Method for preparing poly(p-phenylene) benzo dioxazole composite fiber containing carbon nano tube

A technology of phenylene benzene and composite fibers, which is applied in the direction of fiber chemical characteristics, single-component synthetic polymer rayon, wet spinning, etc., and can solve problems such as molecular weight growth, low interfacial bonding force, and limited polymer reinforcement effect

Inactive Publication Date: 2009-04-15
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the in-situ polymerization method, since CNTs participate in the polymerization reaction, there is a chemical bond between the CNTs and the polymer, which can greatly improve the interfacial interaction between the CNTs and the polymer, thereby facilitating the transfer of stress between the polymer and the CNTs, and more Good effects such as the enhancement of CNTs are achieved, but this method also has some disadvantages, such as the addition of CNTs will prevent the growth of the molecular weight of the polymer itself, especially for stepwise polymerization, as described in the patent CN 1226326C; and the physical blending method It is usually relatively simple and convenient, especially suitable for large-scale production in industry, but whether the CNTs in the prepared composite material can be well dispersed in the polymer matrix, and the low interfacial bonding force with the polymer, so it is of great concern Polymer reinforcement is very limited
[0007] There is no report on the method of preparing poly-p-phenylene benzobisoxazole composite fibers containing carbon nanotubes in the prior art

Method used

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  • Method for preparing poly(p-phenylene) benzo dioxazole composite fiber containing carbon nano tube
  • Method for preparing poly(p-phenylene) benzo dioxazole composite fiber containing carbon nano tube

Examples

Experimental program
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Embodiment 1

[0029] The carbon nanotube raw material was put into 65% concentrated nitric acid solution, ultrasonicated at room temperature for 30 minutes, heated to reflux for 24 hours, diluted with deionized water, and vacuum-filtered with a polycarbonate filter membrane. The filtered solid was continuously washed with deionized water until the pH value of the filtrate was 7. Then the obtained black solid was vacuum-dried at 40° C. for 24 h to obtain the treated MWNTs.

[0030] The prepolymer A solution, 10wt% TPA / PPA suspension and 2.5wt% MWNTs / PA suspension are pumped into a twin-screw extruder with an aspect ratio of 40 and an inner diameter of 20mm with a metering pump, and the flow rate of the metering pump is controlled. The rotation speed is such that the delivery rate of the prepolymer is 60 g / min, while the delivery rate of the TPA / PPA suspension is 1.8 g / min, and the delivery rate of the MWNTs / PA suspension is 17.6 g / min. The shear force in the extruder is 500S -1 , the tempe...

Embodiment 2

[0032]Distribute the prepolymer A solution, 15wt% TPA / PPA suspension and 3wt% MWNTs / PA suspension with a metering pump into a twin-screw extruder with an aspect ratio of 40 and an inner diameter of 20mm, and control the speed of the metering pump , the delivery rate of the prepolymer is 60g / min, while the delivery rate of the TPA / PPA suspension is 1.2g / min, and the delivery rate of the MWNTs / PA suspension is 30g / min. The shear force in the extruder is 500S -1 , the temperature is between 190 and 210°C, and the residence time is about 30 minutes. After passing through the metering pump, the material was spun by dry jet-wet spinning to obtain fibers with an average diameter of 28 μm, a tensile strength of 3.7 GPa, and a tensile modulus of 101 GPa.

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Abstract

The invention relates to a preparation method of PBO composite fibers containing carbon nano tubes, which comprises the steps of carrying out acid oxidation treatment to the carbon nano tubes, preparing PBO prepolymer solution, adding a carbon nano tube solution after the acid oxidation treatment, a TPA suspension and the PBO prepolymer solution into a double screw extruder for carrying out high-efficient blending reaction so as to be extruded, preparing the PBO composite fibers containing the carbon nano tubes by dry-jet wet spinning and the like. Compared with the PBO composite fibers synthesized under the same conditions, the PBO composite fibers prepared by the method of the invention have the tensile strength improved by 10 to 90 percent and the modulus improved by 10 to 50 percent. The PBO composite fibers containing carbon nano tubes and prepared by the method can be taken as a reinforcing agent of thermosetting resin, rubber, plastics and the like, and can be applied in protective clothing, flame resistant materials, or friction material and the like.

Description

technical field [0001] The invention relates to a preparation method of poly-p-phenylene benzobisoxazole composite fiber containing carbon nanotubes. Background technique [0002] Poly-p-phenylene benzobisoxazole (PBO) fiber is a new type of lyotropic liquid crystal aromatic heterocyclic polymer fiber. Its structure is shown in formula 1. It is made by silk technology, so it has high mechanical properties, and its thermal stability is closer to the theoretical limit of organic polymer crystals. Therefore, it has become a new type of high-performance fiber material and is called the super high-performance fiber of the 21st century. [0003] [0004] The chemical structural formula of formula 1 poly-p-phenylene benzobisoxazole (PBO) [0005] Carbon nanotubes (CNTs) are quasi-one-dimensional materials with special structures, which have excellent mechanical and electrical properties and good thermal stability. , and compound or hybridize it with polymer materials to obtai...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/74D01F1/10C08K9/02D01D5/06
Inventor 韩哲文周承俊庄启昕李欣欣胡兵陈晓军田雪
Owner EAST CHINA UNIV OF SCI & TECH
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