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A kind of preparation method of graphene and liquid crystal polyester synergistically reinforced polymer fiber

A technology of liquid crystal polyester and graphene, applied in the direction of conjugated synthetic polymer rayon, fiber processing, fiber chemical characteristics, etc., can solve the problems of poor spinnability, complicated preparation process, high product price, etc. The effect of improving tensile strength at break, crystallinity and crystal regularity

Active Publication Date: 2022-06-21
TIANJIN POLYTECHNIC UNIV
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0005] Liquid crystal polyester (LCP) is a kind of polymer material containing conjugated aromatic ring structure. The tensile breaking strength of its fiber can reach more than 20cN / dtex, but its raw material is not easy to obtain, the preparation process is complicated, and the temperature window of spinning is relatively narrow. Narrow, poor spinnability, after the fiber is formed, it needs to be heat treated at a higher temperature and in an inert gas for tens of hours, such as the heat treatment time reported in "Synthetic Fiber Industry (2017, 41(9): 29)" is 20~ 60h, which ends up making the product expensive

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  • A kind of preparation method of graphene and liquid crystal polyester synergistically reinforced polymer fiber
  • A kind of preparation method of graphene and liquid crystal polyester synergistically reinforced polymer fiber
  • A kind of preparation method of graphene and liquid crystal polyester synergistically reinforced polymer fiber

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preparation example Construction

[0023] The invention provides a preparation method (method for short) of a synergistic reinforced polymer fiber of graphene and liquid crystal polyester, which is characterized in that the method comprises the following steps:

[0024] (1) The graphene and liquid crystal polyester pellets are mixed uniformly in a high-speed mixer as component A; the polymer is used as component B; wherein the mass ratio of graphene to liquid crystal polyester is 0.05~2:98.0~99.95;

[0025] Preferably, the mixed material of graphene and liquid crystal polyester is melt-extruded and granulated in an extruder, and dried as component A;

[0026] The graphene refers to graphene whose radial dimension is submicron or nanometer (0.1-0.9 μm), single-layer or few-layer (1-3 layers), and whose moisture content is lower than 120 ppm, including reduced graphene oxide and graphite oxide. graphene (GO) or functionalized graphene; the use of submicron or nanometer radial size graphene is beneficial to achiev...

Embodiment 1

[0039] Poly(2-hydroxy-6-naphthoic acid-p-hydroxybenzoic acid) copolymer (2-hydroxy- The molar ratio of 6-naphthoic acid and p-hydroxybenzoic acid was 73:27) and 98 parts by mass were mixed uniformly as component A.

[0040] Take 10 parts by mass of component A, and add 90 parts by mass of PET (component B) with an intrinsic viscosity of 1.2 to a single-screw extruder with a diameter of 25 mm. , 300 ℃, pump seat temperature 300 ℃, spinneret diameter 0.25mm.

[0041] After the thread was cooled in an air tunnel at 60°C, 65% relative humidity, and 0.4m / s wind speed, the speed of the first godet roll was 1500m / min, the first draft roll was 150°C, the second draft roll was 160°C, The drafting roller is 230°C, and the draft is 4.0 times. After setting by a 160°C hot roller, the composite fiber is wound at a speed of 5950 m / min.

[0042] The tensile breaking strength of the composite fiber was measured to be 10.2 cN / dtex, which was significantly higher than that of the PET industri...

Embodiment 2

[0045] 0.05 parts by mass of 1-3 layers of graphene with an average radial size of 0.1 microns, an intrinsic viscosity of 2.0 dL / g bisphenol A and isophthalic acid / terephthalic acid random copolymer (bisphenol A and m-terephthalic acid) The molar ratio of phthalic acid / terephthalic acid was 50:50) and 99.5 parts by mass was mixed uniformly as the A component.

[0046] Take 20 parts by mass of component A, and add it together with 80 parts by mass of PA66 with a relative viscosity of 3.1 into a single screw extruder with a diameter of 25 mm for melt extrusion and spinning. Other process and process parameters are the same as in Example 1.

[0047] The tensile breaking strength of the composite fiber was measured to be 9.5cN / dtex, which was significantly higher than that of the PA66 industrial yarn, and the crystallinity of the fiber reached 61%.

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Abstract

The invention discloses a method for preparing graphene and liquid crystal polyester synergistically reinforced polymer fibers. The method uses graphene and liquid crystal polyester with a radial dimension of submicron or nanometer as reinforcements, and adjusts graphene / liquid crystal The ratio of polyester to play a synergistic reinforcing effect, and then use conventional melt spinning or melt composite spinning to prepare molten filaments with common industrial yarn raw materials, and then obtain primary fibers after air cooling, and then post-drawing treatment Or without post-drawing treatment, high-strength composite fibers can be obtained after heat setting. The polymer matrix obtained by this method is loaded with two reinforcements of graphene and liquid crystal polyester. The two reinforcements are well dispersed in the polymer matrix and form regular crystals on the surface by inducing the polymer molecular chain. structure, improve the crystallinity of the fiber, and transfer its high physical and mechanical properties into the polymer matrix, and obtain a polymer composite fiber with lower product price and high strength.

Description

technical field [0001] The invention relates to the field of high-performance fiber preparation, in particular to a preparation method of a synergistically reinforced polymer fiber of graphene and liquid crystal polyester. Background technique [0002] Polyhexamethylene adipamide (PA66), polycaprolactam (PA6), polyethylene terephthalate (PET) and polyethylene naphthalate (PEN) are commonly used raw materials for the preparation of industrial yarn. The product is further solid-phase viscosified or liquid-phase viscosified to obtain high-molecular-weight polymers, and indirect or direct melt spinning can prepare high-strength industrial yarns, which are used in the fields of tire cords, ropes, cable jackets, conveyor belts, etc. Has a wide range of applications. "Tire Industry (2007, 27(10): 618)" discloses the preparation method of PA66 industrial yarn. The thermal stability of the resin is improved by solid phase tackifying and adding heat stabilizer, and the tensile breaki...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F8/14D01F8/12D01F1/10D01D5/08D01D5/088
CPCD01F8/14D01F8/12D01F1/10D01D5/08D01D5/088
Inventor 张兴祥于文广高雪峰张先叶刘海辉
Owner TIANJIN POLYTECHNIC UNIV
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