CN109265986A - A kind of high thermal conductivity nylon composite materials - Google Patents
A kind of high thermal conductivity nylon composite materials Download PDFInfo
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- CN109265986A CN109265986A CN201811118945.8A CN201811118945A CN109265986A CN 109265986 A CN109265986 A CN 109265986A CN 201811118945 A CN201811118945 A CN 201811118945A CN 109265986 A CN109265986 A CN 109265986A
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- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
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Abstract
The present invention relates to field of polymer composite material, provide a kind of high thermal conductivity nylon composite materials, and raw material composition includes nylon resin, reinforcing material, heat filling and lubricant, and the nylon resin includes at least a kind of containing graphene PA6 resin.The invention has the advantages that and the utility model has the advantages that 1) solve the problems, such as because graphene bulk density it is small caused by squeeze out processing fugitive dust.2) graphene in containing graphene PA6 resin can be organically combined with typical thermal-conductive fillers, generate unexpected syneryistic effect, overcome typical thermal-conductive material and be difficult to reach the technical bottleneck problem of high thermal conductivity coefficient under the low loading of heat filling.3) present invention need to only introduce a small amount of graphene (0.1%~2%) in typical thermal-conductive fillers filling nylon composite material system, it can assign nylon composite materials excellent heating conduction, compared with directly using graphene powder, it is effectively reduced graphene additive amount, production cost is considerably reduced, it can large-scale industrial production.
Description
Technical field
The present invention relates to field of polymer composite material, and in particular to a kind of high thermal conductivity nylon composite wood of containing graphene
Material.
Background technique
In recent years, with the fast development of great-power electronic, electric product, necessarily will appear more and more due to product
The problems such as fever, causes product efficacy to reduce, reduced service life.Data show that electronic component temperature is every to increase 2 DEG C,
Its reliability decrease 10%；Service life at 50 DEG C only has 1/6 at 25 DEG C.To guarantee that electronic component can be normal in a long time
The heat transfer of generation is in time crucial by work.Conventional thermal conductive material is mostly metal and metal oxide and other non-gold
Belong to material, such as graphite, carbon black, AlN.With the development of science and technology and production, many products propose more Heat Conduction Material
High request, it is desirable to which it is light, chemical corrosion resistance is strong, impact resistance, machine-shaping are easy with more excellent comprehensive performance
Deng.High molecular material has the advantages such as light, good fluidity, good machinability and low cost, gradually replaces tradition and leads
Hot material is used in more and more in electronic device and equipment.However, most of polymer is that the bad of heat is led
Body, extremely low (the < 0.5Wm of thermal coefficient-1·K-1), in order to expand high molecular material in electronic equipment, heat exchanger, the sun
The application of energy energy device, LED and automobile etc., preparing inexpensive, high thermal conductivity polymer material is trend of the times, and
Very practical and promising research topic.
