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Inorganic whisper reinforced polyolefin composite material in-situ filled polymerization preparing method

A composite material and inorganic whisker technology, which is applied in the field of in-situ filling and polymerization preparation of inorganic whisker-reinforced polyolefin composite materials, and achieves the effects of remarkable tensile properties, improved mechanical properties and smooth surface.

Inactive Publication Date: 2007-01-24
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

[0010] Although people have adopted various methods to surface-treat whiskers or change different processing and molding methods, there are no patents and literature reports on the preparation of polyolefin / inorganic whisker composites by in-situ polymerization.

Method used

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  • Inorganic whisper reinforced polyolefin composite material in-situ filled polymerization preparing method
  • Inorganic whisper reinforced polyolefin composite material in-situ filled polymerization preparing method
  • Inorganic whisper reinforced polyolefin composite material in-situ filled polymerization preparing method

Examples

Experimental program
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Effect test

Embodiment 1

[0040] 0.6 g of magnesium salt whiskers that have been dried, dehydrated and deoxygenated, in N 2 Under protection, add it to a dry, dehydrated and deoxygenated polymerization bottle. After replacing the ethylene monomer several times, add 100mL of toluene and stir for 30 minutes to ensure that the whiskers are fully dispersed. Quickly add the catalyst TiCl with a syringe. 4 1mL, stir until the toluene absorption is stable, then add the measured triethylaluminum according to the Al / Ti (molar ratio) 30 / 1, raise the temperature to 80°C, keep the ethylene pressure at 0.1MPa to start polymerization, react for 30 minutes, add ethanol to stop the reaction , left to stand for 12 hours, filtered, and vacuum-dried to obtain 12.8 grams of fluffy powdery white polyethylene / whisker composites. After injection molding, the mechanical properties of the composite material were measured, the tensile strength was 39MPa, the tensile modulus was 960MPa, and the elongation at break was 58%.

Embodiment 2

[0042] 1.2 grams of calcium sulfate whiskers that have been dried, dehydrated and deoxidized are treated in N 2 Under protection, add it to a dry, dehydrated and deoxygenated polymerization bottle. After replacing the ethylene monomer several times, add 100mL cyclohexane and stir for 30 minutes to ensure that the whiskers are fully dispersed. Quickly add the catalyst TiCl with a syringe 4 1ml, stir until the toluene absorption is stable, add triethylaluminum according to Al / Ti (molar ratio) 30 / 1, raise the temperature to 80°C, and keep the ethylene pressure at 0.1MPa to start polymerization. After 30 minutes of reaction, add ethanol to stop the reaction , left to stand for 12 hours, filtered, and vacuum-dried to obtain 17.3 grams of fluffy powdery white polyethylene / whisker composites. After injection molding, the mechanical properties of the composite material were measured, the tensile strength was 41MPa, the tensile modulus was 1.2GPa, and the elongation at break was 22%. ...

Embodiment 3

[0044] 1.2 grams of magnesium salt whiskers that have been dried, dehydrated and deoxidized are treated in N 2 Under protection, add it to a dry, dehydrated and deoxygenated polymerization bottle. After replacing the ethylene monomer several times, add 100mL of toluene and stir for 30 minutes to ensure that the whiskers are fully dispersed. Quickly add the catalyst TiCl with a syringe. 4 1ml, stir until toluene is absorbed stably, add metered triisobutylaluminum according to Al / Ti (molar ratio) 30 / 1, heat up to 80°C, keep ethylene pressure at 0.1MPa to start polymerization, react for 30 minutes, add ethanol to stop React, leave standstill 12 hours, filter, vacuum-dry, obtain fluffy powdery white polyethylene / whisker composite material 8.2 grams. After injection molding, the mechanical properties of the composite material were measured, the tensile strength was 36MPa, the tensile modulus was 990MPa, and the elongation at break was 62%.

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Abstract

The invention relates to a kind of insitu filling polymerization-manufacturing method of inorganic whisker intensification polyolefin composite material. Load olefinic polymerization catalyst in the surface of inorganic whisker with preliminary stirring-dispersing treatment, and then take alkene monomer polymerization in its surface in order to get polyolefin / whisker composite material. The composite material is composed with 3-80% inorganic mineral whisker and 20-97% polyolefin polymer. The manufacturing method in the invention is convenient. The composite material manufactured by the method has high filling extent of whisker, retentive slenderness ratio of whisker, and also the whisker has well distribution in matrix polymer and fine adhesion with matrix interface, so that it can give full play to intensification characteristic of whisker, in order to get polyolefin / inorganic whisker composite material with the advantages such as easiness to formation and processing, fine cleanliness of product, and excellent mechanical property. Plastics matrix can be manufactured into polyolefin from low molecular weight, middle molecular weight, and high molecular weight to superhigh molecular weight, such as polypropylene or polythene. The material acquired can be used not only as structural material by direct injection formation, but also as masterbatch after having crossblend with commercial polyolefine.

Description

technical field [0001] The invention relates to a preparation method of polyolefin composite material, in particular to a preparation method of in-situ filling polymerization of inorganic whisker reinforced polyolefin composite material. Background technique [0002] Thermoplastic polymer composites have a wide variety of uses. The traditional preparation method is to prepare thermoplastic polymer composites by melt blending. The disadvantage of this method is that the dispersion of the filler in the matrix polymer is not uniform enough, especially for fine-sized fillers. In addition, the interfacial bonding performance between the filler and the matrix polymer surface is not good enough, which affects the improvement of the mechanical properties of this type of material. By improving the mixing effect, or surface treatment of fillers, such as using coupling agents or surface coating (also known as microencapsulation), the mechanical properties of composite materials can b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L23/00C08K7/04C08F2/44
Inventor 张军朱宁何嘉松孙文华
Owner INST OF CHEM CHINESE ACAD OF SCI
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