2,3,6,7-tetracarboxylic dianhydride triptycene and method for synthesizing the same

A technology of tetracarboxylic dianhydride triptycene and tetramethyl triptycene, applied in 2 fields, can solve problems such as difficulty in synthesizing polyimide, and achieve the effects of avoiding side reactions, easy production and low price

Inactive Publication Date: 2009-07-15
HUAQIAO UNIVERSITY
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  • Abstract
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Problems solved by technology

[0007] However, there are few reports on the polyimide with triptycene triphenyl ring plane as the main chain direction due to the difficulty in the synthesis of monomers.

Method used

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  • 2,3,6,7-tetracarboxylic dianhydride triptycene and method for synthesizing the same
  • 2,3,6,7-tetracarboxylic dianhydride triptycene and method for synthesizing the same

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Embodiment Construction

[0025] The following is the best embodiment of the invention

[0026] Under the conditions of ice-salt bath and vigorous stirring, 30g (grams) of aluminum chloride was divided into three additions and added in a 500ml three-necked flask equipped with 65ml (milliliters) of o-xylene and a mechanical stirrer, and then added 15g of phthalic anhydride in three batches, During the feeding process, ensure that the system temperature is lower than -5°C. After the addition, let the system stir at room temperature for 3 hours (hours), and then react in a water bath at 55° C. for 3 hours. Afterwards, slowly disperse the viscous mixed reactant in 500ml of 5% hydrochloric acid ice-water mixed solution. During the pouring process, vigorous stirring is required so that the excess aluminum chloride can be fully hydrolyzed. of white solid. Dissolve this solid in 300ml of 5% sodium hydroxide solution, let it stand for stratification, the upper layer is a small amount of o-xylene, and the lowe...

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Abstract

The invention discloses 2,3,6,7-tetracarboxylic dianhydride triptycene and a synthetic method thereof. The synthetic method comprises the following steps: preparing 2,3-dimethyl anthracene by a series of reaction of oxylene and phthalic anhydride which are cheap and easily obtained, and further reacting with 2-amino-4,5-hemellitic acid to obtain 2,3,6,7-tetramethyl triptycene; obtaining high-purity 2,3,6,7-tetramethyl triptycene by simple and rapid separation on columns, further oxidizing by potassium permanganate to obtain 2,3,6,7-tetracarboxylic acid triptycene, then obtaining the 2,3,6,7-tetracarboxylic dianhydride triptycene by dehydration. The method has the advantages of cheap and easily-obtained raw material, simple preparation method, high product purity which is up to 98% and the like, and the obtained product dianhydride monomer is fit for preparation of polyimide materials with good heat resistance and dissolubility.

Description

technical field [0001] The present invention relates to 2,3,6,7-tetracarboxylic dianhydride triptycene and its synthesis method, more specifically to a kind of 2,3 , The preparation method of 6,7-tetracarboxylic dianhydride triptycene. Background technique [0002] As a class of important structural and functional materials, aromatic polyimides are widely used in microelectronics technology, aerospace, etc., but the contradiction between high performance and processability greatly limits its application. Nowadays, the more common method for synthesizing linear polyarimides is the polycondensation reaction between dianhydride and diamine monomers. It is of great significance to expand the application of polyimide to develop new dianhydride monomers from monomer molecular design. [0003] In recent years, triptycene-based conjugated polymers, aromatic polyesters, and polyurethanes have been continuously developed, which not only have been widely used, but also indicate the p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/08
Inventor 程琳熊兴泉许震荆彬汪家喜
Owner HUAQIAO UNIVERSITY
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