Nylon base heat conducting material rapidly becomes grinding for thermal conductive polymer material due to excellent heat resistance and weatherability
Study carefully object.Being modified using heat filling to nylon is improve nylon and other Polymer Thermal Conductivities current more common
Means.The prior art is retrieved and is found, currently used heat filling has metal powder, metal oxide, metal nitride, charcoal
Black, graphite, carbon nanotube, silicon carbide etc., but itself thermal conductivity of these fillers is not high, can just make only under high additive amount compound
Material obtains higher thermal conductivity, as patent CN106046779A discloses a kind of fire-retardant nylon that the good thermal coefficient of wearability is high
Composite material and preparation method selects silicon carbide micro-powder as heat filling, and heat filling dosage is 35%~40%, material
The thermal coefficient of material is only 0.70~0.86Wm-1·K-1；It is multiple that patent CN102408710A discloses a kind of high thermal conductivity nylon66 fiber
Condensation material and preparation method thereof, heat filling are selected aluminium nitride and aluminum oxide respectively to account for the mixture of 50% weight ratio, are led
Hot amount of filler is 52%, and the thermal coefficient of nylon 66 composite material obtained is 1.28Wm-1·K-1；Patent
CN106675008A discloses a kind of high thermal conductivity nylon 6 composite material and preparation method thereof, selects aluminium oxide, magnesia, oxygen
Change one of zinc, aluminium powder, aluminium nitride, boron nitride or silicon carbide or a variety of mixtures as heat filling, heat filling dosage
Up to 60%, the highest thermal coefficient of material is also only 2.3Wm-1·K-1；Patent CN102757640A discloses a kind of thermally conductive
Nylon composite materials and preparation method thereof, heat filling are the mixture of carbon nanotube, aluminium nitride and silicon carbide, heat filling
Dosage is 60%, and the thermal coefficient of Heat conduction nylon composite material obtained is also only 2.8Wm-1·K-1.By the above-mentioned prior art
It is found that using typical thermal-conductive fillers, even if its loading is very high, but heating conduction is not still high, and high filler loading capacity can be significantly
The mobility for reducing material, considerably increases difficulty of processing；Simultaneously because heat filling is inorganic material, with nylon resin matrix
Poor compatibility, interface cohesion it is very weak, the mechanical properties decrease that will lead to nylon material is obvious.
Graphene is a kind of novel two-dimentional carbon nanomaterial, has very high specific surface area, has excellent mechanicalness
Energy and heating conduction.Theoretical research shows that the room temperature thermal coefficient of single-layer graphene is up to 5300Wm-1·K-1, it is approximately copper
14 times, 3.5 times of graphite, are the materials with highest thermal coefficient being currently known, and are a kind of ideal heat fillings.
It is directly mixed with to obtain with macromolecule resin currently, graphene heat-conducting plastic generallys use graphene.But the sp of graphene2It is miscellaneous
The flat sheet structure of change determines that graphene is easy to assemble, and is added into polymer resin matrix and easily occurs reuniting now
As, cause its original excellent properties to lose, thus to reach certain thermal conductivity, it is necessary to carry out high-content filling.Such as China
Patent CN105368043A discloses a kind of graphene heat-conducting plastic and preparation method thereof, using graphene, macromolecule resin and
Other function ingredients and auxiliary agent directly mix, and prepare heat-conducting plastic through double screw extruder extrusion, when graphene dosage is 5wt%
When, the thermal conductivity of material prepared is only 3.3Wm-1·K-1, when graphene dosage is 9wt%, the thermal conductivity of material prepared
Rate is also only 3.5Wm-1·K-1.Since the price is very expensive (1~100 yuan/gram) for graphene, the high thermally conductive modeling of filled graphite alkene
Expect that price is also very high, it is made to be difficult to promote and apply on a large scale.In addition, the bulk density of graphene is small, it is directly added to gather
When closing object matrix, it is easy to happen dust raising phenomenon, so that processing deterioration, further constrains graphene in heat-conductive composite material circle
Industrialize large-scale application.
Currently, have and be used in combination by introducing typical thermal-conductive fillers and graphene in formula system, or to graphene into
Row pre-treatment improves its dispersibility in resin matrix, to realize low cost, high thermal conductivity effect, but result people not to the utmost
Graphite is added merely if patent CN106633827A discloses a kind of graphene nylon composite materials and preparation method thereof in meaning
Alkene is as heat filling, and loading is up to 25%, and the composite material vertical thermal conductivity of preparation is 7.8Wm-1·K-1, use
15% graphene and 10% high thermal conductivity graphite as heat filling, the composite material vertical thermal conductivity of preparation is directly down to
4.9W·m-1·K-1, when the dosage of graphene is reduced to 5% (high thermal conductivity graphite levels are 25%), the composite material of preparation hangs down
Straight thermal coefficient is only 1.2Wm-1·K-1.Patent CN107474354A discloses a kind of high dispersive graphene heat-conducting plastic system
Preparation Method and products thereof and application, by the way that graphene pretreatment at high concentration slurries, to be then added in matrix and be processed,
To reach the dispersibility for improving graphene in heat-conducting plastic, the higher mechanical strength of the plastics and preferable heating conduction are assigned
Purpose.However mixed with other powder components of high concentration slurry form and recipe ingredient, mixing resistance is increased to heavens
Power, there are other components to disperse non-uniform risk, and still lower using heat-conducting plastic heating conduction made from this method, stone
Black alkene dosage also added 10% conduction powder auxiliary agent (aluminium oxide, silicon carbide), thermal coefficient is also only 4Wm up to 30%-1·K-1。
Summary of the invention
The technical problem to be solved by the present invention is to overcome drawbacks described above of the existing technology, provide one kind and be suitable for
The high thermal conductivity nylon composite materials of the low cost of industrialized production, containing graphene, it is compound in typical thermal-conductive fillers filled nylon
Minute quantity graphene is introduced in the form of resin matrix in material system, it can be achieved that assigning under the lower loading of typical thermal-conductive fillers multiple
The excellent heating conduction of condensation material pushes away to not only ensure that high thermal conductivity but also maintain the basic mechanical performance of composite material
The extensive use of heat-conducting plastic is moved.
