CN109054365B - Preparation method of solid-phase polymerization graphene nylon heat conduction material - Google Patents
Preparation method of solid-phase polymerization graphene nylon heat conduction material Download PDFInfo
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Abstract
A preparation method of a solid-phase polymerization graphene nylon heat conduction material belongs to the field of graphene polymer nano composite materials, and comprises the following steps: (1) Carrying out surface treatment on the graphene slurry by using a coupling agent, and drying to constant weight; (2) drying the nylon by using circulating heating nitrogen; (3) And adding the graphene and the nylon subjected to surface treatment into a solid-phase polymerization device, controlling the heating temperature to be 160-300 ℃, controlling the stirring speed to be 2000-6000rpm, and performing solid-phase polymerization for 10-24 hours in a gradual heating mode to obtain the heat-conducting graphene nylon material. The graphene is grafted to a nylon molecular chain in the process of nylon tackifying polymerization, and the graphene with large specific surface area can be used as a central link of a nylon crystal region and an amorphous region, so that the interface thermal resistance of heat conduction is reduced, the heat conduction capability of the material is improved, the mechanical performance of the material is also improved, the graphene can be applied to parts with certain heat conduction or heat dissipation functions, and the application range of the nylon material is expanded.
Description
Technical Field
The invention discloses a preparation method of a solid-phase polymerization graphene nylon heat conduction material, belonging to the field of graphene polymer nano composite materials.
Background
The graphene is formed from a single layer sp 2 A honeycomb hexagonal plane two-dimensional crystal formed by arranging hybridized carbon atoms, and sp is arranged on the two-dimensional plane 2 The hybridized carbon atoms are connected with three adjacent carbon atoms through strong sigma bonds, the rest P electron orbitals are perpendicular to the plane of the graphene and form large pi bonds with surrounding atoms, so that the graphene has good electric and thermal conductivity and mechanical properties, and the room-temperature thermal conductivity of the graphene is 4.84 multiplied by 10 3 -5.3×10 3 W/(m.k), graphene is the highest thermal conductivity material of several allotropes of carbon.
The nylon used as engineering plastic has the advantages of high mechanical strength, low friction coefficient, self-lubricity, shock absorption, good noise reduction, excellent barrier property, heat resistance, wear resistance, good chemical resistance and the like, and can be widely applied to the fields of the automobile industry, the electronic and electrical communication field, the film packaging field, the military and aerospace industry, the rail transit industry and the like; when the heat conduction and heat dissipation function is involved, the common nylon material cannot meet the requirements, the heat conduction filler needs to be added, the material with the best heat conduction performance is graphene at present, special process conditions are needed when the graphene is added into the nylon material, the graphene is uniformly dispersed in the nylon through a simple melt blending adding mode, and therefore the heat conduction effect of the graphene nylon material is influenced.
The heat conduction carrier is phonon, the heat conductivity coefficient of the polymer is orderly related to the crystallization of the polymer, the semi-crystallization characteristic of the polymer in a nylon resin matrix determines that the heat transfer effect of a crystal area of the polymer is higher than that of an amorphous area, and the interface thermal resistance exists between the crystal area and the amorphous area of the nylon, so that the improvement of the heat conductivity coefficient of the nylon cannot be directly influenced finally. Because the oxygen-containing functional group on the graphene can react with the terminal amino group and the terminal carboxyl group on the nylon molecular chain, the graphene is grafted to the nylon molecular chain, and the graphene with large specific surface area spans between the nylon crystal region and the amorphous region. The graphene is uniformly dispersed in the nylon matrix, can become a central link of a crystal region and an amorphous region in the nylon composite material, and reduces the interface thermal resistance during heat conduction. The graphene sheets are mutually overlapped to form a heat conduction network chain, so that the heat conductivity coefficient of the graphene nylon composite material is improved.
