CN106977908A - A kind of shock resistance scratch-resistant Heat conduction nylon composite material and preparation method thereof - Google Patents
A kind of shock resistance scratch-resistant Heat conduction nylon composite material and preparation method thereof Download PDFInfo
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- CN106977908A CN106977908A CN201610030453.8A CN201610030453A CN106977908A CN 106977908 A CN106977908 A CN 106977908A CN 201610030453 A CN201610030453 A CN 201610030453A CN 106977908 A CN106977908 A CN 106977908A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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Abstract
The present invention relates to a kind of shock resistance scratch-resistant Heat conduction nylon composite material and preparation method thereof, shock resistance scratch-resistant Heat conduction nylon composite material is made by " two step melt-blending processes " with heat conduction component, fire retardant, antioxidant, coupling agent and optional scratch resistance liniment using the nylon composite comprising copolymer nylon as resin matrix in it.The Heat conduction nylon composite material toughness and low-temperature impact property are good, case hardness is low, scraping and wiping resistance performance is excellent, heat conductivility, mechanical property and fire resistance are good, can be widely applied to the higher plastic items field of the cooling requirements such as electric power tool shell, battery pack case, LED radiator, automobile-used LED support.
Description
Technical field
The invention belongs to technical field of polymer materials, and in particular to a kind of shock resistance scratch-resistant heat conduction nylon is combined
Material and preparation method thereof.
Background technology
With electronic equipment lightweight and the development of miniaturization, Electronic Assemblies density is improved rapidly, and this requires member
The heat that device is produced in the course of the work must be distributed and conducted in time, otherwise will influence system energy efficiency profit
With the service life with product.Therefore, heat-conductive composite material turns into new developing direction.
The main method for preparing heat-conductive composite material at present is the filling high heat conduction component into polymeric matrix, is passed through
Interaction between heat filling, forms similar chain or netted distributional pattern-heat conduction network chain in system
And improve the thermal conductivity of composite.
Patent CN104672897A discloses a kind of composite of flame-retarded heat-conducting antistatic nylon 66, and it is with normal
Rule PA66 is matrix, is blended, is made by double screw extruder extruding pelletization with heat filling, antistatic additive,
There is poor toughness, scraping and wiping resistance performance in prepared heat-conductive composite material, had a strong impact on the property of product
Can, limit the application of material.
Patent CN104744935A discloses a kind of Long carbon chain Heat conduction nylon composite material, and it is with Long carbon chain type Buddhist nun
Dragon is matrix, is blended, is made by double screw extruder extruding pelletization with heat filling, fire retardant, prepared
Improvement of the heat-conductive composite material in terms of toughness it is limited, while Long carbon chain type nylon resin matrix cost is general
All over higher.
Patent CN104788951A discloses a kind of LED high thermal conductivities composite, and it is with conventional nylon
For matrix, it is blended, is made by double screw extruder extruding pelletization with heat filling, fire retardant, it is prepared
There is also the problems such as poor toughness, scraping and wiping resistance performance difference for heat-conductive composite material.
It is above-mentioned in the prior art, because inorganic heat filling case hardness is higher, loading is larger, and filler from
The compatibility of body and resin is not ideal enough, causes that such composite has toughness and resistance to low temperature is poor, table
The problems such as surface hardness is big, scraping and wiping resistance performance is poor.Therefore, the problem of presently, there are is to be badly in need of research and development one kind to resist
Impact scratch-resistant Heat conduction nylon composite material and preparation method thereof.
The content of the invention
The technical problems to be solved by the invention are that there is provided a kind of shock resistance is resistance to for above-mentioned the deficiencies in the prior art
Scrape Heat conduction nylon composite material, its using the composition comprising copolymer nylon as resin matrix, with heat conduction component,
Fire retardant, antioxidant, coupling agent and optional scratch resistance liniment are made by " two step melt-blending processes ".This
Inventive method prepare shock resistance scratch-resistant Heat conduction nylon composite material case hardness is low, scraping and wiping resistance performance is good, it is tough
Property and low-temperature impact property are good, and heat conductivility, mechanical property and fire resistance are good.
