CN104987445A - Organobentonite and multi-wall carbon nanotube reinforced polypropylene resin for automobile parts and preparation method thereof - Google Patents
Organobentonite and multi-wall carbon nanotube reinforced polypropylene resin for automobile parts and preparation method thereof Download PDFInfo
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Abstract
Organobentonite and multi-wall carbon nanotube reinforced polypropylene resin for automobile parts is prepared, by weight, by the following raw materials of 350-380 parts of liquid propylene, 2.5-3.5 parts of multi-wall carbon nanotube load Ti-Zr catalysts, 100-110 parts of liquid ethylene, 7-9 parts of triethyl aluminum, 5.4-6.2 parts of diphenyldimethoxysilane, 0.8-1.1 parts of organobentonite, 50-60 parts of n-heptane, appropriate hydrogen, 0.1-0.2 part of ammonium hexafluorosilicate, 15-20 parts of 1-butylene, 0.1-0.2 part of thionyl chloride, 0.1-0.2 part of 2-aminopyridine, 0.1-0.2 part of ethidene diamine and 8-12 parts of water. According to the organobentonite and multi-wall carbon nanotube reinforced polypropylene resin for the automobile parts and a preparation method thereof, modification is conducted on the multi-wall carbon nanotube load Ti-Zr catalysts, the activity of the catalysts is improved, polarity differences are reduced, the binding force between multi-wall carbon nanotubes and macromolecules is increased, and the mechanical property of polypropylene is improved; the organobentonite is used in cooperation, the toughness and the elongation at break of the polypropylene are improved, and the polypropylene is suitable for manufacturing the automobile parts.
Description
Technical field
The present invention relates to polypropylene production technical field, particularly relate to a kind of auto parts organobentonite and multi-walled carbon nano-tubes Reinforced Polypropylene resin and preparation method thereof.
Background technology
In polyolefine, introduce nanoparticle (as polynite, carbon nanotube and graphene oxide) become polyolefin modified and important channel that is high performance.Be scattered in inorganic rigid particle in polyolefin substrate at loading level seldom (being usually less than 5%(w) with nanoscale) just can significantly improve or improve polyolefinic mechanical property, thermal characteristics and resistive energy, and there is functional nanoparticles (as redox graphene etc.) such as extremely strong conductive and heat-conductive also can give polyolefine certain electrical and thermal conductivity.Therefore, getting a promotion further of olefin polymerization nanometer composite material, Application Areas can significantly be expanded.
Preparing in the numerous method of carbon nanotube composite polypropylene, in-situ polymerization technology is considered to one of the most effective method.This technology is the catalytic active center catalyzing propone monomer polymerization reactions by carbon nanotube loaded transition-metal catalyst, avoid the thermodynamic (al) rigors caused by polypropylene and carbon nanotube polarity difference to a certain extent, and then prepare the carbon nanotube Reinforced Polypropylene resin of excellent performance.But carbon nanotube and polypropylene still exist polarity difference, need improving technique, improve the performance of carbon nanotube Reinforced Polypropylene further.Can also assign to improve polyacrylic performance by improving polyacrylic one-tenth.
Summary of the invention
The object of the present invention is to provide a kind of auto parts organobentonite and multi-walled carbon nano-tubes Reinforced Polypropylene resin, this resin originally has good mechanical property and higher elongation at break.
Technical scheme of the present invention is as follows:
A kind of auto parts organobentonite and multi-walled carbon nano-tubes Reinforced Polypropylene resin, is characterized in that being made up of the raw material of following weight part: propylene liquid 350-380, carbon multi-wall nano tube loaded Ti-Zr catalyzer 2.5-3.5, liquid ethylene 100-110, triethyl aluminum 7-9, dimethoxydiphenylsilane 5.4-6.2, organobentonite 0.8-1.1, normal heptane 50-60, hydrogen are appropriate, ammonium hexafluorosilicate 0.1-0.2,1-butylene 15-20, thionyl chloride 0.1-0.2, PA 0.1-0.2, quadrol 0.1-0.2, water 8-12.
Described auto parts organobentonite and multi-walled carbon nano-tubes Reinforced Polypropylene resin, is characterized in that: it be 5%, Zr is 2% that described carbon multi-wall nano tube loaded Ti-Zr catalyzer contains Ti mass percent.
