CN1185283C - Thermoplastic high polymer micro balloons and method for preparing same - Google Patents
Thermoplastic high polymer micro balloons and method for preparing same Download PDFInfo
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- CN1185283C CN1185283C CNB011155299A CN01115529A CN1185283C CN 1185283 C CN1185283 C CN 1185283C CN B011155299 A CNB011155299 A CN B011155299A CN 01115529 A CN01115529 A CN 01115529A CN 1185283 C CN1185283 C CN 1185283C
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Abstract
The present invention relates to a thermoplastic high polymer microsphere which has the particle diameter of 0.1 to 10 mu m by detection through a scanning electron microscope. The thermoplastic high polymer microsphere is a polyamide microsphere. In the present invention, the high polymer microsphere is prepared from at least two kinds of thermoplastic high polymer resin with melting processing performance by a melt blending processing and high polymer melt separating method. The high polymer microsphere prepared by the method has a wide application range, and can be used for the mass preparation of micron order and submicron order high polymer microspheres comprising various high polymers comprising non-polar high polymers, polar polymers and the like and compositions of copolymers and the high polymers which can be melted and processed, and the high polymer microsphere has the advantages of simple preparation method and operation, low cost, etc.
Description
The application is to be 981006 the applying date, and application number is 98120124.5, and the invention exercise question is dividing an application of a kind of thermoplastic high polymer micro balloons and preparation method thereof.
The present invention relates to the technology that a kind of superpolymer is processed into microballoon, particularly relate to a kind of technology by the preparation high polymer micro balloons that is separated.
Te Kaiping 6-142505 has reported the manufacture method of hydrophobicity polyamino acid or cellulose microsphere, and amino acid or cellulosic organic solution are entered aqueous phase by the Glass tubing with many micropores, forms oil/water-in-oil emulsion.Organic solvent is removed in evaporation from emulsion, can get polyamino acid or cellulosic water dispersion.Separablely from the water dispersion go out to have monodispersed microballoon.Journal of Polymer Science:Part A:Polymer Chemistry, Vol.29,857-867 (1991) have reported the employing emulsion polymerisation process and have prepared poly (methyl methacrylate) micro-sphere.CN1132213 has reported a kind of synthetic method that combines with the swelling suspension polymerization technique of aqueous media system with the heterogeneous solution polymerization technique of organic medium system, and in polymerization, adopted the macromolecular solution hole forming technology, synthesized crosslinked polystyrene microsphere.But aforesaid method requires superpolymer to have good solvent, and complicated operating process, and yield is low, and the cost height is difficult for suitability for industrialized production.
It is low that the present invention has overcome in the prior art preparation high polymer micro balloons yield, output is little, the shortcoming that is difficult for production in enormous quantities, providing a kind of produces in batches, size can be regulated, and minimum grain size can reach 100nm thermoplastic high polymer micro balloons and a kind of technology that adopts melt-processed and high polymer molten phase disengagement method to prepare high polymer micro balloons.
A kind of thermoplastic high polymer micro balloons of the present invention detects by scanning electron microscope, and particle diameter is 0.1-10 μ m.
A kind of thermoplastic high polymer micro balloons of the present invention is the polymeric amide microballoon, and particle diameter is 0.1-10 μ m.
A kind of thermoplastic high polymer micro balloons of the present invention is that two or more the thermal plasticity high polymer resin that will have melt-processible passes through melt blending, be separated, a kind of component in the selective solvent dissolving superpolymer blend, more after filtration, step such as separation prepares.
Concrete preparation method step in the following order carries out:
1. with a kind of thermal plasticity high polymer resin and another kind of thermal plasticity high polymer resin as dispersion medium 0.1-20 by weight: 80-99.9 mixes, and obtains mixture.
2. said mixture is heated to 240-300 ℃, carries out melt blending, after 2-20 minute, extrude, Cast Strip, pelletizing through forcing machine, the superpolymer blended slice.
3. the section of gained superpolymer blend is placed inorganic heat-resisting media such as crystallization sodium-chlor or quartz sand, heat-treat under 240-300 ℃, be 10-60 minute heat-up time.
4. the solvent of superpolymer blend after the thermal treatment and selection is made into 1: 10 to 1: 1000 suspension, stirred 12-72 hour, fall as the thermal plasticity high polymer of dispersion medium is dissolved in the blend, remaining is thermoplastic high polymer micro balloons.
5. after filtration, washing is purified, and separates from suspension, makes high polymer micro balloons.
Above-mentioned a kind of thermoplastic resin can be but be not limited to be polystyrene, polyethylene, polypropylene, polyester or polymeric amide.
Above-mentioned another kind of thermoplastic resin can be but be not limited to be polystyrene, polyethylene, polypropylene, polyester or polymeric amide.
Above-mentioned superpolymer blend can be but be not limited to be the combination of above-mentioned two kinds of incompatible superpolymer such as polystyrene/polyethylene, polystyrene/polypropylene, polyphenylethylene/polyester, polyphenylethylene/polyamide blend.