Therefore, first aspect present invention provides a kind of shock resistance scratch-resistant Heat conduction nylon composite material, it is based on
Component a-c and optional component d gross weight meter include following component：
According to the present invention, the nylon resin is the nylon composite comprising copolymer nylon；The copolymer nylon is
Copolymer comprising the construction unit of nylon 6 Yu nylon66 fiber construction unit；The relative viscosity of the copolymer nylon is
2.8-3.5；The number-average molecular weight of the copolymer nylon is 15000-20000；The molecular weight distribution of the copolymer nylon
Index is 1.7-2.5；The mol ratio of the construction unit of nylon 6 and nylon66 fiber construction unit is in the copolymer nylon
4:1。
According to the present invention, the heat conduction component is that stratiform heat filling and/or needle-like heat filling are filled out with spherical heat conduction
The compound of material and/or spherical heat filling；Based on the gross weight meter of heat conduction component, layered heat filling
And/or content≤30wt% of needle-like heat filling.
In some embodiments of the invention, layered heat filling includes hexahedron type boron nitride and/or expansion
Type graphite；The needle-like heat filling includes carbon fiber and/or halloysite nanotubes；The spherical heat filling bag
Include ball-aluminium oxide and/or spherical alumina magnesium.
According to the present invention, the fire retardant is halogen-free flame retardants；The halogen-free flame retardants includes phosphorus nitrogen fire-retardant
Agent and/or inorganic fire-retardant agent；The phosphorus nitrogen fire-retardant agent includes melamine-Quadrafos, melamine
One or more in amine-polyphosphate, melamine-cyanurate and melamine-focusing phosphate；Institute
Stating inorganic fire-retardant agent includes the one or more in APP, aluminium hydroxide and magnesium hydroxide.
In some embodiments of the invention, the scratch resistance liniment includes calcirm-fluoride, molybdenum disulfide and polytetrafluoroethyl-ne
One or more in alkene；It is preferred that the scratch resistance liniment is calcirm-fluoride.
In other embodiments of the present invention, the antioxidant includes Hinered phenols antioxidant and/or phosphite ester
Kind antioxidant.
In other embodiments of the invention, the coupling agent includes silane coupler and/or epoxy radicals aliphatic is common
Polymers.
Second aspect of the present invention provides a kind of preparation method of composite as described in the first aspect of the invention, its
Including：
Step A, heat conduction component, coupling agent and optional scratch resistance liniment are well mixed, and pretreatment thing is made；
Step B, pretreatment thing is well mixed with nylon resin, mixture I is made；
Step C, using melt-blending process, by mixture I by double screw extruder melting extrusion, granulation,
Master batch is made；
Step D, master batch is well mixed with fire retardant and antioxidant, and mixtures II is made；
Step E, using melt-blending process, by mixtures II by double screw extruder melting extrusion, granulation,
Shock resistance scratch-resistant Heat conduction nylon composite material is made.
In some embodiments of the invention, in step, the temperature of the mixing is 50-70 DEG C；It is described
The time of mixing is 2-3min.
In other embodiments of the present invention, in step C, the process conditions of the double screw extruder are：
One area's temperature：200-220℃；Two area's temperature：240-260℃；Three area's temperature：240-260℃；Four area's temperature：
250-270℃；Five 240-260 DEG C of area's temperature；Six area's temperature：230-250℃；Seven 230-250 DEG C of area's temperature；
Eight area's temperature：235-250℃；Nine area's temperature：230-245℃；Screw speed is：350-400r/min.
In other embodiments of the invention, in step E, the process conditions of the double screw extruder are：
One area's temperature：210-230℃；Two area's temperature：240-260℃；Three area's temperature：250-270℃；Four area's temperature：
255-270℃；Five 240-260 DEG C of area's temperature；Six area's temperature：230-250℃；Seven 230-250 DEG C of area's temperature；
Eight area's temperature：235-250℃；Nine area's temperature：230-245℃；Screw speed is：300-350r/min.
Brief description of the drawings
Come to be described in further detail the present invention below in conjunction with the accompanying drawings.
