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Naphthalene-containing polyetherimide polymer and preparation method thereof

A naphthalene polyetherimide and polymer technology, which is applied in the field of polyetherimide preparation, can solve the problem of low heat resistance, and achieve the effects of improving cost performance, large market and development prospects, and reducing production costs.

Inactive Publication Date: 2010-01-20
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the heat resistance level of this type of polyetherimide is not high, and its glass transition temperature is concentrated at 210-290°C. In order to further improve the heat resistance level of polyetherimide without increasing its production cost, we designed A new type of six-membered ring polyetherimide containing naphthalene anhydride, this polymer has a higher glass transition temperature of 280-380°C

Method used

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  • Naphthalene-containing polyetherimide polymer and preparation method thereof
  • Naphthalene-containing polyetherimide polymer and preparation method thereof
  • Naphthalene-containing polyetherimide polymer and preparation method thereof

Examples

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Effect test

Embodiment 1

[0055] Atmospheric pressure (1.01×10 5 Pa) under, equipped with stirrer, condenser, water trap, thermometer, argon (argon gas is fed from the beginning of the experiment to the end of the experiment. The aforementioned reflux water device refers to the condenser and the separator here. Add 4.69g (0.02mol) 4-chloro-1,8-naphthalene anhydride, 2.00g (0.01mol) 4,4'-diaminodiphenyl ether, 40ml N,N -Dimethylacetamide (DMAc), 10ml of xylene, stirred at room temperature for 1 hour, then started to heat slowly, maintained at 150°C with water for 2 hours, and the system was reddish brown at this time. After the water is completely carried out, xylene is released, and then the temperature of the reaction system is raised to 160°C for 6 hours. After the reaction was completed, the solid was filtered out, then washed twice with acetone and ethanol to remove the residual solvent, and finally the obtained solid was dried in vacuum at 60°C for 5 hours to obtain 3.6 g of golden yellow solid p...

Embodiment 2

[0057] Atmospheric pressure (1.01×10 5 Pa), add 97.7g (0.4mol) 4-chloro-1,8-naphthalene anhydride, 40.0g (0.2 mol) 4,4'-diaminodiphenyl ether, 500ml N,N-dimethylacetamide (DMAc), 70ml xylene, stirred at room temperature for 1 hour, began to heat slowly, and maintained at 150°C with water for 6h, at this time The system is reddish brown. Wait for the water to be completely released, xylene is released, and the temperature is raised to 160°C for 12 hours. After the reaction was completed, the precipitated solid was filtered, then washed twice with acetone and ethanol to remove the residual solvent, and finally the obtained solid was dried in vacuum at 60°C for 15 hours to obtain 81.2 g of golden yellow solid powder, with a yield of 66.0%. (Monomer 1, name: 4,4'-bis(N-phenyl-4-chloro-1,8-naphthalimide) ether), higher than the yield of Example 1.

Embodiment 3

[0059] Atmospheric pressure (1.01×10 5 Pa), add 4.69g (0.02mol) 4-chloro-1,8-naphthalene anhydride, 1.08g (0.01 mol) p-phenylenediamine, 30ml N,N-dimethylacetamide (DMAc), 8ml xylene, stirred at room temperature for 1 hour, started to heat slowly, maintained at 150°C with water for 2 hours, and the system was reddish brown at this time. Wait for the water to be completely released, xylene is released, and the temperature is raised to 160°C for 8 hours. After the reaction was completed, the precipitated solid was filtered, then washed twice with acetone and ethanol to remove the residual solvent, and finally the obtained solid was dried in vacuum at 60° C. for 5 h to obtain 2.7 g of golden yellow solid powder (monomer 2, Name: 4,4'-bis(4-chloro-1,8-naphthalimide)benzene), yield 50.3%.

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Abstract

The invention belongs to the polyetherimide preparation technical field and particularly relates to a naphthalene-containing polyetherimide polymer prepared from a new dihalogen monomer containing naphthalene ring and a preparation method thereof. The preparation method comprises the following steps: dissolving 4-halogeno-1,8-naphthalic anhydride and diamine in DMAc, entraining water in the present of water-carrying agent, then dewatering at high temperature to obtain the dihalogen monomer containing imide structure; then adopting the monomer and sodium salt of bisphenol as reactants and tetramethylene sulfone (TMS) as solvent to perform high emperature polymerization in the present of xylene carrying water and synthesizing a new polyetherimide containing naphthalene structure. The invention synthesizes the new polyetherimide containing naphthalene structure which has higher glass-transition temperature and six-membered imide ring containing naphthalene ring structure is introduced so as to increase the hydrolysis resistance of polyetherimide material to a certain degree. The polymerization method avoids to prepare the polyetherimide of the invention through the synthesis of ether-containing dianhydride and adopts sulfolane as solvent for polymerization which can be recycled so as to lower the production cost.

Description

technical field [0001] The invention belongs to the technical field of polyetherimide preparation, and in particular relates to a naphthalene-containing polyetherimide polymer prepared by using a novel dihalogen monomer containing a naphthalene ring and a preparation method of the polymer. Background technique [0002] Since Staudinger published his famous treatise on polymerization reaction in 1932 and established modern polymer science, polymer science has developed at an astonishing speed. With a preliminary understanding, some polymer chemists began to try to design and synthesize various new polymers from the perspective of molecular design in order to obtain organic polymer materials with excellent properties, which made great progress in the field of polymer materials. As a result, various polyaddition and polycondensation polymers such as polyolefins, polyamides, and polyesters have emerged, and these polymers have been synthesized by various methods and realized ind...

Claims

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Application Information

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IPC IPC(8): C08G65/34
Inventor 党国栋李鹏陈春海周宏伟赵晓刚
Owner JILIN UNIV
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