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Semi-continuous preparation method of poly-p-phenylene benzobisoxazazole polymer

A technology of benzobisoxazole and polyparaphenylene, applied in the direction of single-component synthetic polymer rayon, fiber chemical characteristics, textiles and papermaking, etc., can solve the problem of inability to obtain high molecular weight polymers and batch-to-batch polymerization Large differences in material properties, difficult material transportation and transfer, etc., to achieve the effect of increasing surface renewal ability, ensuring performance and quality, and shortening the reaction time

Active Publication Date: 2013-02-20
CHINA BLUESTAR CHENGRAND CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 1. The existing kettle-type polymerization takes a long time and the utilization rate of the equipment is low;
[0007] 2. In the existing kettle-type polymerization, due to the high viscosity of the polymerization system, it is difficult to stir, and it is difficult to continue to increase the molecular weight of the polymer after reaching a certain level, and it is impossible to obtain high-molecular-weight polymers;
[0008] 3. In the existing kettle-type polymerization, due to the high viscosity of the polymerization system, it is difficult to transport and transfer materials after the polymerization is completed;
[0009] 4. The existing kettle-type polymerization, because it is a batch-type polymerization, the properties of the polymers vary greatly between batches, resulting in discontinuous spinning and unstable fiber performance

Method used

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  • Semi-continuous preparation method of poly-p-phenylene benzobisoxazazole polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A semi-continuous preparation method of poly-p-phenylene benzobisoxazole polymer, comprising the following processing steps:

[0028] A. Add terephthalic acid, 4,6-diaminoresorcinol hydrochloride, polyphosphoric acid and phosphorus pentoxide to the kneader with the discharge screw conveying device under the belt to remove hydrogen chloride and material Mixing, and then the mixture is transported to the mixing kettle through the lower discharge screw conveying device of the kneader;

[0029] B. Mix and defoam the mixture delivered to the mixing tank at 120° C. for 1 hour, and then deliver it to a filter for conventional filtration in the field;

[0030] C, after the mixture is filtered, it directly enters more than 2 screw extruders in series for polymerization to obtain the product of the present invention i.e. the described polyparaphenylene benzobisoxazole polymer; the polymerization temperature in the screw extruder The control is 130°C.

Embodiment 2

[0032] A semi-continuous preparation method of poly-p-phenylene benzobisoxazole polymer, comprising the following processing steps:

[0033] A. Add terephthalic acid, 4,6-diaminoresorcinol hydrochloride, polyphosphoric acid and phosphorus pentoxide to the kneader with the discharge screw conveying device under the belt to remove hydrogen chloride and material Mixing, and then the mixture is transported to the mixing kettle through the lower discharge screw conveying device of the kneader;

[0034] B. Mix and defoam the mixture delivered to the mixing tank at 180°C for 10 hours, and then deliver it to a filter for conventional filtration in this field;

[0035] C, after the mixture is filtered, it directly enters more than 2 screw extruders in series for polymerization to obtain the product of the present invention i.e. the described polyparaphenylene benzobisoxazole polymer; the polymerization temperature in the screw extruder The control is 220°C.

Embodiment 3

[0037] A semi-continuous preparation method of poly-p-phenylene benzobisoxazole polymer, comprising the following processing steps:

[0038] A. Add terephthalic acid, 4,6-diaminoresorcinol hydrochloride, polyphosphoric acid and phosphorus pentoxide to the kneader with the discharge screw conveying device under the belt to remove hydrogen chloride and material Mixing, and then the mixture is transported to the mixing kettle through the lower discharge screw conveying device of the kneader;

[0039] B. Mix and defoam the mixture delivered to the mixing tank at 150° C. for 5.5 hours, and then deliver it to a filter for conventional filtration in this field;

[0040] C, after the mixture is filtered, it directly enters more than 2 screw extruders in series for polymerization to obtain the product of the present invention i.e. the described polyparaphenylene benzobisoxazole polymer; the polymerization temperature in the screw extruder The control is 175°C.

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Abstract

The invention relates to a semi-continuous preparation method of poly-p-phenylene benzobisoxazazole polymer, belonging to the production field of high-performance fibers. The semi-continuous preparation method comprises the steps of adding raw materials into a kneading kettle, and conducting dehydrochlorination on a monomer in the kneading kettle to increase the surface updating capability of a high-viscosity system and accelerate the dehydrochlorination; then entering the materials into a mixing kettle, removing bubbles of a polymer, mixing, pumping the materials into a filter by a metering pump, directly connecting the filter with more than two screw extruders which are connected in series, filtering the materials subjected to dehydrochlorination and bubble removal, and then polymerizing. According to the preparation method, the continuity of operation is improved.

Description

technical field [0001] The invention relates to a polymer preparation method, more specifically, the invention relates to a semi-continuous preparation method of poly-p-phenylene benzobisoxazole polymer, which belongs to the field of high-performance fiber production. Background technique [0002] PBO fiber is the abbreviation of cis-polyparaphenylene benzobisoxazole (PBO) fiber. The main performance indicators of the fiber, such as the tensile strength of 5.8GPa, the modulus of 280GPa, the LOI value of 68, and the decomposition temperature of 650°C, are among the best performances of organic and inorganic fibers at present. 12 to 14 times that of steel, the specific modulus is 1.4 times that of steel, and the specific gravity is 1.54 to 1.56g / cm 3 , only 1 / 5 of steel. [0003] Due to its superior performance, PBO fiber has been regarded as a new generation of super fiber for advanced structural composite materials such as aerospace and military since its inception. PBO i...

Claims

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Application Information

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IPC IPC(8): C08G73/22D01F6/74
Inventor 范新年严家策许伟赵亮郭玲李欣欣钱军
Owner CHINA BLUESTAR CHENGRAND CO LTD
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