Preparation method of porous polyimide microspheres

A technology of polyimide microspheres and polyamic acid, which is applied in the field of preparation of porous polyimide microspheres, can solve problems such as low solid content, poor reproducibility of preparation methods, and difficult control of micropore morphology and distribution. Achieve the effect of improving production efficiency and simplifying steps

Inactive Publication Date: 2013-11-06
TAIYUAN UNIV OF TECH
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  • Abstract
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Problems solved by technology

[0005] The purpose of the present invention is to overcome the disadvantages of the existing porous polyimide microspheres, such as the difficulty in controlling the micropore morphology and distribution, the poor reproducibility of the preparation method, and the low solid content, and provide a simple process, large specific surface area and microporous polyimide microspheres. A method for preparing micron-scale porous polyimide microspheres with relatively uniform distribution, good reproducibility, and high monomer solid content

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  • Preparation method of porous polyimide microspheres
  • Preparation method of porous polyimide microspheres
  • Preparation method of porous polyimide microspheres

Examples

Experimental program
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Effect test

Embodiment 1

[0036] A preparation method for preparing porous polyimide microspheres, the specific preparation method is as follows:

[0037] Step one, prepare the continuous phase. Dissolve 10.0g of surfactant Span85 in 50ml of liquid paraffin to become the continuous phase;

[0038] Step 2, preparing the dispersed phase. Weigh 1.0g of 4,4'-diaminodiphenyl ether and dissolve it in N,N-dimethylformamide to form a dispersed phase;

[0039] Step 3, forming a non-aqueous inverse emulsion. According to the volume ratio: 1:5 (volume ratio of N,N-dimethylformamide to liquid paraffin), mix the continuous phase prepared in step 1 and the dispersed phase prepared in step 2, and emulsify with ultrasonic stirring , the emulsification time is 60 minutes, adjust the temperature of the system to 20°C, after forming a stable non-aqueous inverse emulsion, add ether at a volume ratio of 1:1 (volume ratio of liquid paraffin to ether);

[0040] Step 4, preparing polyamic acid emulsion and its chemical imid...

Embodiment 2

[0043] This example is basically the same as Example 1, except that 6.0g of surfactant (the mass ratio of Span85 and monoaminopolyetheramine is 2:1) is dissolved in 50ml of liquid paraffin to become the continuous phase; 1.0g of 4,4'-diaminodiphenyl ether is dissolved in N,N-dimethylformamide to become a dispersed phase; the volume ratio of 1:10 (N,N-dimethylacetamide and liquid paraffin volume ratio), mix the continuous phase prepared in step 2 with the dispersed phase prepared in step 1, and emulsify with ultrasonic stirring. The emulsification time is 60 minutes, and the temperature of the system is adjusted to 15°C until a stable non-aqueous reverse phase is formed. After the emulsion, methanol was added in a volume ratio of 10:1 (volume ratio of liquid paraffin to methanol); under nitrogen protection and constant stirring, 1.14 g of solid pyromellitic anhydride was added to the non-aqueous inverse emulsion, After 6 hours of reaction, 2ml of pyridine / acetic anhydride (mola...

Embodiment 3

[0045] This example is basically the same as Example 1, except that 5.0g of surfactant (the mass ratio of Span60 and monoaminopolyetheramine is 1:1) is dissolved in 50ml of liquid paraffin to become the continuous phase; 1.0g of 4,4'-diaminodiphenyl ether is dissolved in N,N-dimethylformamide to become a dispersed phase; the volume ratio of 1:10 (N,N-dimethylacetamide and liquid paraffin volume ratio), mix the continuous phase prepared in step 2 with the dispersed phase prepared in step 1, and emulsify with ultrasonic stirring. The emulsification time is 60 minutes, and the temperature of the system is adjusted to 15°C until a stable non-aqueous reverse phase is formed. After the emulsion, tetrahydrofuran was added at a volume ratio of 2:1 (volume ratio of liquid paraffin to tetrahydrofuran); under nitrogen protection and constant stirring, 1.14 g of solid pyromellitic anhydride was added to the non-aqueous inverse emulsion, After 6 hours of reaction, 3ml of pyridine / acetic an...

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Abstract

The invention provides a preparation method of porous polyimide microspheres. Non-aqueous reversed-phase emulsion is adopted as a reaction system; liquid paraffin is used as a continuous phase; N,N-dimethylformamide is used as a dispersed phase, and lipophilic sorbitan ester, or a compound of the lipophilic sorbitan ester and another surface active agent is used as an emulsifying agent; used monomers are respectively dianhydride and diamine; and a used pore-forming agent is a low-boiling-point organic solvent. The method provided by the invention has the advantages of simple process, high reproducibility, high solid content of the monomers, uniform grain size of the microspheres, even pore distribution and wide application prospect.

Description

technical field [0001] The invention relates to a preparation method of porous polyimide microspheres, in particular to a preparation method of porous polyimide microspheres. Background technique [0002] Porous materials have the characteristics of low relative density, large specific surface area, and easy chemical modification on the surface. They have high application value in the fields of adsorption and separation, catalyst carriers, biological tissue materials, aerospace materials, and microelectronic materials. In addition to the above characteristics, the porous microspheres prepared by polyimide also have high mechanical strength, excellent dielectric properties, chemical corrosion resistance and radiation resistance, especially its excellent resistance to Thermal properties, can better make up for the defect that polystyrene, polyacrylic acid and other porous microspheres with low thermal stability cannot be used for a long time under high temperature conditions. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/10C08J9/28C08L79/08
Inventor 刘妙青林立卢建军黄伟
Owner TAIYUAN UNIV OF TECH
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