The preparation method of above-mentioned polymeric amide microballoon step in the following order carries out:
1. with polyamide resin and another kind of thermal plasticity high polymer resin as dispersion medium 0.1-20 by weight: 80-99.9 mixes, and obtains mixture,
With said mixture at 240-300 ℃, after forcing machine carries out melt blending 2-20 minute, extrude, Cast Strip, pelletizing, the superpolymer blend section,
3. the section of gained superpolymer blend is placed inorganic heat-resisting media such as crystallization sodium-chlor or quartz sand, under 240-300 ℃, heat-treated 10-60 minute,
4. select solubilized dispersion medium superpolymer and can not dissolve the solvent of polymeric amide, cut into slices by 10 with the superpolymer blend after the thermal treatment: 1-1000: 1 mixes, be made into suspension, stirred 12-72 hour, and another kind of thermal plasticity high polymer was dissolved, after filtration, washing, purify, from suspension, separate, obtain the microballoon of polymeric amide.The intrinsic viscosity of above-mentioned polymeric amide is 2.0-3.5.
Above-mentioned a kind of thermoplastic resin as dispersion medium can be but be not limited to be polystyrene.
Above-mentioned solvent can be but be not limited to be toluene.
High polymer micro balloons of the present invention is by adjusting the processing parameter of producing apparatus, the controlled 0.1-10 μ m that is made as of particle diameter, the high polymer micro balloons of Zhi Zaoing is applied widely in this way, can be used for making in enormous quantities micron order and submicron order high polymer micro balloons, comprise non-polar polymer, multiple superpolymer that can melt-processed such as polar polymer, multipolymer and polymeric compositions have simple to operate, the low cost and other advantages of manufacture method.
Embodiment and Comparative Examples
The present invention intends by following embodiment and Comparative Examples simple declaration characteristics of the present invention and advantage, but can not think that the present invention only limits to the content of embodiment.
Embodiment 1
Being that 2.2 polymeric amide carries out vacuum-drying with intrinsic viscosity under 140 ℃, is that 9 polystyrene carries out mechanically mixing with melt flow index then, and the content of polymeric amide is 10wt%, and the content of polystyrene is 90wt%.The sample that mixes is adopted the twin screw extruder melt blending, and blending temperature is 280 ℃, and screw speed is 250 rev/mins, gets the superpolymer blend section.The superpolymer blend section is placed sodium chloride medium, 270 ℃ of following thermal treatments 30 minutes.Superpolymer blend section after the thermal treatment mixes by 6: 1000 with toluene, stirs after 48 hours, and with acidproof G6 funnel decompress filter, washing is purified, and isolates the polymeric amide microballoon.The polymeric amide microballoon is the ball of diameter at 0.4-2.7 μ m.
Claims (2)
1, a kind of thermoplastic high polymer micro balloons is characterized in that described thermoplastic high polymer micro balloons is that particle diameter is the polymeric amide microballoon of 0.1-10 μ m.
2, the preparation method of a kind of thermoplastic high polymer micro balloons according to claim 1 is characterized in that step is carried out in the following order:
(1) with intrinsic viscosity be polyamide resin and the polystyrene of 2.0-3.5,0.1-20: 80-99.9 mixes by weight, obtains mixture,
(2) with said mixture at 240-300 ℃, after forcing machine carries out melt blending 2-20 minute, extrude, Cast Strip, pelletizing, the blend section,
(3) above-mentioned blend section is placed crystallization sodium-chlor or the heat-resisting medium of quartz sand,, heat-treated 10-60 minute at 240-300 ℃,
(4) toluene is cut into slices by 10 with above-mentioned thermal treatment blend: 1-1000: 1 mixes, and stirs 12-72 hour, after the polystyrene dissolving, obtains the polymeric amide microballoon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011155299A CN1185283C (en) | 2001-04-27 | 2001-04-27 | Thermoplastic high polymer micro balloons and method for preparing same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011155299A CN1185283C (en) | 2001-04-27 | 2001-04-27 | Thermoplastic high polymer micro balloons and method for preparing same |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 98120124 Division CN1250061A (en) | 1998-10-06 | 1998-10-06 | Thermoplastic polymer microballoon and its preparation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1434069A CN1434069A (en) | 2003-08-06 |
| CN1185283C true CN1185283C (en) | 2005-01-19 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB011155299A Expired - Fee Related CN1185283C (en) | 2001-04-27 | 2001-04-27 | Thermoplastic high polymer micro balloons and method for preparing same |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101077910B (en) | 2006-05-23 | 2010-06-09 | 上海杰事杰新材料股份有限公司 | Method for preparing particle diameter controllable high molecular weight nylon micro-sphere |
| CN101768282B (en) * | 2008-12-29 | 2012-05-30 | 合肥杰事杰新材料股份有限公司 | Method for preparing nylon random copolymer micro-sphere with controllable melting point and grain diameter |
| CN103665839B (en) * | 2012-09-14 | 2017-02-08 | 合肥杰事杰新材料股份有限公司 | Polyamide microspheres and preparation method thereof |
| CN104045826B (en) * | 2014-06-25 | 2016-03-30 | 江苏科技大学 | A kind of environment-friendly type preparation method of polymeric amide microballoon |
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2001
- 2001-04-27 CN CNB011155299A patent/CN1185283C/en not_active Expired - Fee Related
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| CN1434069A (en) | 2003-08-06 |
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