CN106543710A - A kind of preparation method of PA6 heat-conductive composite materials - Google Patents
A kind of preparation method of PA6 heat-conductive composite materials Download PDFInfo
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- CN106543710A CN106543710A CN201611119927.2A CN201611119927A CN106543710A CN 106543710 A CN106543710 A CN 106543710A CN 201611119927 A CN201611119927 A CN 201611119927A CN 106543710 A CN106543710 A CN 106543710A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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Abstract
A kind of preparation method of PA6 heat-conductive composite materials, belongs to field of material preparation, it is characterised in that comprise the steps：（1）Take aluminium oxide, titanate coupling agent is mixed with isopropanol, pour into be obtained with aluminium oxide in mixer it is alumina powder jointed；（2）Crystalline flake graphite, isopropanol are taken, is stirred in beaker with titanate esters, pour mixing for standby use in mixer into；（3）PA6/PET modified matrix and alumina powder jointed, the mixed at room temperature in high mixer are taken, double screw extruder pelletizing is put into, is dried in baking oven, the material input injection machine after drying is prepared into into sample.By the improvement to traditional handicraft, based on PA6, PET, by improving both compatibilitys, lifting toughness, the excellent modified matrix of processability；Selective oxidation aluminum and crystalline flake graphite powder body prepare heat conduction PA6/PET composites as conduction powder, and composite property prepared by the method for the invention is reliable and stable, is suitable to popularization and application.
Description
Technical field
The invention belongs to field of material preparation, more particularly to a kind of preparation method of PA6 heat-conductive composite materials.
Background technology
PA6 is also known as polyamide 6, industrial to cause ring-opening polymerisation to be obtained by acid or alkali using caprolactam more.Due to its knot
The height regularity of structure, with high crystalline and excellent comprehensive mechanical property, but there is poor dimensional stability, high water absorption
The shortcomings of property.With social development, the application of engineering plastics is increasingly extensive, used as one of important engineering plastics, the application of PA6
Field is also constantly expanded.
With the fast development of plastic industry, high performance, the plastics of multifunction increasingly cause the mesh of Chinese scholars
Light.Heat-conducting plastic development is especially rapid, compares traditional aluminium section bar, and heat-conducting plastic possesses light weight, environmental protection, insulation, easy processing, low
The advantages such as cost.PA6 compares the general-purpose plastics such as PE, PP, good etc. excellent with technological temperature width, excellent in mechanical performance, heat stability
Point, requires higher field in LED lamp etc. to plastics performance, and PA6 is more subject to favoring for scholars and enterprisers.
Heat-conducting plastic possesses the advantages of lightweight, easy to process, design freedom is high；Heat conductive rubber is in thermal interface material
It is widely used, is projected with heat-conducting silicon rubber especially；Phase-change material is a kind of material for possessing energy storage capacity, is applied in computer CPU etc.
Upper extremely wide, its interface state will not change with ambient temperature, reduce system thermal resistance, improve thermal conductivity.
PET has the advantages such as higher heat stability, weatherability, dimensional stability, expands its application in heat conduction field
Tool has very important significance, and especially prepares conducting alloy with PA6 blendings.But PET is higher because of its glass transition temperature, crystallization speed
Degree is slow, and injection mo(u)lding plastic is in fragility, is difficult to apply to large-scale mechanical part.
The content of the invention
Present invention seek to address that the problems referred to above, there is provided a kind of preparation method of PA6 heat-conductive composite materials.
The technical scheme is that：
A kind of preparation method of PA6 heat-conductive composite materials, it is characterised in that comprise the steps：（1）Take aluminium oxide, titanate esters idol
Connection agent, titanate coupling agent and isopropanol are mixed in beaker, after placing half an hour, are dropwise poured in high-speed mixer
Mix at a temperature of 80 DEG C 20 minutes with aluminium oxide, be obtained alumina powder jointed；Reselection silane coupler, using dehydrated alcohol as
Diluent, both ratios are 1: 2, prepare the alumina powder jointed of silane coupled agent content respectively 1%；（2）Take crystalline flake graphite, different
Propanol, isopropanol and titanate coupling agent are mixed in beaker, after placing half an hour, are dropwise poured in high-speed mixer
Mix 20 minutes at a temperature of 80 DEG C with graphite；120 DEG C of dryings 1 hour, it is standby；（3）Take PA6/PET modified matrix and aluminium oxide
Powder body, after mixed at room temperature 5min in high mixer, input twin-screw extrusion machine travel, pelletizing are dried in baking oven, after drying
Material input injection machine be prepared into sample.
