Preparation method of poly(p-phenylene benzobisoxazole) fibers

A technology of benzobisoxazole and poly-p-phenylene, which is applied in the field of preparation of poly-p-phenylene benzobisoxazole fibers, can solve the problems of non-uniform reaction, easy agglomeration, poor dispersion effect, etc., and achieves favorable degassing. , The effect of reducing viscosity and improving degassing efficiency

Active Publication Date: 2021-05-07
SHANDONG NON METALLIC MATERIAL RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method solves the shortcomings of poor mixing and dispersion effect of traditional solid raw materials and solvents, easy agglomeration, and non-uniform reaction, and ensures the consistency of the end point of the prepolymerization reaction, reducing process errors

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036]A preparation method of poly-p-phenylene benzobisoxazole fiber, comprising the steps of:

[0037] (1) Mixing and degassing: Replace the air in the mixing tank with nitrogen, mix 240g of 4,6-diaminoresorcinol hydrochloride, 187g of terephthalic acid with a particle size of 13μm, and 977.1g of frozen polyphosphoric acid powder , 322.3g of phosphorus pentoxide and 7.8g of stannous chloride were stirred and mixed and put into the reactor. The temperature of the reactor was raised to 93°C, and vacuum was started for degassing. The vacuum degree was -0.06MPa, and the degassing time was 6h.

[0038] (2) Pre-polymerization: feed nitrogen to the reactor to make the negative pressure into a positive pressure of 0.01MPa to continue the pre-polymerization, heat up the material obtained in step (1) degassing to 100°C and drop 60.4g of phosphorus pentoxide and keep it warm for 3h. Then keep the temperature at 120°C for 3.5 hours, raise the temperature to 135°C, add 20.1g of phosphorus...

Embodiment 2

[0043] A preparation method of poly-p-phenylene benzobisoxazole fiber, comprising the steps of:

[0044] (1) Mixing and degassing: Replace the air in the mixing tank with nitrogen, mix 325.6g of 4,6-diaminoresorcinol hydrochloride, 253.8g of terephthalic acid with a particle size of 8μm, and 1325.6g of frozen polymer Phosphoric acid powder, 409.9g of phosphorus pentoxide and 15.8g of stannous chloride were stirred and mixed and put into the reactor. The temperature of the reactor was raised to 88°C, and vacuum was started for degassing. The vacuum degree was -0.08MPa, and the degassing time was 7.2h. .

[0045] (2) Pre-polymerization: feed nitrogen to the reaction kettle to make the negative pressure into a positive pressure of 0.01MPa to continue the pre-polymerization, heat up the material obtained in step (1) degassing to 100°C and drop 92.9g of phosphorus pentoxide and keep it warm for 3h. Then keep it at 120°C for 4 hours, raise the temperature to 135°C, put in 43.7g of ...

Embodiment 3

[0050] A preparation method of poly-p-phenylene benzobisoxazole fiber, comprising the steps of:

[0051] (1) Mixing and degassing: replace the air in the mixing tank with nitrogen, and 434g of 4,6-diaminoresorcinol hydrochloride, 338g of terephthalic acid with a particle size of 8 μm, 1767g of frozen polyphosphoric acid powder, 509.5g of phosphorus pentoxide and 17.7g of stannous chloride were stirred and mixed and put into the reactor. The temperature of the reactor was raised to 82°C, and vacuum was started for degassing. The vacuum degree was -0.093MPa, and the degassing time was 9.8h.

[0052] (2) Pre-polymerization: feed nitrogen to the reactor to make the negative pressure into a positive pressure of 0.01MPa to continue the pre-polymerization, heat up the material obtained in step (1) degassing to 100°C and drop in 145.7g of phosphorus pentoxide and keep it warm for 4h. Then keep the temperature at 120°C for 4 hours, raise the temperature to 135°C, add 72.9g of phosphoru...

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Abstract

The invention belongs to the field of high-performance fibers, and particularly relates to a preparation method of poly(p-phenylene benzobisoxazole) fibers. The preparation method comprises the following steps of taking frozen polyphosphoric acid powder, phosphorus pentoxide, 4,6-diaminoresorcinol hydrochloride and terephthalic acid as raw materials, putting the phosphorus pentoxide into a reaction system step by step in a reasonable proportion in a proper time period, and detecting and regulating the apparent viscosity of the materials in real time in a prepolymerization process to ensure that a prepolymer with uniform apparent viscosity is obtained; performing post-polymerization to obtain PBO spinning slurry; and performing dry-jet wet spinning and post-spinning to obtain the finished PBO fibers. The method overcomes the defects that traditional solid raw materials are poor in solvent mixing and dispersing effect, easy to agglomerate and incapable of uniformly reacting, ensures the consistency of a prepolymerization reaction end point, and reduces the process errors. The intrinsic viscosity of the polymer in the same batch in different time periods is small in change and high, the mechanical property of the fibers can be obviously improved, and the quality stability is also improved.

Description

technical field [0001] The invention belongs to the field of high-performance fibers, and in particular relates to a preparation method of poly-p-phenylenebenzobisoxazole fibers. Background technique [0002] Poly-p-phenylenebenzobisoxazole (PBO) (cis and trans conformations) both the benzene ring and the oxazole ring are almost coplanar with the chain axis, and it is a left-right symmetrical rigid rod-like molecular structure. This structure is the lowest energy a form of Due to the use of liquid crystal spinning technology, the macromolecular chains, crystals and microfibrils / fibrils are almost completely oriented along the fiber axis, forming a highly oriented ordered structure. Therefore, the unique structure of PBO fiber determines its excellent and outstanding performance. It has the characteristics of high strength, high modulus, high heat resistance and good flame retardancy. It has good dimensional stability and high chemical resistance. It is the most comprehensiv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/74C08G73/22
CPCD01F6/74C08G73/22
Inventor 陈湘栋刘群刘薇钟蔚华郭程刘宗法张晓光张殿波孟昭瑞
Owner SHANDONG NON METALLIC MATERIAL RES INST
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