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Method for preparing PBO (piperonyl butoxide) polymer by taking 2-(p-formylchloride phenyl)-5-amino-6-hydroxybenzoxazole as raw material

A technology of hydroxybenzoxazole and formyl chloride phenyl is applied in the field of preparation of PBO polymers, which can solve the problems of large amount of corrosive raw materials and long reaction period, and achieves avoiding poor solubility, reducing dosage and high reaction active effect

Active Publication Date: 2014-06-25
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve the problem that the existing method for synthesizing PBO polymers has a long reaction cycle and a large amount of corrosive raw materials, and provides 2-(p-formyl chloride phenyl)-5-amino-6-hydroxybenzene Oxazole is the method for raw material preparation PBO polymer

Method used

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  • Method for preparing PBO (piperonyl butoxide) polymer by taking 2-(p-formylchloride phenyl)-5-amino-6-hydroxybenzoxazole as raw material
  • Method for preparing PBO (piperonyl butoxide) polymer by taking 2-(p-formylchloride phenyl)-5-amino-6-hydroxybenzoxazole as raw material
  • Method for preparing PBO (piperonyl butoxide) polymer by taking 2-(p-formylchloride phenyl)-5-amino-6-hydroxybenzoxazole as raw material

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specific Embodiment approach 1

[0015] Specific embodiment one: the present embodiment takes 2-(p-formyl chloride phenyl)-5-amino-6-hydroxyl benzoxazole as the method for raw material preparation PBO polymer to implement according to the following steps:

[0016] 1. Under the protection of nitrogen, the P 2 o 5 Add it into the phosphoric acid solution, raise the temperature to 115-125°C, stir for 2 hours and cool down to 90°C to obtain a polyphosphoric acid solution;

[0017] 2. Under nitrogen protection, add AB type PBO monomer 2-(p-formyl chloride phenyl)-5-amino-6-hydroxybenzoxazole to the polyphosphoric acid solution in step 1 to prepare a PBO polymerization mixture , under full stirring, the PBO polymerization mixture was heated from 90°C to 120°C, and P was added continuously during the heating process. 2 o 5 , P in the control system 2 o 5 The mass percentage concentration is 80%~85%, obtains initial reaction liquid;

[0018] 3. Under the protection of nitrogen, the initial reaction liquid obtai...

specific Embodiment approach 2

[0023] Specific embodiment two: the difference between this embodiment and specific embodiment one is that the P in the polyphosphoric acid solution obtained in step one 2 o 5 The mass fraction is 80% to 85%. Other steps and parameters are the same as those in Embodiment 1.

[0024] The mass fraction described in this embodiment is by P 2 o 5 count.

specific Embodiment approach 3

[0025] Specific embodiment three: the difference between this embodiment and specific embodiment one or two is the AB type PBO monomer 2-(p-formyl chloride phenyl)-5-amino-6-hydroxybenzoxazole described in step two The preparation method is implemented according to the following steps:

[0026] 1. Under the protection of an inert gas, add 4,6-diaminoresorcinol hydrochloride to the ionic liquid at a molar ratio of 1: (2 to 4) to obtain a mixed solution A, and raise the temperature of the obtained mixture to 50 After stirring at ℃~90℃ for 100min~150min, the liquid mixture A is obtained;

[0027] Wherein, the ionic liquid described in step 1 is a disubstituted imidazole type N-methylimidazolium tetrafluoroborate ionic liquid;

[0028] 2. Under the protection of an inert gas, add terephthaloyl chloride to the liquid mixed solution A obtained in step 1 to obtain a mixed solution B, heat the obtained mixed solution B to 100°C-140°C and stir for 10h-18h, then Cool to room temperatu...

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Abstract

The invention relates to a method for preparing a PBO (piperonyl butoxide) polymer by taking 2-(p-formylchloride phenyl)-5-amino-6-hydroxybenzoxazole as raw material. The invention relates to a preparation method of a PBO polymer and aims at solving the problems of long reaction period and large using quantity of corrosive raw material of the existing method for synthesizing the PBO polymer. The preparation method comprises the following steps: 1) preparing a polyphosphoric acid solution; 2) adding an AB type PBO monomer into the polyphosphoric acid solution, and continuously supplementing P2O5 in the heating process to obtain an initial reaction solution; 3) performing gradient heating on the initial reaction solution obtained in the step 2) to prepare a polymer solution; 4) placing the polymer solution in deionized water to soak, and then performing vacuum drying to obtain the PBO polymer. According to the method disclosed by the invention, the PBO polymer with high molecular weight is generated in a polyphosphoric acid system after short-time polymerization, the using quantity of the corrosive raw material P2O5 is reduced, and the total consumed time in the polymerization stage can be shortened to 5-12 hours.

Description

technical field [0001] The invention relates to a preparation method of PBO polymer. Background technique [0002] Around the preparation of PBO polymers, a lot of research work at home and abroad is going on, which mainly includes the research on the synthesis process of PBO monomer, the research on PBO polymerization method, the research on PBO polymerization method and technology. Different PBO monomers mean significant differences in the PBO polymer preparation process. [0003] PBO polymers are generally prepared by polycondensation reaction of 4,6-diaminoresorcinol with terephthalic acid (TPA) or terephthaloyl chloride in a polyphosphoric acid (PPA) medium. There are also researchers who use 4,6-diaminoresorcinol hydrochloride and terephthalic acid to generate a complex salt in aqueous solution, and then dry to obtain a complex salt product, which is then polymerized in polyphosphoric acid. In addition, 4,6-diaminoresorcinol and trimethylsilane can also be used as ra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/22
Inventor 黄玉东李祥龙孟令辉
Owner HARBIN INST OF TECH
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