplastics, and in particular relates to a preparation method of a polybenzimidazole polymer with high molecular weight and high solubility. Background technique [0002] Polybenzimidazole polymers are the most high-end engineering thermoplastics today, and are currently the materials with the highest temperature resistance in plastics. They are thermosetting materials, have no melting point, can be used for a long time at a temperature of 400°C, and have the best mechanical properties, etc. advantage. Polybenzimidazole polymers are an ideal material for use in extreme high temperatures, harsh chemical and plasma environments, or applications requiring high product durability and wear resistance that other resins cannot meet. It has excellent flame resistance, radiation stability, mechanical stability, electrical insulation, chemical stability, thermal stability, oxidation resistance stability, tou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/06C08L79/04C08J5/18H01M8/103H01M8/1032
CPCC08G73/0677C08J5/18H01M8/103H01M8/1032C08J2379/04Y02E60/50
Inventor 何正标李铃春胡金波
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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