Fig. 1 is that the ESEM of shock resistance scratch-resistant Heat conduction nylon composite material prepared by the embodiment of the present invention 3 shines
Piece.
Embodiment
To make the present invention easier to understand, the present invention is described in detail below in conjunction with embodiment and accompanying drawing, this
A little embodiments only serve illustrative, it is not limited to application of the invention.
As it was previously stated, heat-conductive composite material of the prior art there is toughness and resistance to low temperature is poor, surface is hard
The problems such as degree is big, scraping and wiping resistance performance is poor, has had a strong impact on product properties, has limited the application of composite.
The present inventor's research is found, using copolymer nylon as resin matrix, with heat conduction component, fire retardant, antioxygen
Agent, coupling agent and optional scratch resistance liniment pass through heat-conductive composite material made from " two step melt-blending processes "
Toughness and low-temperature impact property are good, and case hardness is low, scraping and wiping resistance performance is excellent, heat conductivility, mechanical property
It is good with fire resistance.The present invention is based on what above-mentioned discovery was made.
Therefore, the shock resistance scratch-resistant Heat conduction nylon composite material involved by first aspect present invention is based on component a-c
And optional component d gross weight meter includes following component：
In above-mentioned Heat conduction nylon composite material, the nylon resin is the nylon composite comprising copolymer nylon.
Term " composition for including copolymer nylon " of the present invention refers to that the nylon resin can be copolymerization Buddhist nun
Dragon, or the composition of copolymer nylon and general nylon.The general nylon include nylon 6, nylon66 fiber,
One or more in nylon 11, nylon 12, nylon 612, nylon 1212 and aromatic nylon.For example,
In some embodiments of the invention, the nylon resin is copolymer nylon；In other embodiments of the present invention
In, the nylon resin is the composition of copolymer nylon and nylon 6；In other embodiments of the invention, institute
It is copolymer nylon and nylon 6 and the composition of nylon66 fiber to state nylon resin.
In above-mentioned Heat conduction nylon composite material, the copolymer nylon is to include the construction unit of nylon 6 and nylon66 fiber
The copolymer of construction unit.
In above-mentioned Heat conduction nylon composite material, the copolymer nylon by caprolactam and PA66 salt catalyst,
It is made in the presence of water and initiation monomer by hydrolytic polymerization.
In above-mentioned Heat conduction nylon composite material, the relative viscosity of the copolymer nylon is 2.8-3.5；It is preferred that described common
The relative viscosity of poly- nylon is 3.2-3.5；The number-average molecular weight of the copolymer nylon is 15000-20000；It is preferred that
The number-average molecular weight of the copolymer nylon is 18000-20000；The molecular weight distributing index of the copolymer nylon is
1.7-2.5；It is preferred that the molecular weight distributing index of the copolymer nylon is 1.8-2.5；The further preferred copolymerization Buddhist nun
The molecular weight distributing index of dragon is 2.2-2.5；It is preferred that the construction unit of nylon 6 and nylon66 fiber in the copolymer nylon
The mol ratio of construction unit is 4:1.
Term " relative viscosity " of the present invention refers to the concentrated sulfuric acid solution of copolymer nylon (concentration is 0.01g/mL)
Viscosity and concentrated sulfuric acid solution viscosity ratio, the mass fraction of the concentrated sulfuric acid is 96%.Phase in the present invention
Test to viscosity is this area conventional technical means, for example, determine copolymer nylon respectively by Ubbelohde viscometer
The delivery time of sulfuric acid solution and the delivery time of the concentrated sulfuric acid, the ratio of the two are relative viscosity value.
Copolymer nylon is introduced in the nylon resin of the present invention as resin matrix, passes through nylon66 fiber in copolymer nylon
Construction unit has upset the regular arrangement of the molecular structure of nylon 6, reduces the crystallinity of system, makes 6 points of nylon
The amorphous region increase of son, reduces intramolecular hydrogen bond effect, greatly improves the toughness of resin matrix, drop
The low case hardness of composite.
