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Polyimide microspheres and preparation method and application thereof

A polyimide and polyimide resin technology, applied in the field of functional polymer microspheres, can solve the problems of low yield and poor solubility of polyimide microspheres, and achieve high sphericity and glass transition. The effect of high temperature and uniform particle size distribution

Active Publication Date: 2012-09-26
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the poor solubility of the selected polyimide resin in organic solvents (<2wt%) in this method, the yield of polyimide microspheres is very low

Method used

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  • Polyimide microspheres and preparation method and application thereof
  • Polyimide microspheres and preparation method and application thereof
  • Polyimide microspheres and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] Example 1: Preparation from 3,3′,4,4′-diphenyl ether tetraacid dianhydride (ODPA) and 2,2′-bistrifluoromethyl-4,4′-biphenyldiamine (TFDB) Polyimide microspheres (emulsification stirring speed: 700rpm)

[0065] Add 2.41g (7.53mmol) TFDB and 10g NMP in a 500mL three-necked flask, stir until dissolved to form a homogeneous solution; add 2.26g (7.25mmol) ODPA and 10g NMP solvent to the above solution, and the system cools down to 5 °C, reacted for 2h; added 0.083g (0.56mmol) phthalic anhydride (PA), stirred and reacted for 12h to obtain a viscous polyamic acid resin solution with a solid content of 20wt%. Add 2g of isoquinoline and 20g of toluene to the polyamic acid resin solution, heat to reflux for 3h; adjust the reaction temperature to 180°C, react for 5h, and then distill off the toluene. The temperature of the reaction system was lowered to room temperature, and the reaction solution was slowly precipitated in absolute ethanol, and the obtained precipitate was filter...

Embodiment 2

[0075] Example 2: Preparation from 3,3′,4,4′-diphenyl ether tetraacid dianhydride (ODPA) and 2,2′-bistrifluoromethyl-4,4′-biphenyldiamine (TFDB) Polyimide microspheres (emulsification stirring speed: 600rpm)

[0076] The soluble polyimide resin prepared in Example 1 was dissolved in DMAc to prepare a 7.5wt% solution. A 5 wt % polyvinylpyrrolidone aqueous solution was added to the solution for emulsification, and the stirring speed was controlled at 600 rpm. Microspheres with smooth surfaces were obtained, which contained some rod-shaped particles. The particle size of microspheres is 12 μm, the degree of sphericity: 95%, and the width of particle size distribution: 0.81. The rod-shaped particles have a length of 20-40 μm. SEM spectrum as Figure 5 shown.

Embodiment 3

[0077] Example 3: Preparation from 3,3′,4,4′-diphenyl ether tetraacid dianhydride (ODPA) and 2,2′-bistrifluoromethyl-4,4′-biphenyldiamine (TFDB) Polyimide microspheres (emulsification stirring speed: 500rpm)

[0078] The soluble polyimide resin prepared in Example 1 was dissolved in DMAc to prepare a 7.5wt% solution. Add 5wt% polyvinylpyrrolidone aqueous solution to the solution for emulsification, and control the stirring speed to 500rpm. Microspheres with smooth surfaces were obtained, which contained some rod-shaped particles. The particle size of the microsphere is 11 μm, the degree of sphericity: 90%, and the width of particle size distribution: 1.1. The rod-shaped particles have a length of 10-50 μm. SEM spectrum as Image 6 shown.

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Abstract

The invention discloses polyimide microspheres and a preparation method and application thereof. In the preparation method disclosed by the invention, under forcibly shearing condition, the aqueous solution of dispersing agent is added to soluble polyimide (with structure showed in formulaI)solution, and through the emulsification of resin solution, polyimide microspheres with controllable particle size and appearance can be obtained. The polyimide microspheres prepared through the method have the characteristics of high sphericity, even particle size distribution, glossy surface, high glass transition temperature (Tg) and the like. The polyimide microspheres prepared through the method can be applied in the fields such as catalyst carrier, composite material toughening and panel partition of liquid crystal displays. (FormulaI).

Description

technical field [0001] The invention belongs to the field of functional polymer microspheres, and relates to a polyimide microsphere and its preparation method and application. Background technique [0002] Polyimide has excellent high temperature resistance, low temperature resistance, high strength and high toughness, high electrical insulation, corrosion resistance, radiation resistance, low dielectric constant and dielectric loss, and can be processed into films, fibers, adhesives, Various types of materials such as engineering plastics and composite materials have been widely used in high-tech fields such as aerospace, microelectronics, advanced display, solar energy, and wind power generation. However, it is quite technically difficult to process polyimide into highly spherical microspheres with diameters ranging from nanometers to micrometers. Currently, there are no commercial polyimide microspheres on the market. Polymer microspheres with high sphericity and excell...

Claims

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Application Information

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IPC IPC(8): C08G73/10C08L79/08B01J32/00
Inventor 杨士勇沈登雄刘金刚
Owner INST OF CHEM CHINESE ACAD OF SCI
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