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Soluble polyimide comprising tertiary butyl and morpholinyl structure and preparation method of soluble polyimide

A soluble polyimide and morpholine-based technology, which is applied in the field of soluble polyimide and its preparation, can solve problems such as reduction, and achieve the effects of excellent optical properties, superior heat resistance stability, and low dielectric constant

Inactive Publication Date: 2015-09-23
广西云智九沃实验仪器有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although such high temperature resistant materials have excellent thermal and mechanical properties, due to their rigid main chain structure, strong interactions between molecules and close packing of molecular chains, most commercial polyimides Amines have a high melting temperature and are insoluble in organic solvents (mostly only soluble in concentrated sulfuric acid), which brings difficulties to their molding and processing
In addition, due to the high aromatic conjugation of the molecular main chain and the charge complex transfer effect within the molecular chain, the traditional polyimide films mostly have very dark colors and poor optical transparency.

Method used

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  • Soluble polyimide comprising tertiary butyl and morpholinyl structure and preparation method of soluble polyimide
  • Soluble polyimide comprising tertiary butyl and morpholinyl structure and preparation method of soluble polyimide
  • Soluble polyimide comprising tertiary butyl and morpholinyl structure and preparation method of soluble polyimide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 3,3'-di-tert-butyl-4,4'-diaminophenyl-4'-morpholine to a 50 ml three-necked round-bottomed flask equipped with a mechanical stirrer, reflux condenser, and nitrogen air tube 1.0000 g (2.1201 mmol) of phenylmethane, 0.4624 g (2.1201 mmol) of 3,3′,4,4′-pyromellitic dianhydride, 13.20 g of N,N-dimethylacetamide, at room temperature The reaction was stirred for 24 hours to obtain a precursor polyamic acid solution. Then add the obtained precursor polyamic acid solution to 8ml of acetic anhydride-pyridine mixed solution with a volume ratio of 6:4, stir and react at room temperature for 1 hour, and stir and react at 120°C for 8 hours to obtain a viscous polyimide solution , cooled to room temperature, poured into 500 ml ethanol to precipitate, filtered, and the filtrate was dried in a vacuum oven at 80°C to obtain a light yellow fibrous soluble polyamide containing tert-butyl and morpholino structures. imine. Its structural formula is as follows:

[0029] .

Embodiment 2

[0031] Add 3,3'-di-tert-butyl-4,4'-diaminophenyl-4'-morpholine to a 50 ml three-necked round-bottomed flask equipped with a mechanical stirrer, reflux condenser, and nitrogen air tube 1.0000 g (2.1201 mmol) of phenylmethane, 0.6238 g (2.1201 mmol) of 3,3′,4,4′-biphenyltetracarboxylic dianhydride, 14.61 g of N,N-dimethylacetamide, at room temperature The reaction was stirred for 24 hours to obtain a precursor polyamic acid solution. Then add the obtained precursor polyamic acid solution into 8ml of acetic anhydride-pyridine mixed solution with a volume ratio of 6:4, stir the reaction at room temperature for 1 h, and stir the reaction at 120°C for 8 h to obtain a viscous polyimide solution. After cooling to room temperature, slowly pour it into 500ml of ethanol to precipitate, filter, put the filtrate into a vacuum drying oven and dry it at 80°C, and then obtain a light yellow fibrous soluble polyimide containing tert-butyl and morpholino structures. amine. Its structural for...

Embodiment 3

[0034]Add 3,3'-di-tert-butyl-4,4'-diaminophenyl-4'-morpholine to a 50 ml three-necked round-bottomed flask equipped with a mechanical stirrer, reflux condenser, and nitrogen air tube 1.0000 g (2.1201 mmol) of phenylmethane, 0.6577 g (2.1201 mmol) of 3,3′,4,4′-diphenyl ether tetracarboxylic dianhydride, 15.00 g of N,N-dimethylacetamide, in The reaction was stirred at room temperature for 24 hours to obtain a precursor polyamic acid solution. Then, the prepared precursor polyamic acid solution was added to 8 ml of acetic anhydride-pyridine mixed solution with a volume ratio of 6:4, stirred and reacted at room temperature for 1 hour, and then stirred and reacted at 120°C for 8 hours to obtain viscous polyimide solution. After cooling to room temperature, slowly pour it into 500ml of ethanol to precipitate, filter, put the filtrate into a vacuum drying oven and dry it at 80°C, and finally obtain a light yellow fibrous soluble polyamide containing tert-butyl and morpholino structu...

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Abstract

The invention discloses soluble polyimide comprising a tertiary butyl and morpholinyl structure and a preparation method of the soluble polyimide. The structural formula of the soluble polyimide comprising the tertiary butyl and morpholinyl structure is shown as follows. The soluble polyimide comprising the tertiary butyl and morpholinyl structure is obtained through reaction between aromatic diamine of a non-coplanar structure and various different tetracid dihydrides according to a 'two-step method'. The polyimide has excellent solubility property, can dissolve in high-boiling-point organic solvents including N, N'- dimethylformamide (DMF), N, N-dimethylacetamide (DMAc), N-methyl pyrrolidone (NMP), dimethyl sulfoxide (DMSO) and m-cresol and can also dissolve in low-boiling-point organic solvents including tetrahydrofuran (THF), chloroform (CHC13), dichloromethane (CH2C12), ethyl acetate and acetone.

Description

technical field [0001] The invention belongs to the field of polymer material science, in particular to a soluble polyimide containing tert-butyl and morpholino structures and a preparation method thereof. Background technique [0002] Polyimide is an important class of functional high-temperature-resistant polymers. It can not only be used as a composite material matrix, electronic packaging materials, and gas separation in the modern high-tech fields of membranes, but also has been widely used in aerospace, automotive industry, electronics, etc. electrical industry, etc. Polyimide (PI) is a class of high-performance polymers containing imide ring structure in the molecular structure. Although such high temperature resistant materials have excellent thermal and mechanical properties, due to their rigid main chain structure, strong interaction between molecules and close packing of molecular chains, most commercial polyimides Amines have a high melting temperature and are ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10
Inventor 黄孝华梅媚刘婵娟韦春
Owner 广西云智九沃实验仪器有限公司
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