CN104987446A - Wood powder and multi-walled carbon nanotube reinforced polypropylene resin and preparation method thereof - Google Patents
Wood powder and multi-walled carbon nanotube reinforced polypropylene resin and preparation method thereof Download PDFInfo
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Abstract
Wood powder and multi-walled carbon nanotube reinforced polypropylene resin is prepared from, by weight, 350-380 parts of liquid propylene, 2.5-3.5 parts of a multi-walled carbon nanotube load Ti-Zr catalyst, 110-130 parts of liquid ethylene, 7-9 parts of triethyl aluminum, 5.4-6.2 parts of diphenyldimethoxysilane, 1-1.5 parts of nanometer silver colloid, 0.1-0.3 part of ceric oxide, 0.2-0.3 part of MoO3, 4-5 parts of organobentonite, 0.6-0.9 part of maleic anhydride, 4-5 parts of wood powder, 50-60 parts of n-heptane, appropriate hydrogen, 0.1-0.2 part of ammonium hexafluorosilicate, 9-12 parts of 1-octylene and 8-12 parts of water. According to the wood powder and multi-walled carbon nanotube reinforced polypropylene resin, due to the fact that the wood powder and the organobentonite are used for modification, the shock resistance and the fire resistance of polypropylene are reinforced; due to the fact that the nanometer silver colloid is added, the polypropylene has a lasting antimicrobial property; modification is conducted on the multi-walled carbon nanotube load Ti-Zr catalyst, the activity of the catalyst is improved, polarity differences are reduced, and the binding force between multi-walled carbon nanotubes and macromolecules is increased.
Description
Technical field
The present invention relates to polypropylene production technical field, particularly relate to a kind of wood powder 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 wood powder and multi-walled carbon nano-tubes Reinforced Polypropylene resin, this resin has the feature of shock-resistance and good flame resistance, also has lasting anti-microbial property.
Technical scheme of the present invention is as follows:
A kind of wood powder 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 110-130, triethyl aluminum 7-9, dimethoxydiphenylsilane 5.4-6.2, nano silver colloidal sol 1-1.5, cerium dioxide 0.1-0.3, MoO30.2-0.3, organobentonite 4-5, maleic anhydride 0.6-0.9, wood powder 4-5, normal heptane 50-60, hydrogen are appropriate, ammonium hexafluorosilicate 0.1-0.2,1-octene 9-12, water 8-12.
Described wood powder 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 wood powder and multi-walled carbon nano-tubes Reinforced Polypropylene resin, is characterized in that:
(1) by nano silver colloidal sol, cerium dioxide, MoO3, wood powder mixing, grinding 40-60 minute, obtains modified wood powder; Ammonium hexafluorosilicate, maleic anhydride are added to the water, then add carbon multi-wall nano tube loaded Ti-Zr catalyzer, be heated to 60-70 DEG C, stirring reaction 20-30 minute, dry, then mix with modified wood powder, 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-octene 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 carries out modification by using wood powder and organobentonite, enhancing polyacrylic shock-resistance and flame retardant resistance, by adding nano silver colloidal sol, making polypropylene have lasting anti-microbial property; By carrying out modification to carbon multi-wall nano tube loaded Ti-Zr catalyzer, improve the activity of catalyzer, reducing polarity difference, add the bonding force between multi-walled carbon nano-tubes and polymer.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; This polypropylene is applicable to make auto parts and daily necessities.
Embodiment
A kind of wood powder and multi-walled carbon nano-tubes Reinforced Polypropylene resin, be made up of the raw material of following weight part (kilogram): propylene liquid 370, carbon multi-wall nano tube loaded Ti-Zr catalyzer 3, liquid ethylene 120, triethyl aluminum 8, dimethoxydiphenylsilane 5.9, nano silver colloidal sol 1.3, cerium dioxide 0.2, MoO30.2, organobentonite 4.5, maleic anhydride 0.8, wood powder 4.5, normal heptane 55, hydrogen are appropriate, ammonium hexafluorosilicate 0.1,1-octene 10, water 10.
Described wood powder 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 wood powder and multi-walled carbon nano-tubes Reinforced Polypropylene resin, is characterized in that:
(1) by nano silver colloidal sol, cerium dioxide, MoO3, wood powder mixing, grind 50 minutes, obtain modified wood powder; Ammonium hexafluorosilicate, maleic anhydride are added to the water, then add carbon multi-wall nano tube loaded Ti-Zr catalyzer, be heated to 65 DEG C, stirring reaction 25 minutes, dry, then mix with modified wood powder, 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-octene 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 60 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 800%, and under normal temperature, notched Izod impact strength reaches 38.5kJ/ ㎡, and modulus in flexure is 660Mpa.
Claims (3)
1. wood powder 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 110-130, triethyl aluminum 7-9, dimethoxydiphenylsilane 5.4-6.2, nano silver colloidal sol 1-1.5, cerium dioxide 0.1-0.3, MoO30.2-0.3, organobentonite 4-5, maleic anhydride 0.6-0.9, wood powder 4-5, normal heptane 50-60, hydrogen are appropriate, ammonium hexafluorosilicate 0.1-0.2,1-octene 9-12, water 8-12.
2. wood powder 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 wood powder according to claim 1 and 2 and multi-walled carbon nano-tubes Reinforced Polypropylene resin, is characterized in that:
(1) by nano silver colloidal sol, cerium dioxide, MoO3, wood powder mixing, grinding 40-60 minute, obtains modified wood powder; Ammonium hexafluorosilicate, maleic anhydride are added to the water, then add carbon multi-wall nano tube loaded Ti-Zr catalyzer, be heated to 60-70 DEG C, stirring reaction 20-30 minute, dry, then mix with modified wood powder, 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, at 50-80 DEG C, slurry polymerization 7-9 hour is carried out under 2-3MPa condition, add the liquid ethylene of 1/5 and the 1-octene of 1/3 again, 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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