High-temperature-resistant, easy-to-dissolve and flame-retardant fluorinated polyaryl ether nitrile resin and preparation method thereof

A technology of polyarylether nitrile resin and polyarylether nitrile, which is applied in the field of high-temperature-resistant, soluble, flame-retardant fluorine-containing polyarylether nitrile resin and its preparation, and can solve the problem of difficult removal of high-boiling-point polar solvents and increase of PEN Dielectric loss, affecting the dielectric properties of PEN, etc., to achieve good mechanical strength, good flame retardant properties, and excellent mechanical properties

Inactive Publication Date: 2018-06-08
CHANGAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the solution casting process, most of PEN can only be dissolved in high-boiling polar solvents at present, which will lead to high temperature required in the subsequent solvent removal process, and it is difficult to remove high-boiling polar solvents, which will eventually increase The dielectric loss of PEN, which in turn affects the dielectric properties of PEN at high temperature (T>100°C) and low frequency (f<10Hz)

Method used

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  • High-temperature-resistant, easy-to-dissolve and flame-retardant fluorinated polyaryl ether nitrile resin and preparation method thereof
  • High-temperature-resistant, easy-to-dissolve and flame-retardant fluorinated polyaryl ether nitrile resin and preparation method thereof
  • High-temperature-resistant, easy-to-dissolve and flame-retardant fluorinated polyaryl ether nitrile resin and preparation method thereof

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preparation example Construction

[0030] The preparation method of fluorine-containing polyarylether nitrile resin of the present invention comprises the following steps:

[0031] Step 1: Take the raw materials, use bisphenol AF and 2,6 dichlorobenzonitrile as the main raw materials, and use sulfolane, toluene and potassium carbonate as auxiliary raw materials; wherein sulfolane is the solvent, toluene is the dehydrating agent, and potassium carbonate is the condensation polymerization reaction The catalyst, the molar ratio between the amount of each raw material is: bisphenol AF: 2,6 dichlorobenzonitrile: sulfolane: toluene: potassium carbonate=1:1:(5~11):(1.5~2):(1.1 ~1.6).

[0032] Step 2: Synthesize fluorine-containing polyarylether nitrile by aromatic nucleophilic substitution reaction under normal pressure.

[0033] 201. First, add the monomers of the above raw materials and anhydrous potassium carbonate into a 100mL three-neck flask, equipped with a mechanical stirrer, add sulfolane (TMS) and toluene, ...

Embodiment 1

[0050] Prepare materials with the molar ratio of bisphenol AF:2,6 dichlorobenzonitrile:sulfolane:toluene:potassium carbonate=1:1:11:2:1.1.

[0051] Put various raw materials in a three-necked flask equipped with a water separator, a condenser, and a stirrer, slowly introduce nitrogen gas, keep azeotropic at 165°C for 2 hours, and release the water generated by the reaction through the water separator. Continue to raise the temperature to about 175°C and react for 0.3h, continue to dehydrate, then release all the toluene, raise the system temperature to 220°C, react for 4 hours, and stop the reaction when rod climbing occurs. The reaction solution in the three-necked bottle was poured into the prepared dilute hydrochloric acid (PH=5) while hot to obtain off-white fibrous product. After pulverizing and drying, wash with boiling water for 20 minutes, dissolve with acetone (10 mL of solvent per gram of product is added to dissolve it), and precipitate in deionized water again, and...

Embodiment 2

[0055] Prepare materials with the molar ratio of bisphenol AF:2,6 dichlorobenzonitrile:sulfolane:toluene:potassium carbonate=1:1:8:1.6:1.3.

[0056] Put various raw materials in a three-necked flask equipped with a water separator, a condenser, and a stirrer, slowly introduce helium gas, keep azeotroping at 160°C for 3 hours, and release the water generated by the reaction through the water separator. Continue to raise the temperature to about 185°C and react for 0.5h, continue to dehydrate, then release all the toluene, raise the temperature of the system to 230°C, react for 4.5 hours, and stop the reaction when rod climbing occurs. The reaction solution in the three-necked flask was poured into methanol while hot to obtain off-white fibrous product. After crushing and drying, wash with boiling water for 30 minutes, dissolve with tetrahydrofuran (add 12 mL of solvent per gram of product to dissolve it), and precipitate in deionized water again, and after washing and suction f...

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Abstract

The invention relates to a high-temperature-resistant, easy-to-dissolve and flame-retardant fluorinated polyaryl ether nitrile resin and a preparation method thereof. Firstly, bisphenol AF, 2,6-dichlorobenzonitrile and a catalyst are mixed to obtain a mixture, a solvent and a dehydrating agent are added to the mixture, and an aromatic nucleophilic substitution reaction is carried out in a protective atmosphere, wherein the molar ratio of bisphenol AF to 2,6-dichlorobenzonitrile to the catalyst to the solvent to the dehydrating agent is 1:1:(1.1-1.6):(5-11):(1.5-2); after the aromatic nucleophilic substitution reaction is finished, the reaction product is poured into a precipitant and is precipitated, and precipitates are dried and crushed, and after purification, the high-temperature-resistant, easy-to-dissolve and flame-retardant fluorinated polyaryl ether nitrile resin is obtained. Fluorine atoms are introduced to the product, so the solubility of polyaryl ether nitrile is improved,and the polyaryl ether nitrile can be dissolved in low-boiling-point organic solvents such as acetone, chloroform, tetrahydrofuran and the like; and because of containing of F atoms, the polyaryl ether nitrile resin has good flame retardancy, thermal stability and mechanical properties.

Description

technical field [0001] The invention belongs to the technical field of macromolecular materials, and in particular relates to a high-temperature-resistant, easily soluble, flame-retardant fluorine-containing polyarylether nitrile resin and a preparation method thereof. Background technique [0002] Since the 21st century, the rapid development of aerospace, electronic information, mechanical equipment and chemical industries has put forward higher requirements for traditional polymers, and aromatic ring polymer materials with high temperature resistance, insulation, excellent mechanical properties and processing properties have been developed. Rapid development. Compared with common special polymer materials such as polyphenylene sulfide (PPS), polyether ether ketone (PEEK) and polyarylether (PAR), polyarylether nitrile (PEN) started late, but with its excellent thermal Properties such as stability, mechanical strength, flame retardancy and radiation resistance are expected...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/40
CPCC08G65/40
Inventor 魏俊基孟晓娟白亚飞晏妮王凤燕宋家乐
Owner CHANGAN UNIV
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