The technical solution adopted by the present invention to solve the technical problems is as follows:
A kind of high thermal conductivity nylon composite materials, raw material composition include nylon resin, reinforcing material, lubricant and thermally conductive fill out
Material, the nylon resin include at least a kind of containing graphene PA6 resin.
Wherein, the containing graphene PA6 resin is made using situ aggregation method, specific steps are as follows:
(1) it is small that the graphene powder of 5 parts by weight is placed in progress ultrasonic disperse 0.5~1 in the dehydrated alcohol of 20 parts by weight
When, the coating material of 5 parts by weight is then added, continues ultrasound and is dried after 0.5~1 hour, obtain surface modification graphite
Alkene powder；
(2) 100 weight are added in the surface modification graphene powder of 0.01~5 parts by weight and 1~3 parts by weight of deionized water
In the caprolactam melt of part, high speed (350~450rpm) stirs and evenly mixs to form dispersion liquid at 80 DEG C；
(3) under N2 protection, the dispersion liquid that step (2) is obtained is added in batch condensation polymerization reactor, is warming up to 240 DEG C~270
DEG C, it is reacted 2~4 hours at 0.5~1MPa；It reacts 4~6 hours under vacuum again, obtains polymer melt, it finally will polymerization
The water cooled granulation of object melt obtains the containing graphene PA6 resin that graphene content is 0.01wt%~5wt%；
Wherein, the graphene powder select one of graphene microchip, graphene oxide, redox graphene or
It is several；
The coating material selects one of silane coupling agent, titanate coupling agent or aluminate coupling agent or several
Kind.
The containing graphene PA6 resin prepared using this method, the low caprolactam monomer of small volume, viscosity is in molten
It can be achieved to mix with the uniform of graphene under state, the uniformity and physical properties of system be effectively ensured, and can be simultaneous simultaneously
The synthesis for caring for the evenly dispersed and polymer of graphene, ensure that the stabilization of polyamide basic performance.
Preferably, the weight percent of containing graphene PA6 resin is 5%~30% in the nylon resin.
Preferably, the nylon resin further include PA6, PA66, PA46, PA11, PA12, PA610, PA612,
PA1010、PPA、PA1012、PA1212、PA4T、PA6T、PA9T、PA10T、PA6I、PAMXD6、PA6I、PA66/6、PA6/66、
One or more of PA6T/6I, PA6T/66.
Further, preferably, the high thermal conductivity nylon composite materials, by weight, raw material components include:
The inorganic heat filling selects metal powder, metal oxide, metal nitride, conductive black, graphite, graphite
One or more of alkene, carbon nanotube.
The present invention introduces a small amount of graphite in typical thermal-conductive fillers filling nylon composite material system in the form of resin matrix
Alkene not only reduces the application cost of graphene in heat-conductive composite material system as synergistic thermal conducting agent, but also has evaded direct use
Agglomeration traits caused by graphene and processing fugitive dust problem, more surprisingly can be under the lower loading of typical thermal-conductive fillers
Obtain excellent heating conduction.