The preparation method of PA6 heat-conductive composite materials of the present invention, the alumina particle are 4 μm.
The preparation method of PA6 heat-conductive composite materials of the present invention, the temperature setting of the extruder is 180 DEG C -270
℃。
The preparation method of PA6 heat-conductive composite materials of the present invention, the temperature setting of the injection moulding machine is 270
℃。
The preparation method of PA6 heat-conductive composite materials of the present invention, the oven temperature are 100 DEG C, and drying time is 6
Hour.
The method have technical effect that：
The preparation method of PA6 heat-conductive composite materials of the present invention, by the improvement to traditional handicraft, based on PA6, PET
Body, by improving both compatibilitys, lifting toughness, the excellent modified matrix of processability；Selective oxidation aluminum and crystalline graphite powder
Body prepares heat conduction PA6/PET composites as conduction powder, and composite property prepared by the method for the invention stably may be used
Lean on, be suitable to popularization and application.
Specific embodiment
Embodiment
A kind of preparation method of PA6 heat-conductive composite materials, it is characterised in that comprise the steps：（1）Take aluminium oxide, metatitanic acid
Ester coupling agent, titanate coupling agent and isopropanol are mixed in beaker, after placing half an hour, dropwise pour mixed at high speed into
Mix at a temperature of 80 DEG C 20 minutes with aluminium oxide in machine, be obtained alumina powder jointed；Reselection silane coupler, with dehydrated alcohol
Used as diluent, both ratios are 1: 2, prepare the alumina powder jointed of silane coupled agent content respectively 1%；（2）Take scale stone
Ink, isopropanol, isopropanol and titanate coupling agent are mixed in beaker, after placing half an hour, are dropwise poured into mixed at a high speed
Mix 20 minutes at a temperature of 80 DEG C with graphite in conjunction machine；120 DEG C of dryings 1 hour, it is standby；（3）Take PA6/PET modified matrix with
Alumina powder jointed, after mixed at room temperature 5min in high mixer, input twin-screw extrusion machine travel, pelletizing are dried in baking oven, will
Material input injection machine after drying is prepared into sample.
The preparation method of PA6 heat-conductive composite materials of the present invention, the alumina particle are 4 μm.
The preparation method of PA6 heat-conductive composite materials of the present invention, the temperature setting of the extruder is 180 DEG C -270
℃。
The preparation method of PA6 heat-conductive composite materials of the present invention, the temperature setting of the injection moulding machine is 270
℃。
The preparation method of PA6 heat-conductive composite materials of the present invention, the oven temperature are 100 DEG C, and drying time is 6
Hour.
Jing after coupling agent treatment, powder body activation grade is significantly increased, and titanate coupling agent treatment effect is best.Due to untreated
Filler surface hydrophilic oleophobic and easily reunite, which is poor with the compatibility of organic polymer, and it is bad to easily cause interfacial adhesion, so as to
Material overall mechanical properties are caused to decline.In titanate coupling agent, RO- groups are hydrolyzable lower alkyloxies, can with it is inorganic
Thing surface hydroxyl reacts, so as to reach the purpose of chemical coupling；OX- can be carboxyl, alkoxyl, sulfonic group, phosphorio etc., this
A little groups are critically important, determine the specific function that titanate esters have, and pyrophosphoryl epoxide has the performance for strengthening bonding.By upper conclusion
Know, alumina powder jointed activation grade highest handled by titanate coupling agent.
Coupling agent substantially can play a part of to peel off reunites, and reduces the hydroxy radical content of powder surface, makes reunion powder body depolymerization,
Powder surface lipophile, so as to disperse in dehydrated alcohol camber.Its modification theory is：Using charge-transfer complexation body, pass through
Organo-functional group carries out chemisorbed or chemical reaction to particle surface, is that surface modifier is covered in particle surface.
In titanate coupling agent, OX- groups can occur ester exchange reaction with the polymer with carboxyl.Because matrix used be
The blend of polyester-polyamide, contains substantial amounts of end carboxyl in blend, during melting extrusion, coupling agent is anti-with matrix resin
Should, the alumina powder jointed of connection can be used as the part of grafting, and obvious to the reinforcement effect of segment, the mechanical property of composite is carried
It is high.
Jing after coupling agent treatment, there is not the phenomenon condensed, this table in alumina powder jointed obvious high degree of dispersion in the base
Bright coupling agent significantly improves the property of powder surface, allows powder body preferably to scatter in the base, so as to composite wood
The mechanical property of material, thermal conductivity have improvement.
