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Ionic liquid and method for preparing aromatic polymer microspheres by adopting ionic liquid as solvent

A technology of aromatic polymers and ionic liquids, which is applied in the field of preparation of aromatic polymer microspheres, can solve problems such as high recycling costs, environmental and operator hazards, and macromolecular degradation, so as to reduce production costs and improve machinery Performance, the effect of spherical rounding

Inactive Publication Date: 2015-10-28
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, strong acid is very corrosive, which brings a lot of inconvenience to the equipment and operation of industrial production. At the same time, it is easy to cause the degradation of macromolecules when dissolved; while using traditional organic solvents, on the one hand, the volatility of organic solvents is harmful to the environment and operators. It causes great harm, and the cost of recycling is high. On the other hand, in order to improve the solubility of aromatic polymers in organic solvents, it is often necessary to add non-polar substances such as LiCl to organic solvents, and the addition of LiCl is also easy to cause macromolecules. degradation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh 1.0 g of polym-phenylene isophthalamide (PMIA), add it to 30 mL of 1-butyl-3-methyl-imidazolium chloride ([BMIM]Cl), and swell at 25°C After 1h, the temperature was raised to 80°C to dissolve for 5h to form a homogeneous solution. Add 150mL of liquid paraffin and 3mL of Span80 into a 500mL three-necked flask, heat it in an oil bath to 60°C, then slowly add the PMIA solution into the three-necked flask under low-speed stirring, set the stirring speed to 900r / min after the addition, and start timing. After 30 minutes, the heating was stopped and the temperature was slowly lowered to 50°C, and the PMIA solution was condensed into balls through reverse suspension and programmed cooling. During the stirring process, slowly add 100 mL of distilled water with a dropper to solidify the PMIA solution droplets to form PMIA microspheres, and continue stirring for 10 min after adding the distilled water. Stirring is stopped, and the oil-water phase is separated after standi...

Embodiment 2

[0026] Weigh 2.0 g of polybenzimidazole (PBI), add it to 50 mL of 1-ethyl-3-methyl-imidazolium bromide ([EMIM]Br), and swell at 40 °C for 2 h, then heat up to Dissolve at 100°C for 10h to form a homogeneous solution. Add 100mL castor oil and 2.5mL Tween85 into a 500mL three-necked flask, put it in an oil bath and heat to 80°C, then slowly add the PBI solution into the three-necked flask under low-speed stirring, and set the stirring speed to 700r / min after the addition ,start the timer. After 20 minutes, stop heating and slowly cool down to 30°C, and the PBI solution coagulates into balls through reverse suspension and programmed cooling. During the stirring process, slowly add 150 mL of distilled water with a dropper to solidify the PBI solution droplets to form PBI microspheres, and continue stirring for 30 min after adding the distilled water. Stop stirring, and separate the oil-water phase after standing still, and then use a centrifuge to separate the PBI microspheres f...

Embodiment 3

[0028] Weigh 2.0g of poly-p-phenylenebenzobisoxazole (PBO), add it to 50mL of 1-allyl-3-methyl-imidazolium chloride ([AMIM]CI), under the condition of 30°C After swelling for 1 hour, heat up to 70°C and dissolve for 7 hours to form a uniform solution. Add 300mL peanut oil and 7.5mL Span80 into a 500mL three-necked flask, put them in an oil bath and heat to 80°C, then slowly add the PBO solution into the three-necked flask under low-speed stirring, and set the stirring speed to 300r / min after the addition is complete. start the timer. After 30 minutes, stop heating and slowly cool down to 50°C, and the PBO solution condenses into balls through reverse suspension and programmed cooling. During the stirring process, slowly add 100 mL of distilled water with a dropper to solidify the PBO solution droplets to form PBO microspheres, and continue stirring for 20 min after adding the distilled water. Stop stirring, and separate the oil-water phase after standing still, and then use ...

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PUM

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Abstract

The present invention relates to an ionic liquid and a method for preparing aromatic polymer microspheres by adopting the ionic liquid as a solvent. According to the present invention, an aromatic polymer is dissolved in an ionic liquid, the obtained aromatic polymer solution is added to an oil phase, the aromatic polymer solution is condensed into liquid droplets through reverse phase suspension and programmed cooling, a curing agent is added to cure the aromatic polymer solution so as to form aromatic polymer microspheres, and finally washing and soaking are performed with distilled water to remove the ionic liquid component from the aromatic polymer microspheres so as to obtain the aromatic polymer microspheres; compared with the ionic liquid in the prior art, the ionic liquid of the present invention has characteristics of safety, no toxicity, no volatility, strong dissolving ability, recycling, environmental protection and operator health benefiting; and the aromatic polymer microspheres prepared by using the method has characteristics of porous structure, regular round shape, good mechanical property, good thermal stability, good acid resistance and good alkali resistance, wherein the particle sizes of 95% of the microspheres are distributed in the range of 40-200 [mu]m.

Description

technical field [0001] The invention relates to a method for preparing aromatic polymer microspheres, in particular to a solvent in the process of preparing aromatic polymer microspheres. Background technique [0002] Aromatic polymers have the characteristics of high strength, high modulus and high temperature resistance, and are important materials for national defense and special industries. Aromatic polymers are rigid rod-shaped polymers with large cohesive energy between macromolecules and are difficult to dissolve. They can only be dissolved in strong acids or very polar organic solvents. US Patents 3,767,756 and 5,296,185 disclose methods for dissolving and spinning poly(p-phenylene terephthalamide) and poly(p-phenylene benzobisoxazole) in strong acid respectively. However, strong acid is very corrosive, which brings a lot of inconvenience to the equipment and operation of industrial production. At the same time, it is easy to cause the degradation of macromolecules ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L77/10C08L79/04C08J3/16C08J9/00
CPCC08L77/10B01J13/02C08J3/16C08J9/0061C08L79/04C08L2201/08C08L2201/56C08L2205/02C08L2205/025C08L91/06C08L91/00
Inventor 万锕俊赵婷婷
Owner SHANGHAI JIAO TONG UNIV