In above-mentioned Heat conduction nylon composite material, the heat conduction component is stratiform heat filling and/or needle-like heat filling
With spherical heat filling and/or the compound of spherical heat filling；It is described based on the gross weight meter of heat conduction component
Content≤30wt% of stratiform heat filling and/or needle-like heat filling.
In above-mentioned Heat conduction nylon composite material, layered heat filling includes hexahedron type boron nitride and/or expansion
Type graphite；The needle-like heat filling includes carbon fiber and/or halloysite nanotubes (HNTs)；It is described spherical
Heat filling includes ball-aluminium oxide and/or spherical alumina magnesium.
Heretofore described stratiform heat filling is multilayered thermally-conductive filler.
In above-mentioned Heat conduction nylon composite material, the fire retardant is halogen-free flame retardants；The halogen-free flame retardants includes
Phosphorus nitrogen fire-retardant agent and/or inorganic fire-retardant agent；The phosphorus nitrogen fire-retardant agent includes melamine-poly- phosphorus
Hydrochlorate (MPP), melamine-polyphosphate (MPP), melamine-cyanurate (MCA) and
One or more in melamine-focusing phosphate；The inorganic fire-retardant agent includes APP
(APP), aluminium hydroxide (Al (OH)3) and magnesium hydroxide (Mg (OH)2) in one or more.
In above-mentioned Heat conduction nylon composite material, the scratch resistance liniment includes calcirm-fluoride, molybdenum disulfide and polytetrafluoroethyl-ne
One or more in alkene.It is preferred that the scratch resistance liniment is calcirm-fluoride.Based on component a-c and optional component
D gross weight meter, the content of preferably described scratch resistance liniment is 0.5wt%≤scratch resistance liniment≤5wt%；It is furthermore preferred that
The content of the scratch resistance liniment is 2wt%.
The scratch resistance liniments such as calcirm-fluoride, calcirm-fluoride and heat conduction component are added in Heat conduction nylon composite material of the present invention
Cooperative effect can occur in friction process, boron nitride-calcirm-fluoride-nylon (BN-CaF is formed2- Nylon) even
Continuous thin transfer film, the intermolecular force of boron nitride-calcirm-fluoride-nylon improves the combination between transfer membrane and antithesis
The scraping and wiping resistance performance of intensity and composite.
In above-mentioned Heat conduction nylon composite material, the antioxidant includes Hinered phenols antioxidant and/or phosphorous acid esters
Antioxidant.
In above-mentioned Heat conduction nylon composite material, the coupling agent includes silane coupler and/or epoxy radicals aliphatic is common
Polymers.
Silane coupler of the present invention be this area conventional selection, for example, the trade mark be KH792, KH550,
KH560 and KH570 silane coupler.
Term " optionally " of the present invention refers to contain or not contain, and also refers to add or is added without.
The component of scope is limited in the present invention with "≤", refers to the component of optional or selective addition.
For example, " component d, scratch resistance liniment≤5wt% " represent scratch resistance liniment to be optionally added component, and it is added
Measure as 0≤scratch resistance liniment≤5wt%.In another example, " the content of layered heat filling and/or needle-like heat filling
≤ 30wt% " represents stratiform heat filling and/or needle-like heat filling to be optionally added component, and its addition
For 0≤stratiform heat filling and/or needle-like heat filling≤30wt%.
The preparation method of the composite as involved by first aspect present invention involved by second aspect of the present invention
(i.e. " two step melt-blending processes "), including：
Step A, heat conduction component, coupling agent and optional scratch resistance liniment are well mixed, and pretreatment thing is made；
Step B, pretreatment thing is well mixed with nylon resin, mixture I is made；
Step C, using melt-blending process, by mixture I by double screw extruder melting extrusion, granulation,
Master batch is made；
Step D, master batch is well mixed with fire retardant and antioxidant, and mixtures II is made；
Step E, using melt-blending process, by mixtures II by double screw extruder melting extrusion, granulation,
Shock resistance scratch-resistant Heat conduction nylon composite material is made.
In the preparation method of above-mentioned Heat conduction nylon composite material, in step, the temperature of the mixing is
50-70℃；The time of the mixing is 2-3min.