Alumina powder jointed Jing after coupling agent treatment, heat conductivity substantially increases, and serves in the composite preferably
Conductive force.Matrix/filler interface is the approach that heat transfer must be passed through, therefore composite system thermal conductivity directly takes
Certainly in interface binding power.After coupling agent treatment, the degree of alumina powder jointed surface easily moistening is high, the water ratio limit of matrix and filler
Degree is high, and in collective, dispersion is higher, so thermal conductivity increase.Also due to the chemistry between titanate coupling agent and polyester is anti-
Interfacial adhesion should be enhanced, thermal conductivity is higher than the effect that silane coupler and aluminate coupling agent are processed naturally.
Coupling agent is obviously improved effect to composite materials property；And to alumina powder jointed activation grade, dispersion
Coefficient all improves a lot, can remote-effects heat conductivity.Titanate coupling agent has special reactive group,
It is the most notable to the performance impact of the composite based on PA6/PET.Comprehensive analysis, experiment select titanate coupling agent conduct
Surface conditioning agent.
Powder filled matrix has optimum dispersion degree, and when filling fraction is optimum, powder body high degree of dispersion in the base, melting are squeezed
The stretching that can realize composite and bending strength are acted on during going out to the reinforcement effect of the macromolecule end of the chain and stress concentration
Lifted；And the powder body hole that dispersed filler is formed in the base, then it is one of approach of high polymer dispersion external energy, so as to reality
The rising of existing impact strength.The rigidity of the increase matrix of powder content then can be lifted accordingly, directly show as bending moduluses
Increase, there is brittle failure phenomenon in crooked test.
The stretching of the less composite of particle diameter and bending strength are bigger, and impact property is best when being then 10 μm.This be because
For, particle diameter is less bigger with the contact surface of matrix, and cohesive force is also bigger, also stronger to the fixation of the macromolecule end of the chain,
Between the end of the chain, sliding is also just increasingly difficult, so tensile strength is bigger.When particle diameter hour, the hole in matrix is also less, for
Dispersion external force effect is unconspicuous, and powder reuniting is more readily formed, so impact property can decline on the contrary.Comprehensive analysis,
When particle diameter is 10 μm, the impact strength of composite is strengthened the most substantially, and stretch bending intensity, can keep very high
Intensity.
In the case that loading is certain, between big particle diameter filling powder body, effective contact area is little, and the heat conduction network for being constituted is few,
Path thermal resistance is big, is unfavorable for the conduction of heat；In addition, be not that the less lifting to thermal conductivity of particle diameter is bigger, particle diameter Amylum Tritici Testa
Between body, contact area is big, is easier to form thermal conducting path, and heat conduction network is more, but the little powder body of particle diameter is more easy to roll into a ball in the base
Poly-, reunion is unfavorable for the formation of thermal conducting path, and thermal resistance causes greatly the decline of thermal conductivity.10 μm of alumina powder jointed fillings it is compound
Material thermal conductivity is best.
The particle diameter of aluminium oxide conduction powder is had a significant impact to the mechanical property and thermal conductivity of composite, particle diameter it is excessive with
Matrix adhesive force is little, and between intensity difference, and powder body, the little formation thermal conducting path of contact surface is few, and thermal conductivity is little；Particle diameter is little, and adhesive force is strong,
Material mechanical performance is strong, and particle diameter small specific surface product is bigger bigger with substrate contact face, and formation heat conduction network is intensive, and thermal conductivity is high；
But powder body is too small easily to agglomerate into stress concentration in the base, material mechanical performance can be weakened, reunion increase thermal resistance is reduced
Thermal conductivity.
With the raising of alumina powder jointed filling quality fraction, the heat conductivity of composite constantly increases, and reaches and face when 30%
Boundary's point, more than filling critical point after, as heat filling is in the increase of intrinsic silicon heat conduction path number, the hot-fluid net of aluminium oxide
Road is increased, and system thermal resistance also declines rapidly, so as to thermal conductivity realizes rapid rising；Mechanical property is presented the trend fallen after rising,
It is critical point when 10%, powder filled matrix has optimum dispersion degree, when filling fraction is optimum, height divides powder body in the base
Dissipate, the reinforcement effect of the macromolecule end of the chain and stress concentration are acted on during melting extrusion the stretching that can realize composite and
The lifting of bending strength, and the powder body hole that dispersed filler is formed in the base, then be the approach of high polymer dispersion external energy
One of, so as to realize the rising of impact strength.