Disclosure of Invention
The invention provides a preparation method of a solid-phase polymerization graphene nylon heat conduction material, which is characterized in that graphene is dispersed into nylon with low viscosity by a solid-phase polymerization method, and the graphene is grafted to terminal amino or terminal carboxyl of a molecular chain at a part of a nylon amorphous area by heating the nylon to a temperature range above the glass transition temperature and below the melting point of the nylon, so that the strength and the heat conductivity of the nylon material grafted with the graphene are improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a solid-phase polymerization graphene nylon heat conduction material comprises the following steps:
(1) Adding a coupling agent into the graphene slurry, carrying out surface dispersion treatment on the graphene in a high-speed shearing emulsifying machine, wherein the shearing speed is 2000-12000r/min, the time is 1-2h, and then carrying out vacuum drying to constant weight, wherein the drying temperature is 80-100 ℃; the addition amount of the coupling agent is 0.5-2wt% of the solid content of the graphene.
(2) Adding nylon into a drying device, introducing nitrogen into the upper end and the lower end of the drying device to respectively dry the nylon, wherein the nitrogen is circularly introduced, the temperature of the nitrogen is controlled at 120-200 ℃, and the drying time is 6-12h.
(3) After drying, adding graphene and nylon into a solid-phase polymerization device, introducing circulating nitrogen for solid-phase polymerization, and performing solid-phase polymerization for 10-24h by adopting a gradual heating mode to obtain a high-viscosity graphene nylon material, wherein the polymerization temperature is controlled within the range of 160-300 ℃, and the polymerization stirring speed is controlled as follows: 2000-6000rpm.
(4) And cooling the polymerized graphene nylon to obtain the heat-conducting graphene nylon material.
The coupling agent is at least one of silane coupling agent and titanate coupling agent, wherein the silane coupling agent comprises silane coupling agents such as gamma (2, 3-epoxypropoxy) propyl trimethoxy silane, gamma-aminopropyl triethoxy silane, N- (beta-aminoethyl) -gamma-aminopropyl trimethyl (ethoxy) silane, gamma- (methacryloyloxy) propyl trimethoxy silane, gamma-diethylenetriamine propylene triethoxy silane and the like; the titanate coupling agent comprises titanate coupling agents such as isopropyldioleacyloxy (dioctylphosphatoxy) titanate, isopropyltri (dioctylphosphatoxy) titanate, triisostearoyltitanate, bis (dioctyloxypyrophosphato) ethylene titanate, tetraisopropyldi (dioctylphosphatoxy) titanate and the like.
The nylon resin is at least one of nylon 6, nylon 66, nylon 46, nylon 610, nylon 612, nylon 11, nylon 12, nylon 1010, nylon 1212, nylon 6T, nylon 9T and nylon 10T with low viscosity.
The graphene slurry is one or a mixture of more of graphene slurry, biomass graphene slurry and slurry of graphene derivatives, the graphene sheet diameter is more than or equal to 5.0 mu m, the thickness is less than or equal to 3.0nm, and the content of oxygen-containing functional groups on the graphene is 10-20%.
The invention is characterized in that: graphene is uniformly dispersed into nylon by a solid-phase polymerization method, in the solid-phase polymerization process, oxygen-containing functional groups on the graphene react with amino groups or carboxyl groups at the ends of molecular chains at the amorphous regions of the nylon, the graphene is grafted onto the molecular chains of the nylon, the graphene with a large specific surface area spans between the crystalline regions and the amorphous regions of the nylon, and can be used as central links of the crystalline regions and the amorphous regions of the nylon, so that the interface thermal resistance during heat conduction is reduced, the heat conductivity of the material is improved, and the mechanical property of the material is also improved.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
Example 1
The preparation method of the solid-phase polymerization graphene nylon heat conduction material comprises the following steps:
(1) Adding a gamma-diethylenetriamine propylene triethoxysilane coupling agent into graphene slurry, carrying out surface dispersion treatment on graphene in a high-speed shearing emulsifying machine, wherein the shearing speed is 8000r/min, the time is 1.5h, and then carrying out vacuum drying to constant weight, and the drying temperature is 90 ℃; the addition amount of the coupling agent is 0.5wt% of the solid content of the graphene.
(2) Adding nylon 6 into a drying device, introducing nitrogen into the upper end and the lower end of the drying device, drying the nylon 6 by adopting circulating nitrogen, controlling the temperature of the nitrogen at 130 ℃, and drying for 10 hours.