The preparation method of above-mentioned Heat conduction nylon composite material is " two step melt-blending processes ", i.e., squeezed using twin-screw
Go out machine and melting extrusion processing is carried out respectively to mixture I and mixtures II.Specifically, using double in step C
Screw extruder carries out first step melt blending, wherein the process conditions of the double screw extruder are：One area's temperature
Degree：200-220℃；Two area's temperature：240-260℃；Three area's temperature：240-260℃；Four area's temperature：250-270℃；
Five 240-260 DEG C of area's temperature；Six area's temperature：230-250℃；Seven 230-250 DEG C of area's temperature；Eight area's temperature：
235-250℃；Nine area's temperature：230-245℃；Screw speed is：350-400r/min；Used in step E
Double screw extruder carries out second step melt blending, wherein the process conditions of the double screw extruder are：One area
Temperature：210-230℃；Two area's temperature：240-260℃；Three area's temperature：250-270℃；Four area's temperature：
255-270℃；Five 240-260 DEG C of area's temperature；Six area's temperature：230-250℃；Seven 230-250 DEG C of area's temperature；
Eight area's temperature：235-250℃；Nine area's temperature：230-245℃；Screw speed is：300-350r/min.
According to some preferred embodiments of the present invention, the system of the shock resistance scratch-resistant Heat conduction nylon composite material
Preparation Method comprises the following steps：
(1) being added to stratiform heat filling, spherical heat filling, scratch resistance liniment and coupling agent can hot type
Mix in pot, (rotating speed ＞ 100r/min) is well mixed at a high speed, pretreatment thing is made；It is 60 DEG C to mix pot temperature,
Incorporation time is 3min；
(2) pretreatment thing is well mixed with nylon resin high speed (rotating speed ＞ 100r/min), mixture is made
I；The time of the mixing is 3min；
(3) heat conduction, scratch-resistant master batch is made by double screw extruder melting extrusion, granulation in mixture I；
The process conditions of double screw extruder are：One area's temperature：220℃；Two area's temperature：240℃；Three area's temperature：
240℃；Four area's temperature：250℃；Five 240 DEG C of area's temperature；Six area's temperature：230℃；Seven 230 DEG C of area's temperature；
Eight area's temperature：235℃；Nine area's temperature：245℃；Screw speed is：380r/min.
(4) heat conduction, scratch-resistant master batch are well mixed with fire retardant and antioxidant, mixtures II is made；
(5) by mixtures II by double screw extruder melting extrusion, granulation, shock resistance scratch-resistant is made and leads
Hot nylon composite materials；The process conditions of double screw extruder are：One area's temperature：230℃；Two area's temperature：
240℃；Three area's temperature：250℃；Four area's temperature：255℃；Five 240 DEG C of area's temperature；Six area's temperature：230℃；
Seven 230 DEG C of area's temperature；Eight area's temperature：235℃；Nine area's temperature：245℃；Screw speed is：350r/min.
Present invention use " two step melt-blending processes " prepares shock resistance scratch-resistant Heat conduction nylon composite material, with answering
Heat conduction component in condensation material component coordinates, and this method is more beneficial for the layer and layer that Ball-type packing enters layered fillers
Between space, promote two kinds of fillers of different shapes interactions and scattered, that is, be conducive to stratiform heat filling
It is " expansion layer " and scattered, it is ensured that spherical heat filling can be effectively combined with stratiform heat filling, promote heat conduction network chain
Formation, so as to improve the heat conductivility of composite.
The SHJ-35 type twin-screw extrusions produced in the present invention from Nanjing Fu Ya rubber and plastics machines Manufacturing Co., Ltd
Machine carries out melting extrusion to material.
Mold apparatus, injection device, gas injection equipment, injection molding apparatus or extrusion are can select in the present invention
The shock resistance scratch-resistant Heat conduction nylon composite material production that equipment prepares the present invention shapes various products.Such as without spy
Do not mentionlet alone bright, instrument of the present invention, equipment are this area conventional selection.
The shock resistance scratch-resistant Heat conduction nylon composite material that the present invention is provided can be applied to IGBT semiconductor components and devices
The radiating such as plastic casing, electric power tool shell, battery pack case, LED radiator, automobile-used LED support will
Ask higher plastic items field.