It is known that forming effective thermal conducting path in matrix is to improve the effective way of thermal coefficient, filler grain is used
Amount, particle size and its distribution situation in the base influence the formation of thermal conducting path.And graphene is nano-lamellar structure,
Partial size is very small, can be filled in the irregular gap formed between typical thermal-conductive fillers well, play the role of gantry, connection,
Promote to interconnect between each component to run through, to form more stable thermal conducting path, graphene thermal coefficient is very in addition
Height, reach afterwards graphene dosage it is few when, the effect of nylon composite materials heating conduction can be obviously improved.
The reinforcing material selects glass fibre, carbon fiber, aromatic polyamide fibre, wollastonite fibre, ceramic fibre, metatitanic acid
Potassium whisker, alkali magnesium sulfate crystal whisker, silicon carbide whisker or silica, alumina silicate, silica, titanium dioxide, talcum, silicon ash
At least one of stone, diatomite, clay, kaolin, globular glass, mica, gypsum, iron oxide, magnesia, zinc oxide.
The lubricant selects stearate, carboxylic acid series lubricant agent, polyester series lubricant agent, in fatty acid and ester lubricant
It is at least one or several.
Further, the raw material components of the high thermal conductivity nylon composite materials further include 0.5 part~2 parts of other components,
The other components are coupling agent, toughener, impact modifying agent, release agent, heat stabilizer, light stabilizer, antistatic agent, ultraviolet
One or more of absorbent, colorant and antioxidant.
Another object of the present invention is to provide the mechanograph using the preparation of above-mentioned high thermal conductivity nylon composite materials.
Third object of the present invention is to provide utilize above-mentioned high thermal conductivity nylon composite materials or product to shape for manufacturing
The purposes of body.
The invention has the advantages that and the utility model has the advantages that
1) the containing graphene PA6 resin using situ aggregation method preparation is selected, substitution graphene is used for heat-conductive composite material
The habitual practice-of system directly add graphene powder, are filled in heat-conductive composite material formula system, have evaded because of graphite
Processing fugitive dust problem is squeezed out caused by alkene bulk density is small.
2) graphene in containing graphene PA6 resin can be organically combined with typical thermal-conductive fillers, generate unexpected association
Same synergy, the heating conduction compared to the nylon composite materials for the typical thermal-conductive fillers preparation for only adding same amount are significant
Promote that (thermal coefficient is from 2.8Wm-1·K-1It is promoted to 5.1Wm-1·K-1), typical thermal-conductive material is overcome in heat filling
It is difficult to reach the technical bottleneck problem of high thermal conductivity coefficient under low loading.
3) present invention only need to introduce a small amount of graphene in typical thermal-conductive fillers filling nylon composite material system
(0.1%~2%) can assign nylon composite materials excellent heating conduction, compared with directly using graphene powder, effectively
Reduce graphene additive amount, considerably reduce production cost, can large-scale industrial production.
Specific embodiment
Following part is that the present invention will be further described for specific embodiment, but following implementation is only to this hair
Bright is explained further, and does not represent the scope of the present invention and is only limitted to this, all equivalence replacements done with thinking of the invention,
In protection scope of the present invention.
Raw material used in embodiment and comparative example experiment is following raw material, but is not limited to following raw material:
Containing graphene PA6 resin: selecting graphene content is the containing graphene PA6 of 3wt% prepared with the following method
Resin:
(1) by 250g graphene powder in the absolute alcohol of 1kg ultrasonic disperse 1 hour, be added 250g surface treating agent
KH-550, graphene powder after drying is handled after continuation is 1 hour ultrasonic；
(2) graphene powder and 100g deionized water are added in the caprolactam melt of 5kg after handling 150g, at 80 DEG C
Lower high speed (400rpm) stirs and evenly mixs to form dispersion liquid；
(3) under nitrogen protection, batch condensation polymerization reactor is added in above-mentioned dispersion liquid, and is warming up to 240-270 DEG C, in 0.5-
It is reacted 2-4 hours under 1MPa；Then it reacts 4-6 hours under vacuum, obtains polymer melt；Finally by polymer melt through water
Cold granulation obtains the thermally conductive masterbatch of graphene.
