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Process for preparing polymer ultra-fine particles by applying supercritical fluid

A technology of supercritical fluid and ultrafine particles, applied in the production of bulk chemicals, etc., to achieve the effect of perfect crystallization, pure polymer particles, and stable crystal form

Inactive Publication Date: 2010-04-14
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] So far, there is no report on the method of obtaining ultrafine particles with better morphology and crystallinity and wide application to polymer systems through simple equipment and methods

Method used

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  • Process for preparing polymer ultra-fine particles by applying supercritical fluid
  • Process for preparing polymer ultra-fine particles by applying supercritical fluid
  • Process for preparing polymer ultra-fine particles by applying supercritical fluid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Embodiment 1, supercritical carbon dioxide prepares ultra-high molecular weight polyethylene ultrafine particles

[0055] (1) 1g of ultra-high molecular weight (weight-average relative molecular mass is 3.8×10 6 g / mol, relative molecular mass distribution is 6.8) polyethylene joins in the 50ml reactor, utilizes pump to join carbon dioxide gas in the reactor, and make the pressure in the reactor after adding carbon dioxide gas stabilize at 10MPa;

[0056] (2) Heating the reactor of step (1) to 300°C, maintaining the temperature of 300°C and the pressure of 10MPa for 2 hours, then cooling the reactor to 100°C and maintaining it for 1 hour;

[0057] (3) Release the pressure after the reaction kettle of step (2) is cooled to room temperature in a water bath at room temperature, and at the same time use the sample bottle equipped with ethanol as a collection device to collect the CO emitted from the outlet of the reaction kettle. 2 For the carried substances, the remaining ...

Embodiment 2

[0059] Embodiment 2, supercritical carbon dioxide prepares ultra-high molecular weight polyethylene ultrafine particles

[0060] (1) 10g ultra-high molecular weight (weight-average relative molecular mass is 3.8×10 6g / mol, relative molecular mass distribution is 6.8) polyethylene joins in 1 liter reactor, utilizes pump to join carbon dioxide gas in reactor, and make the pressure in the reactor after adding carbon dioxide gas stabilize at 20MPa;

[0061] (2) Heating the reaction kettle of step (1) to 250°C, maintaining the temperature of 250°C and the pressure of 20MPa for 2 hours, then naturally cooling to 121°C for 50 minutes at a constant temperature;

[0062] (3) Naturally cool the reactor in step (2) to 90°C for 30 minutes, then cool the reactor to room temperature in the air and release the pressure, and at the same time use the sample bottle containing ethanol as a collection device to collect the outlet of the reactor Ejected CO 2 For the carried substances, the remai...

Embodiment 3

[0064] Embodiment 3, supercritical ethanol prepares ultra-high molecular weight polyethylene ultrafine particles

[0065] (1) 0.1g ultra-high molecular weight (weight-average relative molecular mass is 3.8×10 6 g / mol, relative molecular mass distribution is 6.8) polyethylene joins in the 10ml reactor, and fills up ethanol in the reactor;

[0066] (2) Heating the reactor of step (1) to 300° C., making the pressure produced by the ethanol in the reactor be 45 MPa, maintaining the temperature of 300° C. and the pressure of 45 MPa for 2 hours, then naturally cooling to 130° C. for 4 hours at a constant temperature;

[0067] (3) After the reaction kettle in step (2) is cooled to room temperature in a water bath at room temperature, directly use a device equipped with ethanol to collect the material in the reaction kettle, and take out the remaining polyethylene that has not produced polyethylene ultrafine particles for reuse ; Then vacuum-dry the obtained polyethylene ultrafine pa...

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Abstract

The invention relates to a process for preparing polymer ultra-fine particles, in particular to a process for preparing polymer ultra-fine particles by applying supercritical fluid, which utilizes the supercritical fluid to process one type of polymer or a mixture of various types of polymers to prepare polymer ultra-fine particles or polymer microcapsule ultra-fine particles. As dissolubility to polymer is increased in a supercritical fluid state, polymer can be precipitated from the supercritical fluid after the supercritical fluid state is eliminated, and then polymer ultra-fine particles or polymer microcapsule ultra-fine particles with high degree of crystallinity and fine shape can be prepared after thermostatic treatment. Besides, the prepared ultra-fine particles are narrow in distribution, and shapes thereof can be controlled into regular spheres. The process is simple in technique and easy in operation without complex devices, the prepared ultra-fine particles are regular in shapes, stable in crystalline form, higher in crystallinity and higher in application value and are adoptable to industrialized production.

Description

technical field [0001] The invention relates to a method for preparing polymer ultrafine particles, in particular to a method for preparing polymer ultrafine particles using supercritical fluid. Background technique [0002] In recent years, ultrafine particles having a particle diameter of approximately 0.1 to 50 μm have attracted attention in many fields, and have become necessary for various applications. For example, it can be used as a resin modifier, as a light diffusing agent or matting agent in the field of coatings or in various displays, as a smoothness imparting agent in the field of cosmetics, and as a material for toners in the field of electronic copiers. It is used in the development of chromatographic stationary phases in the chemical industry, absorbents for gases or liquids, catalyst supports, and loaders in controllable drug release systems in biological materials, etc. Inorganic particles are gradually replaced by polymer particles. The technology of sup...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/12C08L23/06C08L23/12C08L25/06C08L33/12C08L67/02C08L77/06
CPCY02P20/54
Inventor 王长明张秀芹赵莹韩布兴王笃金
Owner INST OF CHEM CHINESE ACAD OF SCI
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