The production method of described auto parts organobentonite and multi-walled carbon nano-tubes Reinforced Polypropylene resin, is characterized in that:
(1) ammonium hexafluorosilicate, thionyl chloride, PA, quadrol are added to the water, add carbon multi-wall nano tube loaded Ti-Zr catalyzer, organobentonite again, be heated to 60-70 DEG C, stirring reaction 20-30 minute, drying, obtains the carbon multi-wall nano tube loaded Ti-Zr catalyzer of modification;
(2) in reactor, add the normal heptane of 4/5, add the propylene liquid of 1/5, the carbon multi-wall nano tube loaded Ti-Zr catalyzer of modification, the triethyl aluminum of 1/5, the dimethoxydiphenylsilane of 1/5, mix, pass into the hydrogen of the 0.02-0.08% of propylene liquid quality again, under 50-80 DEG C, 2-3MPa condition, carry out slurry polymerization 7-9 hour, then add the liquid ethylene of 1/5 and the 1-butylene of 1/3, continue reaction 7-9 hour, obtain the polypropylene of loading multi-wall carbon nanotubes;
(3) under normal temperature, normal pressure, autoclave is full of propylene gas, then passes into the hydrogen of 0.02-0.08% of remaining liquid propylene quality, add 1/2 remaining liquid third rare; Remaining triethyl aluminum, dimethoxydiphenylsilane are added in remaining normal heptane and stirs, add in reactor, add the polypropylene of loading multi-wall carbon nanotubes again, add remaining propylene liquid again, be warming up to 50-80 DEG C, pressure rises to 2-3MPa, reaction 5-8 hour, temperature of reaction kettle is down to room temperature, emptying propylene, then passes into reactor by remaining ethene gasification, then adds other remaining component, be warming up to 50-80 DEG C, pressure rises to 2-3MPa, reaction 8-10 hour, emptying gas, vacuum-drying, to obtain final product.
Beneficial effect of the present invention
The present invention, by carrying out modification to carbon multi-wall nano tube loaded Ti-Zr catalyzer, improves the activity of catalyzer, reduces polarity difference, adds the bonding force between multi-walled carbon nano-tubes and polymer, improves polyacrylic mechanical property; With the use of organobentonite, improve polyacrylic toughness and elongation at break.Production technique of the present invention achieves effective dispersion of nanoparticle and effective control of morphology, makes this resin have higher impelling strength, keeps good intensity and rigidity simultaneously, and this polypropylene is applicable to make auto parts.
Embodiment
A kind of auto parts organobentonite and multi-walled carbon nano-tubes Reinforced Polypropylene resin, be made up of the raw material of following weight part (kilogram): propylene liquid 360, carbon multi-wall nano tube loaded Ti-Zr catalyzer 3, liquid ethylene 105, triethyl aluminum 8, dimethoxydiphenylsilane 5.9, organobentonite 0.9, normal heptane 55, hydrogen are appropriate, ammonium hexafluorosilicate 0.1,1-butylene 18, thionyl chloride 0.1, PA 0.1, quadrol 0.1, water 10.
Described auto parts organobentonite and multi-walled carbon nano-tubes Reinforced Polypropylene resin, is characterized in that: it be 5%, Zr is 2% that described carbon multi-wall nano tube loaded Ti-Zr catalyzer contains Ti mass percent.
The production method of described auto parts organobentonite and multi-walled carbon nano-tubes Reinforced Polypropylene resin, is characterized in that:
(1) ammonium hexafluorosilicate, thionyl chloride, PA, quadrol are added to the water, add carbon multi-wall nano tube loaded Ti-Zr catalyzer, organobentonite again, be heated to 65 DEG C, stirring reaction 25 minutes, drying, obtains the carbon multi-wall nano tube loaded Ti-Zr catalyzer of modification;
(2) in reactor, add the normal heptane of 4/5, add the propylene liquid of 1/5, the carbon multi-wall nano tube loaded Ti-Zr catalyzer of modification, the triethyl aluminum of 1/5, the dimethoxydiphenylsilane of 1/5, mix, pass into the hydrogen of 0.05% of propylene liquid quality again, at 60 DEG C, under 2MPa condition, carry out slurry polymerization 8 hours, then add the liquid ethylene of 1/5 and the 1-butylene of 1/3, continue reaction 8 hours, obtain the polypropylene of loading multi-wall carbon nanotubes;
(3) under normal temperature, normal pressure, autoclave is full of propylene gas, then pass into remaining liquid propylene quality 0.05% hydrogen, add 1/2 remaining liquid third rare; Remaining triethyl aluminum, dimethoxydiphenylsilane are added in remaining normal heptane and stirs, add in reactor, add the polypropylene of loading multi-wall carbon nanotubes again, add remaining propylene liquid again, be warming up to 70 DEG C, pressure rises to 2MPa, reacts 7 hours, temperature of reaction kettle is down to room temperature, emptying propylene, then passes into reactor by remaining ethene gasification, then adds other remaining component, be warming up to 70 DEG C, pressure rises to 2MPa, reacts 9 hours, emptying gas, vacuum-drying, to obtain final product.