When elastomer content increases, composite tensile strength, bending strength and bending moduluses are on a declining curve, and rush
Hit intensity then not only increases, and has in various degree increase than matrix strength and toughness with non-modified matrix phase, and fragility then reduces.
When elastomer content reaches 30%, the impact strength of composite reaches 5.8kJ/m2, the composite than being not added with elastomer
Increase nearly 2 times.
It is slightly decreased with the thermal conductivity of the increase composite of elastomer content, the impact to thermal conductivity is less obvious, and
It is basically identical with unmodified matrix phase specific heat conductance.From table, data can be seen that, the addition of elastomer is for the shape of thermal conducting path
Into impact it is unobvious, do not significantly increase the thermal resistance of composite, the thermal conductivity of composite almost do not affected.
The mechanical property and thermal conductivity of composite prepared by modified matrix are substantially better than composite wood prepared by pure PA6/PET
Material.On the one hand, modified matrix realizes chain extending reaction, and molecular weight increase, mechanical strength are improved；On the other hand, due to improving
The compatibility of PA6/PET, enhances the cohesive force with alumina surface, reduces the fragility of material, and bending moduluses are substantially reduced.
The same aluminium oxide in modified matrix more uniformly spreads, and thermal conducting path is more likely formed, and thermal conductivity is slightly higher.
Claims (5)
1. a kind of preparation method of PA6 heat-conductive composite materials, it is characterised in that comprise the steps：（1）Take aluminium oxide, metatitanic acid
Ester coupling agent, titanate coupling agent and isopropanol are mixed in beaker, after placing half an hour, dropwise pour mixed at high speed into
Mix at a temperature of 80 DEG C 20 minutes with aluminium oxide in machine, be obtained alumina powder jointed；Reselection silane coupler, with dehydrated alcohol
Used as diluent, both ratios are 1: 2, prepare the alumina powder jointed of silane coupled agent content respectively 1%；（2）Take scale stone
Ink, isopropanol, isopropanol and titanate coupling agent are mixed in beaker, after placing half an hour, are dropwise poured into mixed at a high speed
Mix 20 minutes at a temperature of 80 DEG C with graphite in conjunction machine；120 DEG C of dryings 1 hour, it is standby；（3）Take PA6/PET modified matrix with
Alumina powder jointed, after mixed at room temperature 5min in high mixer, input twin-screw extrusion machine travel, pelletizing are dried in baking oven, will
Material input injection machine after drying is prepared into sample.
2. the preparation method of PA6 heat-conductive composite materials according to claim 1, it is characterised in that：The alumina particle
For 4 μm.
3. the preparation method of PA6 heat-conductive composite materials according to claim 1, it is characterised in that：The temperature of the extruder
Degree is set to 180 DEG C -270 DEG C.
4. the preparation method of PA6 heat-conductive composite materials according to claim 1, it is characterised in that：The injection moulding machine
Temperature setting be 270 DEG C.
5. the preparation method of PA6 heat-conductive composite materials according to claim 1, it is characterised in that：The oven temperature is
100 DEG C, drying time is 6 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611119927.2A CN106543710A (en) | 2016-12-08 | 2016-12-08 | A kind of preparation method of PA6 heat-conductive composite materials |
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|---|---|---|---|
| CN201611119927.2A CN106543710A (en) | 2016-12-08 | 2016-12-08 | A kind of preparation method of PA6 heat-conductive composite materials |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109280275A (en) * | 2018-10-17 | 2019-01-29 | 安庆市泽烨新材料技术推广服务有限公司 | Polypropylene scratch-resistant composite material and preparation method |
| CN109467818A (en) * | 2018-10-17 | 2019-03-15 | 安庆市泽烨新材料技术推广服务有限公司 | Scratch resistance PP composite material and preparation method thereof |
| CN109467817A (en) * | 2018-10-17 | 2019-03-15 | 安庆市泽烨新材料技术推广服务有限公司 | Metal-like PP composite material and preparation method thereof |
-
2016
- 2016-12-08 CN CN201611119927.2A patent/CN106543710A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109280275A (en) * | 2018-10-17 | 2019-01-29 | 安庆市泽烨新材料技术推广服务有限公司 | Polypropylene scratch-resistant composite material and preparation method |
| CN109467818A (en) * | 2018-10-17 | 2019-03-15 | 安庆市泽烨新材料技术推广服务有限公司 | Scratch resistance PP composite material and preparation method thereof |
| CN109467817A (en) * | 2018-10-17 | 2019-03-15 | 安庆市泽烨新材料技术推广服务有限公司 | Metal-like PP composite material and preparation method thereof |
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