Preparation method of PBO

A section and reaction technology, applied in the new preparation field of PBO (poly-p-phenylene benzobisoxazole), can solve the problems of difficult transportation, high viscosity of the system, long time, etc., and achieve strong controllability and improved The effect of simple and convenient production scale and process operation

Active Publication Date: 2014-10-01
四川宝利丰科技有限公司
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  • Summary
  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

Although this method solves the problem of batching to a certain extent, its polycondensation reaction time is still very long. The monomer is treated in a polyphosphoric acid medium at 95°C for 32 hours, and then compressed and polymerized at 190°C for 24 hours. Still not ideal, intrinsic viscosity is only 14.5dl/g (25°C, 0.0528g/dl methanesulfonic acid solution)
[0009] The study found that the main problem of the above method is that the terephthalic acid used in the polycondensation process is not soluble in polyphosphoric acid, and the 4,6-diamino-1,3-resorcinol hydrochloride monomer needs to be dissolved in the polyphosphoric acid. Hydrogen chloride is completely removed in high-viscosi

Method used

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  • Preparation method of PBO

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Effect test

Embodiment 1

[0023] Add 6.42g (0.03mol) 4,6-diamino-1,3-resorcinol hydrochloride, 152g polyphosphoric acid, 0.1g stannous chloride dihydrate to a volume of 500ml under nitrogen atmosphere In the batching degassing tank with stirring paddle, temperature control and vacuum system, maintain the system temperature at 120°C to fully stir and degas, then add 4.99g (0.03mol) terephthalic acid and 40g phosphorus pentoxide to the system , so that the raw materials are fully dispersed and mixed evenly. Then turn on the precise metering pump under the raw material preparation degassing tank, and continuously send the prepared polymerization raw materials into the capillary-type microfluidic polymerization reaction tube with a diameter of Φ2~3mm under heating for polymerization reaction. The microfluidic polymerization reaction tubes can be arranged in a grid pattern, in a spiral coil arrangement, etc., so as to be heated by a high-temperature bath. These microfluidic polymerization reaction tube...

Embodiment 2

[0025] Add 102g (0.3mol) 4,6-diaminoresorcinol phosphate, 1520g polyphosphoric acid, 1.5g stannous chloride dihydrate to a volume of 5000ml with stirring paddle, temperature In the ingredient degassing tank of the control and vacuum system, keep the system temperature at 90°C and stir thoroughly for 2 hours, then add 49.9g (0.3mol) terephthalic acid and 40g phosphorus pentoxide to the system to fully disperse and mix the raw materials evenly. Then turn on the precise metering pump under the raw material preparation degassing tank, and continuously send the prepared polymerization raw materials into the capillary-type microfluidic polymerization reaction tube with a diameter of Φ7~8mm under heating for polymerization reaction. The microfluidic polymerization reaction tubes can be arranged in a grid pattern, in a spiral coil arrangement, etc., so as to be heated by a high-temperature bath. These microfluidic polymerization reaction tubes can be divided into four reaction tempera...

Embodiment 3

[0027] Refer to the method of preparing DAR-TA salt in Example 1 in Patent No. 201310735715.7: Dissolve 3.20g of 4,6-diaminoresorcinol hydrochloride (0.015mol) in deionized aqueous solution containing 0.01g of stannous chloride 2.50g of terephthalic acid (0.015mol) was dissolved in 300ml of NaOH solution, and gradually added dropwise to the aforementioned aqueous solution of 4,6-diaminoresorcinol hydrochloride under nitrogen protection. After the dropwise addition was completed, the temperature was raised to 90° C. for 10 minutes to react. After the white solid was precipitated, it was filtered and washed under a nitrogen atmosphere, and then dried in a vacuum oven at 60°C for 48 hours to obtain 4,6-diaminoresorcinol-terephthalate (DAR-TA complex salt), and the samples were taken out and stored under vacuum.

[0028] Add 15.22g of polyphosphoric acid, 6.35g of phosphorus pentasulfide, and 0.02g of tin powder into the reaction kettle. After mixing and stirring, replace the air...

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Abstract

A preparation method of PBO which comprises the following steps: dispersing and mixing the following raw materials: 4,6-diamino-1,3-resorcinol hydrochlorate or phosphate, terephthalic acid, polyphosphoric acid and phosphorus pentoxide at the temperature of 60 to 150 DEG C; degassing under a vacuum circumstance; carrying out polymerization reaction of the mixture in a capillary microfluid reaction space of which the pipe diameter is 1 to 10 mm by passing the mixture through at least three reaction zones in a warmer and warmer manner, wherein the temperature range of 100 to 200 DEG C, the temperature difference of adjacent reaction zones is equal to or higher than 40 DEG C, and the intrinsic viscosity of the obtained PBO end product is 20 to 30 dl/g. Through high efficiency and uniform heat transmission and mass transfer, the temperature in the polymerization reaction system is uniform, the controllability is higher, and polymerization reaction can be carried out and fulfilled efficiently; under the premise of the same polymer molecular weight, the polymerization reaction time can be shortened to several hours, or even dozens of minutes; both the production efficiency and heat efficiency are greatly improved.

Description

technical field [0001] The present invention relates to a new preparation method of PBO (poly-p-phenylene benzobisoxazole). Background technique [0002] PBO fiber is currently the material with the highest tensile strength and tensile modulus among organic synthetic fibers, and it is also the synthetic material with the best heat resistance and stability. Its thermal decomposition temperature is as high as 600°C. It has great application prospects in aerospace, military industry, cable, fire protection, industrial composite materials and industrial fields. The structure of PBO is shown in formula (I), in which the number average degree of polymerization of n is generally 40-80, and 50-65 is more preferable. [0003] [0004] The synthesis of PBO fiber mainly uses monomers such as diaminoresorcinol hydrochloride or phosphate, terephthalic acid or terephthaloyl chloride to carry out high-temperature polycondensation in polyphosphoric acid medium to obtain spinning solut...

Claims

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Application Information

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IPC IPC(8): C08G73/22
Inventor 李晶晶罗芩杨琴纪宏伟
Owner 四川宝利丰科技有限公司
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