Preparation method of high-performance thermotropic liquid crystal polyarylester

A thermotropic liquid crystal and polyarylate technology, applied in liquid crystal materials, chemical instruments and methods, etc., can solve the problems of reduced impact strength, low dielectric constant and dielectric loss, and poor adhesion of polymer materials. , to achieve the effect of improving impact strength, reducing dielectric loss, excellent mechanical properties and processing properties

Inactive Publication Date: 2020-12-25
宁波聚嘉新材料科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

PTFE has a lower dielectric constant and dielectric loss in all resins. At f=10GHz, its dielectric constant is 2.1 and dielectric loss is 0.004. Adding PTFE to LCP can reduce the dielectric constant and dielectric loss of polymer materials. Dielectric loss, but due to the poor wettability of PTFE materials, it cannot be bonded well, which reduces the impact strength of polymer materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0026] Add 100g of amine aqueous solution to a 250ml three-neck flask, cool to 0°C, then add 12g of 4-chloropyridine, heat up and reflux for 1 hour, after cooling, add 40g of toluene, extract twice, combine the extracts, add 8g of anhydrous magnesium sulfate Dry for 24 hours, filter, and rotary evaporate to obtain a crude product, which is added to 40 g of xylene and recrystallized to obtain 7 g of near-colorless flaky crystals of 4-aminopyridine, which are set aside.

[0027] Add 50g of dimethyl 1,4-cyclohexanedione-2,5-dicarboxylate into a 1L four-neck flask, stir, add 0.2L glacial acetic acid and gradually raise the temperature, until 85°C, 1,4-cyclohexane The dimethyl diketone-2,5-dicarboxylate is completely dissolved, and a small amount of iodine and potassium iodide are added when the temperature rises to 100°C. Slowly add 0.012L of 30% H 2 o 2 , add 0.1 L of cold water after 30 min of heat preservation, cool down to room temperature, centrifuge, and wash with distille...

Embodiment 1

[0028] Embodiment 1: The preparation method of the thermotropic liquid crystal polyarylate of this embodiment is realized according to the following steps

[0029] 1. Add 29.7g 2,5-dihydroxyterephthalic acid, 69g p-hydroxybenzoic acid, 94g 2-hydroxy-6-naphthoic acid, 398g acetic anhydride, 6.2g 4-aminopyridine and 0.5g tin chloride to titanium In the alloy polymerization kettle, keep it at 160°C for 6h, then raise the temperature to 335°C at a rate of 0.5°C / min, keep it warm for 3h, fill the titanium alloy polymerization kettle with 0.3MPa nitrogen, and release it through the 10-hole discharge valve with a diameter of 3mm. , crushed, passed through a 20-mesh sieve, and dried at 170°C for 2.5 hours to obtain a prepolymer;

[0030] 2. Place the prepolymer obtained in step 1 in a nitrogen flow of 0.3m 3 Under the protection condition of / h, the solid phase polycondensation reaction was carried out in the rotary kiln at 235°C for 55 hours to obtain high molecular weight polymer p...

Embodiment 2

[0034] Embodiment 2: The preparation method of the thermotropic liquid crystal polyarylate of this embodiment is realized according to the following steps

[0035] 1. Add 29.7g 2,5-dihydroxyterephthalic acid, 69g p-hydroxybenzoic acid, 94g 2-hydroxy-6-naphthoic acid, 398g acetic anhydride, 6.2g 4-aminopyridine and 0.5g tin chloride to titanium In the alloy polymerization kettle, keep it at 160°C for 6h, then raise the temperature to 335°C at a rate of 0.5°C / min, keep it warm for 3h, fill the titanium alloy polymerization kettle with 0.3MPa nitrogen, and release it through the 10-hole discharge valve with a diameter of 3mm. , crushed, passed through a 20-mesh sieve, and dried at 170°C for 2.5 hours to obtain a prepolymer;

[0036] 2. Place the prepolymer obtained in step 1 in a nitrogen flow of 0.3m 3 Under the protection condition of / h, the solid phase polycondensation reaction was carried out in the rotary kiln at 235°C for 55 hours to obtain high molecular weight polymer p...

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Abstract

The invention discloses a preparation method of high-performance thermotropic liquid crystal polyarylester, and relates to a preparation method of thermotropic liquid crystal polyarylester with low dielectric constant and high impact strength, which comprises the following steps of: 1, reacting 2, 5-dihydroxy terephthalic acid with p-hydroxybenzoic acid, 2-hydroxy 6-naphthoic acid, p-hydroxybenzoic acid, p-hydroxybenzoic acid and p-hydroxybenzoic acid; adding acetic anhydride, 4-aminopyridine and an antioxidant into a polymerization kettle, and carrying out melt polycondensation to prepare a prepolymer of the thermotropic liquid crystal polyarylester; 2, performing solid-phase polycondensation reaction on the prepolymer in a rotary kiln under the protection of nitrogen to obtain high-molecular-weight polymer powder; 3, mixing the high-molecular-weight polymer powder with polytetrafluoroethylene resin, cooling and drawing to prepare primary polyarylester; and 4, carrying out heat treatment on the primary polyarylester. The dielectric constant of the thermotropic liquid crystal polyarylester is less than 3.0, the dielectric loss is less than 0.003, the impact strength can reach 35-50kJ/m < 2 >, and the thermotropic liquid crystal polyarylester has high dimensional safety and excellent mechanical properties and processability.

Description

technical field [0001] The invention relates to a preparation method of high-performance thermotropic liquid crystal polyarylate Background technique [0002] With the advent of the 5G era, optoelectronics and mobile communications have put forward higher requirements for high-frequency and high-speed transmission. In signal transmission, the transmission rate of the signal is related to the dielectric constant of the substrate (ε r )related. When the dielectric constant of the substrate is in a stable state at high frequencies, it will be conducive to the rapid transmission of signals and reduce delay; at the same time, the smaller the dielectric loss of the substrate, the faster the signal transmission speed inside the substrate. Therefore, the dielectric constant and dielectric loss are the most important parameters to measure the dielectric properties of the substrate. Secondly, other properties of the substrate, such as moisture resistance, heat resistance, and chemic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L67/04C08L27/18C08G63/685C09K19/38
CPCC08G63/6852C08L67/04C09K19/3809C09K19/3838C08L27/18
Inventor 王阳张彦
Owner 宁波聚嘉新材料科技有限公司
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