(3) And after drying, adding the graphene with the sheet diameter of 8 mu m and the content of 0.3 percent and the nylon 6 with the viscosity of 2.0 and the content of 99.7 percent into a solid-phase polymerization device, introducing circulating nitrogen for solid-phase polymerization, and performing solid-phase polymerization for 18 hours in a gradual temperature rise mode to obtain the high-viscosity graphene nylon material, wherein the polymerization temperature is controlled within the range of 160-180 ℃, and the stirring speed is 5000rpm.
(4) And cooling the polymerized graphene nylon to obtain the heat-conducting graphene nylon 6.
And (3) testing results: the thermal conductivity is 1.42W/(m.K)
Example 2
The embodiment of the invention provides a preparation method of a solid-phase polymerization graphene nylon heat conduction material, which comprises the following steps:
(1) Adding a gamma-diethylenetriamine propylene triethoxysilane coupling agent into graphene slurry, carrying out surface dispersion treatment on graphene in a high-speed shearing emulsifying machine, wherein the shearing speed is 8000r/min, the time is 1.5h, and then carrying out vacuum drying to constant weight, and the drying temperature is 90 ℃; the addition amount of the coupling agent is 0.5wt% of the solid content of the graphene.
(2) Adding nylon 6 into a drying device, introducing nitrogen into the upper end and the lower end of the drying device, and drying the nylon 6 by adopting circulating nitrogen, wherein the temperature of the nitrogen is controlled at 130 ℃ and the drying is carried out for 10 hours.
(3) And after drying, adding the graphene with the sheet diameter of 20 mu m and the content of 0.3 percent, the nylon 6 with the viscosity of 2.0 and the content of 99.7 percent into a solid-phase polymerization device, introducing circulating nitrogen for solid-phase polymerization, and performing solid-phase polymerization for 18h by adopting a gradual heating mode to obtain the high-viscosity graphene nylon 6, wherein the polymerization temperature is controlled within the range of 160-180 ℃, and the stirring speed is 5000rpm.
(4) And cooling the polymerized graphene nylon to obtain the heat-conducting graphene nylon 6.
And (3) testing results: the thermal conductivity is 1.65W/(m.K)
Example 3
The embodiment of the invention provides a preparation method of a solid-phase polymerization graphene nylon heat conduction material, which comprises the following steps:
(1) Adding a gamma-aminopropyltriethoxysilane coupling agent into graphene slurry, carrying out surface dispersion treatment on graphene in a high-speed shearing emulsifying machine, wherein the shearing speed is 8000r/min, the time is 2h, and then carrying out vacuum drying to constant weight, wherein the drying temperature is 90 ℃; the addition amount of the coupling agent is 0.5wt% of the solid content of the graphene.
(2) Adding nylon 6 into a drying device, introducing nitrogen into the upper end and the lower end of the drying device, and drying the nylon 6 by adopting circulating nitrogen, wherein the temperature of the nitrogen is controlled at 130 ℃ and the drying is carried out for 10 hours.
(3) And after drying, adding nylon 6 with the sheet diameter of 20 mu m, the content of 0.5 percent of graphene and the viscosity of 2.0 and the content of 99.5 percent into a solid-phase polymerization device, introducing circulating nitrogen for solid-phase polymerization, and performing solid-phase polymerization for 20 hours in a gradual temperature rise mode to obtain the high-viscosity graphene nylon 6, wherein the polymerization temperature is controlled within the range of 160-180 ℃, and the stirring speed is 5000rpm.
(4) And cooling the polymerized graphene nylon to obtain the heat-conducting graphene nylon 6.
And (3) testing results: the thermal conductivity is 2.25W/(m.K)
Example 4
The preparation method of the solid-phase polymerization graphene nylon heat conduction material comprises the following steps:
(1) Adding a gamma-aminopropyltriethoxysilane coupling agent into graphene slurry, carrying out surface dispersion treatment on graphene in a high-speed shearing emulsifying machine, wherein the shearing speed is 8000r/min, the time is 2h, and then carrying out vacuum drying to constant weight, wherein the drying temperature is 90 ℃; the addition amount of the coupling agent is 0.5wt% of the solid content of the graphene.
(2) Adding nylon 66 into a drying device, introducing nitrogen into the upper end and the lower end of the drying device, and drying the nylon 66 by adopting circulating nitrogen, wherein the temperature of the nitrogen is controlled at 140 ℃ and the drying is carried out for 10 hours.