The structural characterization and performance test methods of the Heat conduction nylon composite material of the present invention are as follows：
(1) molecular weight and molecualr weight distribution is tested：Using the gel osmoticing chromatogram analysis of waters companies of the U.S.
Instrument is determined, and uses metacresol for mobile phase and solvent, and copolymer nylon is configured into first between 0.3wt%-0.5wt%
Phenol solution is tested, and column temperature is 70 DEG C, and flow velocity is 1mL/min.
(2) ESEM (SEM) is analyzed：Using the LEO1530VP ESEMs of German LED companies
Observe the surface microscopic topographic of composite；Test sample is 12.5mm from ESEM probe distance WD,
Test voltage (EHT) be 20.00kV, secondary electron throw as signal be SE1, multiplication factor be 3.00k ×.
(3) impact strength is tested：Surveyed using the XJJ-50 types impact tester for simple supported beam of Chengde testing machine factory
Determine impact strength of the composite sample under normal temperature and low temperature.Surveying the low temperature impact strength of composite sample
Before, sample is placed into 2h under conditions of -30 DEG C.
(4) tensile strength and bending strength test：Using the CMT4104 of Nanjing Baruch's experimental instruments and equipment limited
Type electronic universal tester is determined.
(5) UL94 is tested：Using the CZF-4 types horizontal vertical burning of meta analysis Instrument Ltd. on Nanjing
Tester determines the fire resistance of composite sample.It is respectively 1.6mm's and 0.8mm to thickness in test
Sample is tested.
(6) case hardness is tested：Using the XHR-15D plastic Rockwell Hardness meters of Shanghai Material Testing Machine factory
Determine.
(7) wear rate is tested：Using the GT-70R-D types of High Speed Rail Testing Instruments Co., Ltd (GOTECH)
Friabilator is determined.Composite is molded into standard friction test test block, after test block is dried 2 hours through 100 DEG C,
It is placed in standby after cooling 4h in drying basin.Fraction time 2h, sliding speed is 0.43m/s, load 300N.
The precision electronic balance for being 0.01mg with sensibility reciprocal determines mass loss during abrasion, and according to polymeric matrix and filler
Relative density and experiment parameter will wear and tear mass conversion be Volume erosion rate.To each group of test block in identical
4 repetitions are carried out under experiment condition to test, and select 3 statistical averages being closer to as experimental result.
(8) thermal conductivity factor：Thermal conductivity factor is determined using heat conduction coefficient tester Hot Disk, and testing standard is
ISO-DIS22007。
(9) heat distortion temperature：Testing standard is GB/T 1634-2004 (0.45MPa, B method).
The shock resistance scratch-resistant Heat conduction nylon composite material that the present invention is provided has the following advantages that：
(1) toughness and low-temperature impact property are good；
(2) case hardness is low, scraping and wiping resistance performance is excellent；
(3) excellent heat conductivility, heat transfer property and high thermal diffusion coefficient；
(4) flame retarding efficiency height, halogen-free environmental, low flame radiation, smoke density are low；
(5) good insulation preformance, excellent in mechanical performance, high temperature resistant, ageing-resistant；
(6) product molding shrinkage factor is low, good stability of the dimension, low warpage, flatness are high.
