A kind of preparation method of modified polybenzobisoxazole resin polymer

A benzobisoxazole and polymer technology, which is applied in the field of preparation of modified polybenzobisoxazole resin polymers, can solve problems such as poor operation stability, liquid return, and difficult filtration, and achieve improved fiber uniformity , improved production efficiency and simple preparation process

Active Publication Date: 2015-12-02
XUZHOU SILK FIBER TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The resulting consequence is that, from a technological point of view, the high viscosity of the spinning solution will cause difficulty in evenly distributing the spinning solution in the melt pipe, difficulty in filtering, and poor uniformity of spinning; from the perspective of equipment requirements Generally speaking, such a high viscosity requires very high pressure resistance of the entire post-polymerization and spinning system, requiring a metering pump to provide a pressure of up to 30-40 MPa, and the spinning pressure reaches 10-25 MPa
[0006] This pressure range has reached or exceeded the upper pressure limit considered in the design and manufacture of the current spinning equipment, so that in the actual production process of PBO fibers, tiny particles often cannot be completely filtered, Excessive pressure in the pipeline causes problems such as inaccurate measurement of the metering pump, liquid return and leakage, slurry leakage at the joint of the pipeline, and large diameter unevenness of the fiber, which makes the operation stability in large-scale production poor, and the equipment operation rate is low. Process repeatability is not good

Method used

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  • A kind of preparation method of modified polybenzobisoxazole resin polymer
  • A kind of preparation method of modified polybenzobisoxazole resin polymer
  • A kind of preparation method of modified polybenzobisoxazole resin polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] The 1660g of terephthalic acid in the comparative example was replaced with 1328g of terephthalic acid, 166g of phthalic acid, and 166g of isophthalic acid. The contents of other reactants and the polymerization process were the same as those of the comparative example. The spinning conditions are: spinning pressure 10 MPa, spinning temperature 170°C.

[0053] In the modified resin, the content of terephthalic acid structural unit is 0.8 (molar content, the same below), and the content of phthalic acid and isophthalic acid structural unit is both 0.1.

[0054] Its reaction formula is as follows:

[0055]

[0056] The modified polybenzoxazole fiber obtained in this embodiment has an initial thermal decomposition temperature of 589° C., a strength of 4.1 GPa, and an unevenness rate of 8.9%.

Embodiment 2

[0058] The 1660g terephthalic acid in the comparative example was replaced with 1494g terephthalic acid and 166g isophthalic acid, and the contents of other reactants and the polymerization process were the same as the comparative example. The spinning conditions are: spinning pressure 12MPa, spinning temperature 173°C.

[0059] In the modified resin, the content of the terephthalic acid structural unit is 0.9, and the content of the isophthalic acid structural unit is 0.1.

[0060] Its reaction formula is as follows:

[0061]

[0062] The modified polybenzazole fiber obtained in this embodiment has an initial thermal decomposition temperature of 594° C., a strength of 5.3 GPa, and an unevenness rate of 9.7%.

Embodiment 3

[0064] The 1660g of terephthalic acid in the comparative example was replaced with 1328g of terephthalic acid, 166g of phthalic acid, and 216g of naphthalene dicarboxylic acid, and the contents of other reactants and the polymerization process were the same as those of the comparative example. The spinning conditions are: spinning pressure 11 MPa, spinning temperature 175°C.

[0065] In the modified resin, the content of the structural unit of terephthalic acid is 0.8, and the content of the structural units of phthalic acid and naphthalene dicarboxylic acid are both 0.1.

[0066] Its reaction formula is as follows:

[0067]

[0068] The modified polybenzoxazole fiber obtained in this embodiment has an initial thermal decomposition temperature of 591° C., a strength of 4.7 GPa, and an unevenness rate of 8.5%.

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Abstract

The invention discloses a preparation method of a modified polybenzobisoxazole resin polymer. According to the preparation method, 8-12% of polyphosphoric acid (mass ratio) and 12-18% of phosphorus pentoxide (mass ratio) are added; the molar ratio of the molar sum of the added terephthalic acid and other diacid except the terephthalic acid of the residual mass ratio to 4,6-diamidoresorcinol is 1:1, wherein the molar content of terephthalic acid at least accounts for 80% of the total molar content of diacid; at least one of terephthalic acid and isophthalic acid is used for sure; the non-formic acid diacid is used or not, and the molar content does not exceed 10% of the total molar content of diacid if the non-formic acid diacid is used; and a conventional polybenzobisoxazole resin method is adopted for polymerization. The preparation method disclosed by the invention has the advantages that the strength of the fiber obtained by spinning by use of the polymer provided by the invention can exceed 3GPa, the viscosity of the spinning solution is greatly reduced, the equipment requirements in the spinning process are lowered, and the operation rate and production efficiency of the equipment in a production process are improved.

Description

technical field [0001] The invention relates to a preparation method of a polymer, in particular to a preparation method of a modified polybenzobisoxazole resin polymer. Background technique [0002] Polyphenylene benzobisoxazole (referred to as PBO) resin has excellent heat resistance and chemical stability, and the fiber obtained by dry spray wet spinning has the characteristics of high strength and high modulus, and is known as the 21st century The super fiber has a wide range of applications. [0003] The molecular structure of PBO is as follows: [0004] [0005] PBO is formed by polycondensation of 4,6-diaminoresorcinol and terephthalic acid in polyphosphoric acid solvent, and the polymerization system is directly used as spinning solution. Extensive research has been done on the spinning process of PBO. In the spinning process, since the concentration of PBO needs to reach more than 10%, the viscosity of the spinning solution is very high. The resulting consequ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/22D01F6/78
Inventor 孙德荣刘小云
Owner XUZHOU SILK FIBER TECH
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