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Polyetherimide containing anthrone and trifluoromethyl structure and preparation method thereof

A technology of polyetherimide and trifluoromethyl, which is applied in the field of polymer synthesis, can solve problems that have not caused researchers, and achieve the effects of low cost, improved light transmittance, and short process

Active Publication Date: 2018-12-14
JIANGXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As early as 1908, Bogert and Renshaw prepared and reported aromatic polyimide for the first time, but due to the limitations of people's understanding of the nature and characteristics of polymer materials at that time, this discovery did not attract the attention of researchers.

Method used

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  • Polyetherimide containing anthrone and trifluoromethyl structure and preparation method thereof
  • Polyetherimide containing anthrone and trifluoromethyl structure and preparation method thereof
  • Polyetherimide containing anthrone and trifluoromethyl structure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] (1) Synthesis of 9,9-bis(4-hydroxyphenyl)anthracene-10(9H)-one (BHPAO)

[0048]Add 19.4 g (0.1 mol) of xanthone and thionyl chloride (60 mL) into a 250 mL single-necked bottle, reflux for 2 hours, evaporate and recover the remaining thionyl chloride, continue to add 80 mL of xylene and 37 g of excess phenol ( 0.39mol), slowly heated to 130°C, reacted for 3h, stopped the reaction, cooled to room temperature, filtered, the residual solid was washed with an appropriate amount of dichloromethane to obtain a crude product, the crude product was recrystallized with acetone, and after drying, 34g of a light gray powder solid was obtained. The yield is 90%, and the melting point is 306-307°C. 1 H NMR (400MHz, DMSO-d 6 ): δ=9.44(s, 2H), 8.11(d, J=9.6Hz, 2H), 7.59(t, J=7.0Hz, 2H), 7.47(t, J=7.4Hz, 2H), 7.16(d ,J=7.9Hz,2H),6.72(d,J=8.7Hz,4H),6.65(d,J=8.7Hz,4H)( figure 1 ).

[0049] (2) Synthesis of 9,9-bis[4-(4-nitro-2-trifluoromethylphenoxy)phenyl]anthracene-10(9H)-one (BNTPP...

Embodiment 2

[0054] Preparation of polyetheramic acid PAA (taking PAA(a) as an example)

[0055] In pass have N 2 BATPPAO (1mmol, 0.696g) and DMAc (2mL) were first added to a 50mL three-necked flask, stirred in an ice-water bath until completely dissolved, then added perphthalic anhydride (PMDA) (1mmol, 0.218g), and then added DMAc, The solid content of the reaction system is controlled to be about 20%, and the reaction is performed in an ice-salt bath for 1 h, and then at room temperature for 10 h to obtain a transparent viscous polyether amic acid solution. Filter the polyether amic acid viscous liquid with 400-mesh nylon cloth to remove insoluble impurities, and spread the filtrate evenly on the treated and clean glass plate on a film laying machine with a constant temperature of 60°C, and evaporate most of it after 10 hours solvent, and then vacuum-baked at 100° C. for 12 hours to obtain a light yellow transparent polyamic acid PAA (a) film with uniform thickness.

Embodiment 3

[0057] Preparation of polyetherimide film (taking polyetherimide PI(b) as an example)

[0058] Under the protection of nitrogen flow, the polyether amic acid PAA (b) film was thermally cyclized at high temperature (using temperature programming) to become a polyimide PI (b) film. The thermal cyclization process is as follows: first, the temperature is raised from 50°C to 130°C at a rate of 10°C / min, and kept for 2 hours, then the temperature is raised to 210°C, and the rate of increase is 1°C / min, kept for 2 hours, and finally Adjust the temperature to 320°C, increase at a rate of 1°C / min, and keep for 2h.

[0059] (1) Infrared spectrum analysis of polyetherimide

[0060] Image 6 It is the infrared spectrum comparison chart of polyetheramic acid PAA (b) and polyetherimide PI (b) after thermal cyclization, as can be seen from the spectrogram, the characteristic peak of the amine group in the polyetherimide disappears, It shows that the imidization of amino group is complete...

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Abstract

The invention relates to a polyetherimide containing anthrone and trifluoromethyl structure and a preparation method thereof. The method comprises the following steps: taking fluorenone, protochloride, sulfone, phenol, and 2-chloro-5-nitrotrifluorotoluene as main raw materials, sequentially performing one-pot, two-step condensation, nucleophilic substitution and reduction reaction to obtain novelaromatic diamine monomer-9,9-bis[4-(4-amino-2-trifluoromethyl phenoxyl) phenyl]anthracene-10(9H)-ketone; performing low-temperature polycondensation with aromatic dianhydride to obtain corresponding polyether amic acid, forming a film and performing heating cyclisation to obtain polyetherimide. The polyetherimide of the present invention has a large volume of an anthrone structure, an ether bond,and a trifluoromethyl side group introduced into the molecular main chain, and has excellent heat resistance, light transmittance, film formability, and low dielectric constant, can be dissolved in some organic solvents, can be used as a novel high-performance organic polymer material, and has potential application prospects in high-tech fields such as aerospace and microelectronics.

Description

technical field [0001] The invention relates to a polyetherimide containing anthrone and a trifluoromethyl structure and a preparation method thereof. The polyetherimide containing an anthrone structure and a trifluoromethyl side group is a new type of improved The invention relates to a permanent polyimide polymer material, specifically belonging to the technical field of polymer synthesis. Background technique [0002] Aromatic polyimide is one of the organic polymer materials with excellent comprehensive properties. It has excellent electrical properties, good heat resistance, radiation resistance and outstanding mechanical properties. It is used in many fields (such as: engineering plastics, fibers, advanced Composite materials, coatings, adhesives, etc.) have been widely used, especially in high-end technical fields such as aerospace, microelectronics, etc., and are one of the indispensable high-temperature resistant materials. As early as 1908, Bogert and Renshaw prep...

Claims

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Application Information

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IPC IPC(8): C08G73/10
CPCC08G73/1007C08G73/1071
Inventor 盛寿日段海涛唐传超宋琤黄振钟
Owner JIANGXI NORMAL UNIV
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