PA66 resin: EP158, Huafeng Group Corp., Ltd.
PA6 resin: M2400, Meida Nylon Co., Ltd., Xinhui, Guangdong
PPA resin: A-1000, Su Wei company
Glass fibre: ESC10-4.5-568H, Jushi Group Co., Ltd.
Carbon fiber: TYM company of South Korea
Coupling agent: KH550, Nanjing Neng De Chemical Co., Ltd.
Coupling agent: KH570, Nanjing Neng De Chemical Co., Ltd.
Heat filling: 1. conductive black, YM300, Tianjin You Meng Chemical Industry Science Co., Ltd
2. crystalline flake graphite, Wei Jie graphite Co., Ltd of Qingdao City
3. carbon nanotube, the Asia-Pacific Ai Lisheng Co., Ltd
4. aluminium powder, Dongguan Dong Chao new material Science and Technology Ltd.
5. graphene powder, CPG-1606, the poly- carbon composite Co., Ltd in Zhuhai
Lubricant: 1. PE wax: BASF AG
2. calcium stearate: Hangzhou Oil and Fat Chemical Co., Ltd.
Embodiment 1-5 and comparative example 1-3
Material weighing is carried out by the material proportion (parts by weight) of table 1, by load weighted in addition to reinforcing material and coupling agent
Other components are added twin-screw extrude after high-speed mixer and mixing is uniform by main spout, reinforcing filler and lubricant
It is added after blending by side spout, is squeezed out, cross water cooling, be granulated and obtain nylon composite materials after drying.
Performance test methods:
(1) tensile strength is tested according to ISO 527-1/-2 standard method；
(2) bending strength is tested according to 178 standard method of ISO；
(3) particle: being molded into the disk of 12.7 × 2mm by thermal coefficient, when testing 25 DEG C using resistance to laser heat conducting instrument of speeding
Thermal coefficient.
The raw material components and performance of each nylon composite wood in table 1 embodiment 1-5 and comparative example 1-3
As seen from Table 1, the present invention is assigned by introducing containing graphene PA6 resin in Heat conduction nylon composite material system
The excellent heating conduction of Heat conduction nylon composite material, and in the lower situation of typical thermal-conductive fillers dosage (embodiment 4, it is thermally conductive
About 15%), thermal coefficient also can reach 2.1W/mK to filer content.
From embodiment 1 and comparative example 1, comparative example 2, it is evident that in the identical situation of other heat filling contents it is (conductive
45 parts of graphite), minimal amount of graphene (0.3wt%) powder (comparative example 2) is directly added in formula system, thermally conductive nylon is multiple
The heating conduction of condensation material does not have to be promoted that (1 thermal coefficient of comparative example is 2.8W/mK, and the thermal coefficient of comparative example 2 is also only substantially
For 2.9W/mK), and the stone of equal volume is introduced in the form of containing graphene PA6 resin substitutes a small amount of PA6 resin (10 parts)
Black alkene (embodiment 1), the heating conduction of Heat conduction nylon composite material have and are obviously improved that (thermal coefficient of embodiment 1 is 5.1W/
MK, the thermal coefficient of comparative example 1 are only 2.8W/mK, and heating conduction promotes nearly 1 times).
Find out from embodiment 3 and comparative example 3, and in the lower situation of typical thermal-conductive fillers dosage (15 parts of electrically conductive graphite, carbon
5 parts of nanotube, heat filling content 19.6%), 5 parts of PPA resin (conversion graphite is substituted only with containing graphene PA6 resin
Alkene accounts for formula system weight percent, and to be only 0.15%) that the heating conduction of composite material also has significantly promoted, thermal coefficient from
0.7W/mK is promoted to 1.7W/mK, further illustrates that addition containing graphene PA6 resin can assign that typical thermal-conductive fillers are low to be filled out
The excellent heating conduction of Heat conduction nylon composite material under filling.
