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Solid state polymerization preparation method of liquid crystal copolyester

A solid-state polymerization and copolyester technology, applied in liquid crystal materials, chemical instruments and methods, etc., to achieve the effects of easy control of reaction conditions, improved quality, and reduced equipment requirements

Active Publication Date: 2005-03-23
SHANGHAI PRET COMPOSITES +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The application of solid state polymerization method in liquid crystal copolyester has not been reported yet

Method used

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  • Solid state polymerization preparation method of liquid crystal copolyester
  • Solid state polymerization preparation method of liquid crystal copolyester
  • Solid state polymerization preparation method of liquid crystal copolyester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033]This example illustrates the method for solid-state polymerization of poly(p-hydroxybenzoic acid\2,6-naphthalene dicarboxylic acid\terephthalic acid\hydroquinone) liquid crystal copolyester prepolymer according to the present invention. The molar ratio of p-hydroxybenzoic acid (HBA), 2,6-naphthalene dicarboxylic acid (NDA), hydroquinone (HQ) and terephthalic acid (TA) in the prepolymer is 50 / 25 / 15 / 10 , the I.V. of the prepolymer is 1.5dL / g, the melting point is 312.4°C, and the particle diameter is 1.1mm. After vacuum-drying the prepolymer at 110°C for 4 hours, take 10 g and place it in a tubular solid-state polymerization device, blow in nitrogen, raise the temperature to 300°C at a rate of 3°C / min, and then start the solid-state polymerization of the prepolymer. After reaching the set polymerization time, the solid-state polymerization device was cooled to room temperature in air under the condition of blowing nitrogen. In this embodiment, the flow rate of nitrogen ga...

Embodiment 2

[0037] The experimental method is the same as in Example 1, but the solid state polymerization reaction temperature of this example is 280°C. Table 2 lists the melting points of polymer products after solid-state polymerization at different times under this temperature condition. The prepolymer and the products of solid state polymerization reaction for 8 hours and 24 hours were subjected to nanoindentation test, and the test results are shown in Table 3 and attached figure 1 , 2 .

[0038] Polymerization time (h)

[0039]

[0040] This embodiment shows that the solid-state polymerization method of the present invention can significantly improve the molecular weight of poly(p-hydroxybenzoic acid\2,6-naphthalene dicarboxylic acid\terephthalic acid\hydroquinone) liquid crystal copolyester, and its mechanical properties Properties (hardness and modulus) are also greatly improved.

Embodiment 3、4

[0042] Experimental method is the same as embodiment 1. The change of the melting point of the polymerization product was investigated at 240℃ and 260℃ for solid-state polymerization. Together with Examples 1 and 2, under four different solid-state polymerization temperatures, the change of polymer melting point with solid-state polymerization time is shown in the appended image 3 middle. Depend on image 3 It can be seen that the melting point of the reaction at 240°C has not changed. With the increase of the solid-state polymerization temperature, the reaction rate increases, and the time required to reach the expected melting point product is shortened, so the melting point of the product rises rapidly. It can be seen that the temperature range for the solid-state polymerization of the prepolymer is 260-300°C, and 280-300°C is more suitable.

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Abstract

A process for preparing liquid crystal copolyester by solid polymerization includes such steps as heating the prepolymer poly(parahydroxy benzoic acid / 2,6-naphthalenediformic acid / terephthalic acid / hydroquinone) to a temp which is 10-60 deg.c lower than its fusion point, and solid polimerizing reaction under existance of inertial gas.

Description

technical field [0001] The invention belongs to the technical field of liquid crystal polymer materials, and specifically relates to a solid-state polymerization method of thermotropic liquid crystal copolyester poly(p-hydroxybenzoic acid\2,6-naphthalene dicarboxylic acid\terephthalic acid\hydroquinone) . technical background [0002] Thermotropic liquid crystal copolyester (TLCP) is a high-performance polymer material with excellent comprehensive properties: excellent fluidity, high dimensional precision of parts, good dimensional stability, low linear expansion coefficient, and High rigidity, high strength, high toughness, ceramic-like chemical resistance, excellent air tightness, high heat distortion temperature, low moisture absorption, inherent flame retardancy, excellent thermal stability, excellent radiation resistance, Vibration absorbing properties. These excellent comprehensive properties make it an indispensable and irreplaceable material in many high-tech field...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/185C08G63/191C08G63/80C09K19/38
Inventor 潘欣蔚池振国程丹金曼娜卜海山
Owner SHANGHAI PRET COMPOSITES
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