A kind of dianhydride containing 1,2,2-trimethylcyclopentyl alicyclic structure and its preparation method

A technology of trimethylcyclopentyl ester and dianhydride, which is used in the preparation of polyimide film materials and the field of polyimide dianhydride monomers, can solve the difficulty of processing and molding, reduce light transmittance, insoluble, etc. problems, to achieve the effects of low manufacturing cost, simple preparation process, good transparency and heat resistance

Active Publication Date: 2011-12-14
永修县艾科普新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the rigidity of the molecular chain and the large intermolecular force, the general-purpose aromatic polyimide is difficult to dissolve and melt, and it is difficult to process and shape. In addition, the appearance of the aromatic polyimide is deep amber. When used in display devices (such as liquid crystal displays), the light transmittance will be reduced

Method used

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  • A kind of dianhydride containing 1,2,2-trimethylcyclopentyl alicyclic structure and its preparation method
  • A kind of dianhydride containing 1,2,2-trimethylcyclopentyl alicyclic structure and its preparation method
  • A kind of dianhydride containing 1,2,2-trimethylcyclopentyl alicyclic structure and its preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0023] In a 1000mL round bottom flask, add 38g natural camphor containing [2,2,1] bicyclic structure, 2g ZnSO 4 ·7H 2 O, 170mL of distilled water and 360mL of concentrated nitric acid were refluxed at a temperature of 100-110°C for 30h, the resulting solution was cooled to room temperature, and the white solid diacid was obtained by suction filtration, which was purified and dried in vacuum with a yield of 33%. In a 100mL three-neck flask, add 2.0gLiAlH 4 , 3.0g white solid diacid and 70mL anhydrous ether, after reflux at room temperature for 5h, slowly add 8.5gNa 2 SO 4 10H 2 O for quenching, add 50mL CH after quenching 2 Cl 2 Wash, filter with suction, and filter the cake with 50mL CH 2 Cl 2 After washing and suction filtration, the filtrates were combined, and the filtrate was concentrated to obtain a white solid diol, which was purified and dried, with a yield of 50%. In a 250mL three-necked flask, add 7.98g of chlorinated trimellitic anhydride, 2.58g of white soli...

Embodiment 2-4

[0025] 2g FeSO 4 ·7H 2 O-170mL distilled water-360mL concentrated nitric acid system, 2g FeSO 4 ·7H 2 O-170mL distilled water-320mL fuming nitric acid, 2g FeSO 4 ·7H 2 O-170mL distilled water-360mL concentrated sulfuric acid system instead of 2g ZnSO 4 ·7H 2 O, 170mL distilled water and 360mL concentrated nitric acid system, the productive rate is 54%, 56% and 30% respectively. All the other reaction conditions are with specific embodiment 1.

Embodiment 5-6

[0027] The mixed solution of 70mL tetrahydrofuran, 30mL anhydrous ether and 40mL tetrahydrofuran was used instead of 70mL anhydrous ether, and the yields were 57% and 85.3%, respectively. All the other reaction conditions are with specific embodiment 1.

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Abstract

The invention discloses 1,2,2-trimethyl cyclopentyl alicyclic structure-containing dianhydride, which is characterized by having a structural formula which is shown in the specification. A preparation method of the dianhydride comprises the following steps of: (1) oxidizing [2,2,1] dicyclic structure-containing natural camphor; (2) reducing solid diacid; and (3) synthesizing the 1,2,2-trimethyl cyclopentyl alicyclic structure-containing dianhydride. The 1,2,2-trimethyl cyclopentyl alicyclic structure-containing dianhydride has the advantages of simple preparation process, wide raw material source and lower manufacturing cost and fully shows the structural characteristics of the natural product camphor; and thus, a polyimide film material prepared from the dianhydride disclosed by the invention has higher transparency and heat resistance, and the corresponding problems of the conventional aromatic polyimide material are solved better.

Description

technical field [0001] The invention belongs to the field of preparation of semi-aliphatic structure polyimide materials, in particular to a preparation method of a polyimide dianhydride monomer derived from alicyclic structure of natural products and a corresponding polyimide film material. Background technique [0002] Polyimide is a polymer material known for its excellent thermal, mechanical, and electrical properties. It is generally polycondensed from dianhydride and diamine monomers into polyamic acid, and then imidized into polyimide. Due to the rigidity of the molecular chain and the large intermolecular force, the general-purpose aromatic polyimide is difficult to dissolve and melt, and it is difficult to process and shape. In addition, the appearance of the aromatic polyimide is deep amber. When used in display devices (such as liquid crystal displays), the light transmittance will be reduced. [0003] The polyimide synthesized with alicyclic dianhydride or diami...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/89C08G73/10C08J5/18
Inventor 刘峰朱帅柯田志林齐海霞
Owner 永修县艾科普新材料有限公司
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