(3) After drying, adding nylon 66 with the sheet diameter of 20 mu m, the content of 0.5 percent of graphene, the viscosity of 2.0 and the content of 99.5 percent into a solid-phase polymerization device, introducing circulating nitrogen for solid-phase polymerization, and performing solid-phase polymerization for 20 hours in a gradual temperature rise mode to obtain the high-viscosity graphene nylon 66, wherein the polymerization temperature is controlled within the range of 180-200 ℃, and the stirring speed is 5000rpm.
(4) And cooling the polymerized graphene nylon to obtain the heat-conducting graphene nylon 66.
And (3) testing results: the thermal conductivity is 2.32W/(m.K)
Example 5
The embodiment of the invention provides a preparation method of a solid-phase polymerization graphene nylon heat conduction material, which comprises the following steps:
(1) Adding a gamma-aminopropyltriethoxysilane coupling agent into graphene slurry, carrying out surface dispersion treatment on graphene in a high-speed shearing emulsifying machine, wherein the shearing speed is 6000r/min, the time is 1.5h, and then carrying out vacuum drying to constant weight, wherein the drying temperature is 90 ℃; the addition amount of the coupling agent is 0.5wt% of the solid content of the graphene.
(2) Adding nylon 6 into a drying device, introducing nitrogen into the upper end and the lower end of the drying device, and drying the nylon 6 by adopting circulating nitrogen, wherein the temperature of the nitrogen is controlled at 130 ℃ and the drying time is 10 hours.
(3) Adding nylon 6 with the sheet diameter of 30 mu m, the content of 0.5 percent of graphene, the viscosity of 2.0 and the content of 99.5 percent into a solid-phase polymerization device, introducing circulating nitrogen for solid-phase polymerization, and performing solid-phase polymerization for 20 hours in a gradual temperature rise mode to obtain the high-viscosity graphene nylon 6, wherein the polymerization temperature is controlled within the range of 160-180 ℃, and the stirring speed is 5000rpm.
(4) And cooling the graphene nylon after polymerization is finished to obtain the heat-conducting graphene nylon 6.
And (3) testing results: the thermal conductivity is 2.46W/(m.K)
The description and applications of the present invention are illustrative, and not intended to limit the scope of the invention to the embodiments described above, therefore, the present invention is not limited by the embodiments, and any technical solutions obtained by equivalent substitution are within the scope of the present invention.
Claims (1)
1. A preparation method of a solid-phase polymerization graphene nylon heat conduction material is characterized by comprising the following steps:
(1) Adding a gamma-aminopropyltriethoxysilane coupling agent into graphene slurry, carrying out surface dispersion treatment on graphene in a high-speed shearing emulsifying machine, wherein the shearing speed is 6000r/min, the time is 1.5h, and then carrying out vacuum drying to constant weight, wherein the drying temperature is 90 ℃; the addition amount of the coupling agent is 0.5wt% of the solid content of the graphene;
(2) Adding nylon 6 into a drying device, introducing nitrogen into the upper end and the lower end of the drying device, and drying the nylon 6 by adopting circulating nitrogen, wherein the temperature of the nitrogen is controlled at 130 ℃, and the drying time is 10 hours;
(3) Adding nylon 6 with the sheet diameter of 30 mu m, the content of 0.5 percent of graphene, the viscosity of 2.0 and the content of 99.5 percent into a solid-phase polymerization device, introducing circulating nitrogen for solid-phase polymerization, and performing solid-phase polymerization for 20 hours by adopting a gradual heating mode to obtain the high-viscosity graphene nylon 6, wherein the polymerization temperature is controlled within the range of 160-180 ℃, and the stirring speed is 5000rpm;
(4) Cooling the graphene nylon after polymerization to obtain heat-conducting graphene nylon 6;
the content of oxygen-containing functional groups of graphene in the graphene slurry is 10-20%.
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| US6693163B2 (en) * | 2002-03-15 | 2004-02-17 | Mitsubishi Gas Chemical Company, Inc. | Solid-phase drying and solid-phase polymerization of polyamide |
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| CN101768353A (en) * | 2009-01-06 | 2010-07-07 | 东丽纤维研究所（中国）有限公司 | Method for increasing molecular weight of polyamide/graphite composite material through solid-phase polymerization |
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