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Microwave synthesis of poly-2,2',5,5'-benzmidazole and poly-2,5-benzimidazole

A technology of microwave synthesis and benzimidazole, which is applied in the field of microwave synthesis of poly2, can solve the problems of difficult control of product polymerization degree and long time period, and achieve the effects of avoiding local overburning, fast heating speed and high efficiency

Inactive Publication Date: 2007-11-21
NORTHEASTERN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The liquid phase synthesis method is widely used, but this method takes a long time, usually 20 hours or even longer, and the degree of polymerization of the product is not easy to control

Method used

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  • Microwave synthesis of poly-2,2',5,5'-benzmidazole and poly-2,5-benzimidazole
  • Microwave synthesis of poly-2,2',5,5'-benzmidazole and poly-2,5-benzimidazole
  • Microwave synthesis of poly-2,2',5,5'-benzmidazole and poly-2,5-benzimidazole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) Add 50g polyphosphoric acid PPA (chemically pure, content: P 2 o 5 ≥80.0wt%), heated and stirred under nitrogen protection (flow rate: 45mL / min) to 140°C; accurately weighed 20mmol reactant 3,3'-diaminobenzidine (DAB 4HCl 2H 2(2, 97wt%) was slowly added in the round-bottomed flask, after it was dissolved and the HCl in it was volatilized completely, slowly added 20mmol of isophthalic acid (chemically pure, ≥99wt%);

[0037] (2) After stirring and mixing completely, move the reactant into a microwave oven, and program temperature rise: first 120°C, 2min; 140°C, 2min; 160°C, 2min; 170°C, 14min; then 180°C, 2min; Heating at 200°C for 154min, with a microwave power of 400W;

[0038] (3) The reaction product was poured into deionized water while it was hot, and there was obvious stringing phenomenon, and it was left to stand for 15 hours, washed with water until nearly neutral, and neutralized by adding saturated sodium bicarbonate solution;

[0039] (4) Suction filtr...

Embodiment 2

[0043] (1) Add 122g polyphosphoric acid PPA (chemically pure, content: P 2 o 5 ≥80.0wt%), heated and stirred under nitrogen protection (flow rate: 45mL / min) to 140°C; accurately weighed 48.8mmol reactant 3,3'-diaminobenzidine (DAB 4HCl 2H 2 (2, 97wt%) was slowly added in the round bottom flask, after it was dissolved and the HCl in it was volatilized completely, slowly added 48.8mmol of isophthalic acid (chemically pure, ≥99wt%);

[0044] (2) After stirring and mixing completely, move the reactant into a microwave oven, and program temperature rise: first 120°C, 2min; 140°C, 2min; 160°C, 2min; 170°C, 14min; then 180°C, 2min; Heating at 200°C for 68 minutes, the power of the microwave oven is 400W;

[0045] (3) The reaction product was poured into deionized water while it was hot, and there was obvious stringing phenomenon, and it was left to stand for 15 hours, washed with water until nearly neutral, and neutralized by adding saturated sodium bicarbonate solution;

[0046] ...

Embodiment 3

[0050] (1) Add 50g polyphosphoric acid PPA (chemically pure, content: P 2 o 5 ≥80.0wt%), heated and stirred under nitrogen protection (flow rate: 45mL / min) to 140°C; accurately weighed 20mmol reactant 3,3'-diaminobenzidine (DAB 4HCl 2H 2 (2, 97wt%) was slowly added in the round-bottomed flask, after it was dissolved and the HCl in it was volatilized completely, slowly added 20mmol of isophthalic acid (chemically pure, ≥99wt%);

[0051] (2) After the stirring and mixing are complete, move the reactant into a microwave oven, and program temperature rise: first 120°C, 2min; 140°C, 2min; 160°C, 2min; 170°C, 4min; then 180°C, 2min; Heating at 200°C for 76 minutes, with a microwave power of 400W;

[0052] (3) The reaction product was poured into deionized water while it was hot, and there was obvious stringing phenomenon, and it was left to stand for 15 hours, washed with water until nearly neutral, and neutralized by adding saturated sodium bicarbonate solution;

[0053] (4) Suc...

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Abstract

Microwave synthesis of poly-2, 2'-5, 5'-benzimidazole and poly-2, 5-benzimidazole are disclosed. The process of poly-2, 2'-5, 5'-benzimidazole is carried out by taking paraphosphoric acid PPA as solvent, condensation polymerizing under nitrogen protection, adding into 3,3'-diamino-benzidine, dissolving, adding into isophthalic acid, putting mixed liquid into microwave oven, programmed raising temperature at 300-500W, pouring reactant into deionized water, washing by water to become neutral, adding into saturated sodium bicarbonate solution, neutralizing, decompressing, extraction filtering, washing by water, washing by alcohol, drying and grinding into powders; process of poly-2, 5-benzimidazole is carried out by taking PPA as solvent, condensation polymerizing under nitrogen protection, agitating while heating to 200 degree, adding into 3, 4-diamino-benzoic acid, putting mixed liquid into microwave oven, programmed raising temperature at 300-500W, pouring reactant into deionized water, washing by water to become neutral, adding into caustic soda solution 1 mol / L, neutralizing, boiling at 100 degree for 6 hrs remove caustic soda, decompressing, extraction filtering, washing by water, washing by alcohol, drying and grinding into powders. It' efficient, has better radiant energy and shorter reactive time.

Description

technical field [0001] The invention relates to a method for synthesizing poly 2,2'-5,5'-benzimidazole and poly 2,5-benzimidazole by microwave. Background technique [0002] Poly 2,2'-5,5'-benzimidazole has good thermal stability and chemical stability, which is mainly due to the existence of conjugated aromatic heterocycles in the molecular chain, which maintains the arrangement of the polymer aromatic hexahedron structure, its glass transition temperature (Tg) can reach 480°C. In a nitrogen environment, the weight loss begins at 600°C, and the weight loss is 30% at 900°C. The above excellent properties make poly 2,2'-5,5'-benzimidazole suitable for high-temperature fibers, adhesives, lamination resins, heat insulation materials, fireproof materials and proton conductor membrane materials, etc. Among them, the bead-shaped poly 2,2'-5,5'-benzimidazole has the above-mentioned advantages. When in contact with liquid, the pore size and surface area increase dramatically, and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/18
Inventor 何荣桓孙宝英赵寒梅车全通杨景帅
Owner NORTHEASTERN UNIV
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