Experimental data:
The polypropylene of this embodiment is through extrusion moulding, and after tested, tensile strength is 35MPa, and elongation at break is 860%, and under normal temperature, notched Izod impact strength reaches 33.8kJ/ ㎡, and modulus in flexure is 650Mpa.
Claims (3)
1. auto parts organobentonite and a multi-walled carbon nano-tubes Reinforced Polypropylene resin, is characterized in that being made up of the raw material of following weight part: propylene liquid 350-380, carbon multi-wall nano tube loaded Ti-Zr catalyzer 2.5-3.5, liquid ethylene 100-110, triethyl aluminum 7-9, dimethoxydiphenylsilane 5.4-6.2, organobentonite 0.8-1.1, normal heptane 50-60, hydrogen are appropriate, ammonium hexafluorosilicate 0.1-0.2,1-butylene 15-20, thionyl chloride 0.1-0.2, PA 0.1-0.2, quadrol 0.1-0.2, water 8-12.
2. auto parts organobentonite according to claim 1 and multi-walled carbon nano-tubes Reinforced Polypropylene resin, is characterized in that: it be 5%, Zr is 2% that described carbon multi-wall nano tube loaded Ti-Zr catalyzer contains Ti mass percent.
3. the production method of the auto parts organobentonite according to claim 1 and 2 and multi-walled carbon nano-tubes Reinforced Polypropylene resin, is characterized in that:
(1) ammonium hexafluorosilicate, thionyl chloride, PA, quadrol are added to the water, add carbon multi-wall nano tube loaded Ti-Zr catalyzer, organobentonite again, be heated to 60-70 DEG C, stirring reaction 20-30 minute, drying, obtains the carbon multi-wall nano tube loaded Ti-Zr catalyzer of modification;
(2) in reactor, add the normal heptane of 4/5, add the propylene liquid of 1/5, the carbon multi-wall nano tube loaded Ti-Zr catalyzer of modification, the triethyl aluminum of 1/5, the dimethoxydiphenylsilane of 1/5, mix, pass into the hydrogen of the 0.02-0.08% of propylene liquid quality again, under 50-80 DEG C, 2-3MPa condition, carry out slurry polymerization 7-9 hour, then add the liquid ethylene of 1/5 and the 1-butylene of 1/3, continue reaction 7-9 hour, obtain the polypropylene of loading multi-wall carbon nanotubes;
(3) under normal temperature, normal pressure, autoclave is full of propylene gas, then passes into the hydrogen of 0.02-0.08% of remaining liquid propylene quality, add 1/2 remaining liquid third rare; Remaining triethyl aluminum, dimethoxydiphenylsilane are added in remaining normal heptane and stirs, add in reactor, add the polypropylene of loading multi-wall carbon nanotubes again, add remaining propylene liquid again, be warming up to 50-80 DEG C, pressure rises to 2-3MPa, reaction 5-8 hour, temperature of reaction kettle is down to room temperature, emptying propylene, then passes into reactor by remaining ethene gasification, then adds other remaining component, be warming up to 50-80 DEG C, pressure rises to 2-3MPa, reaction 8-10 hour, emptying gas, vacuum-drying, to obtain final product.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103910930A (en) * | 2012-12-31 | 2014-07-09 | 中国科学院化学研究所 | Polypropylene intra-autoclave alloy having carbon nanotubes, preparation method for the alloy, and applications thereof |
| CN103980609A (en) * | 2014-04-30 | 2014-08-13 | 中国科学院化学研究所 | Nanoparticle-containing polypropylene inside-kettle alloy capable of being used for 3D printing, and preparation method and application thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103910930A (en) * | 2012-12-31 | 2014-07-09 | 中国科学院化学研究所 | Polypropylene intra-autoclave alloy having carbon nanotubes, preparation method for the alloy, and applications thereof |
| CN103980609A (en) * | 2014-04-30 | 2014-08-13 | 中国科学院化学研究所 | Nanoparticle-containing polypropylene inside-kettle alloy capable of being used for 3D printing, and preparation method and application thereof |
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