Claims (11)
1. a kind of high thermal conductivity nylon composite materials, raw material composition includes nylon resin, reinforcing material, heat filling and lubricant,
It is characterized in that, the nylon resin includes at least a kind of containing graphene PA6 resin.
2. high thermal conductivity nylon composite materials according to claim 1, which is characterized in that the containing graphene PA6 resin is adopted
It is made with situ aggregation method, specific steps are as follows:
(1) graphene powder of 5 parts by weight is placed in the dehydrated alcohol of 20 parts by weight and carries out ultrasonic disperse 0.5~1 hour, so
The coating material of 5 parts by weight is added afterwards, continues ultrasound and is dried after 0.5~1 hour, obtain surface modification Graphene powder
Body；
(2) 100 parts by weight are added in the surface modification graphene powder of 0.01~5 parts by weight and 1~3 parts by weight of deionized water
In caprolactam melt, high speed (350~450rpm) stirs and evenly mixs to form dispersion liquid at 80 DEG C；
(3) in N2Under protection, the dispersion liquid that step (2) is obtained is added in batch condensation polymerization reactor, is warming up to 240 DEG C~270 DEG C,
It is reacted 2~4 hours under 0.5~1MPa；It reacts 4~6 hours under vacuum again, obtains polymer melt, finally melt polymer
The water cooled granulation of body obtains containing graphene PA6 resin；
Wherein, the graphene powder selects one of graphene microchip, graphene oxide, redox graphene or several
Kind；
The coating material selects one or more of silane coupling agent, titanate coupling agent or aluminate coupling agent.
3. high thermal conductivity nylon composite materials according to claim 1, which is characterized in that containing graphene in the nylon resin
The weight percent of PA6 resin is 5%~30%.
4. high thermal conductivity nylon composite materials according to claim 1, which is characterized in that the nylon resin further includes other
Nylon resin, selected from PA6, PA66, PA46, PA11, PA12, PA610, PA612, PA1010, PPA, PA1012, PA1212,
One of PA4T, PA6T, PA9T, PA10T, PA6I, PAMXD6, PA6I, PA66/6, PA6/66, PA6T/6I, PA6T/66 or
It is several.
5. high thermal conductivity nylon composite materials according to claim 1, which is characterized in that the heat filling selects metal
One of powder, metal oxide, metal nitride, boron nitride, silicon carbide, conductive black, graphite, graphene, carbon nanotube
Or it is several.
6. high thermal conductivity nylon composite materials according to claim 1, which is characterized in that the reinforcing material selects glass fibers
Dimension, carbon fiber, aromatic polyamide fibre, wollastonite fibre, ceramic fibre, potassium titanate crystal whisker, alkali magnesium sulfate crystal whisker, silicon carbide whisker
Must or silica, alumina silicate, silica, titanium dioxide, talcum, wollastonite, diatomite, clay, kaolin, globular glass,
One or more of mica, gypsum, iron oxide, magnesia, zinc oxide.
7. high thermal conductivity nylon composite materials according to claim 1, which is characterized in that the lubricant selects stearic acid
Salt, carboxylic acid series lubricant agent, polyester series lubricant agent, at least one of fatty acid and ester lubricant or several.
8. high thermal conductivity nylon composite materials according to claim 1, which is characterized in that by weight, raw material components packet
It includes:
9. high thermal conductivity nylon composite materials according to claim 1, which is characterized in that the raw material components further include 0.5
Part~2 parts of other components, the other components are that coupling agent, toughener, impact modifying agent, release agent, heat stabilizer, light are steady
Determine one or more of agent, antistatic agent, ultraviolet absorber, colorant and antioxidant.
10. product made of any high thermal conductivity nylon composite materials according to claim 1~9.
11. being used to manufacture the use of formed body according to the high thermal conductivity nylon composite materials or product any in the claims
On the way.
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