Embodiment
Embodiment 1：Two step melt-blending processes prepare Heat conduction nylon composite material
(1) by 1200g ball-aluminium oxides and 9g KH550 be added to can hot type mix pot in, regulation mix
The temperature of pot is 60 DEG C, high-speed uniform mixing 3min, and pretreatment thing is made；
(2) to addition 1500g copolymer nylons in thing are pre-processed, (relative viscosity is 2.8, and number-average molecular weight is
15000, molecular weight distributing index is 1.8, the construction unit of nylon 6 and nylon66 fiber construction unit in copolymer nylon
Mol ratio be 4:1) mixture I is made in resin, high-speed uniform mixing 3min；
(3) heat conduction, scratch-resistant master batch is made by double screw extruder melting extrusion, granulation in mixture I；
The process conditions of double screw extruder are：One area's temperature：220℃；Two area's temperature：240℃；Three area's temperature：
240℃；Four area's temperature：250℃；Five 240 DEG C of area's temperature；Six area's temperature：230℃；Seven 230 DEG C of area's temperature；
Eight area's temperature：235℃；Nine area's temperature：245℃；Screw speed is：380r/min；
(4) heat conduction, scratch-resistant master batch and 150g APPs, 150g magnesium hydroxides and 15g antioxidant are mixed
Close uniform, mixtures II is made；
(5) by mixtures II by double screw extruder melting extrusion, granulation, shock resistance scratch-resistant is made and leads
Hot nylon composite materials；The process conditions of double screw extruder are：One area's temperature：230℃；Two area's temperature：
240℃；Three area's temperature：250℃；Four area's temperature：255℃；Five 240 DEG C of area's temperature；Six area's temperature：230℃；
Seven 230 DEG C of area's temperature；Eight area's temperature：235℃；Nine area's temperature：245℃；Screw speed is：350r/min.
Obtained Heat conduction nylon composite material is made by standard batten using injection molding equipment, and to its progressive
It can test, the results are shown in Table 1.
Embodiment 2：Two step melt-blending processes prepare Heat conduction nylon composite material
(1) being added to 300g boron nitride, 900g ball-aluminium oxides and 9g KH550 can the mixed pot of hot type
In, the temperature that regulation mixes pot is 60 DEG C, high-speed uniform mixing 3min, and pretreatment thing is made；
(2) to addition 1500g copolymer nylons in thing are pre-processed, (relative viscosity is 3.2, and number-average molecular weight is
18000, molecular weight distributing index is 2.2, the construction unit of nylon 6 and nylon66 fiber construction unit in copolymer nylon
Mol ratio be 4:1) mixture I is made in resin, high-speed uniform mixing 3min；
(3) heat conduction, scratch-resistant master batch is made by double screw extruder melting extrusion, granulation in mixture I；
The process conditions of double screw extruder are：One area's temperature：220℃；Two area's temperature：240℃；Three area's temperature：
240℃；Four area's temperature：250℃；Five 240 DEG C of area's temperature；Six area's temperature：230℃；Seven 230 DEG C of area's temperature；
Eight area's temperature：235℃；Nine area's temperature：245℃；Screw speed is：380r/min；
(4) heat conduction, scratch-resistant master batch and 150g APPs, 150g magnesium hydroxides and 15g antioxidant are mixed
Close uniform, mixtures II is made；
(5) by mixtures II by double screw extruder melting extrusion, granulation, shock resistance scratch-resistant is made and leads
Hot nylon composite materials；The process conditions of double screw extruder are：One area's temperature：230℃；Two area's temperature：
240℃；Three area's temperature：250℃；Four area's temperature：255℃；Five 240 DEG C of area's temperature；Six area's temperature：230℃；
Seven 230 DEG C of area's temperature；Eight area's temperature：235℃；Nine area's temperature：245℃；Screw speed is：350r/min.
Obtained Heat conduction nylon composite material is made by standard batten using injection molding equipment, and to its progressive
It can test, the results are shown in Table 1.
Embodiment 3：Two step melt-blending processes prepare Heat conduction nylon composite material
(1) being added to 300g boron nitride, 900g ball-aluminium oxides, 60g calcirm-fluoride and 9g KH550 can
Hot type is mixed in pot, and the temperature that regulation mixes pot is 60 DEG C, and pretreatment is made in high-speed uniform mixing 3min
Thing；
(2) to addition 1440g copolymer nylons in thing are pre-processed, (relative viscosity is 3.5, and number-average molecular weight is
20000, molecular weight distributing index is 2.5, the construction unit of nylon 6 and nylon66 fiber construction unit in copolymer nylon
Mol ratio be 4:1) mixture I is made in resin, high-speed uniform mixing 3min；
(3) heat conduction, scratch-resistant master batch is made by double screw extruder melting extrusion, granulation in mixture I；
The process conditions of double screw extruder are：One area's temperature：220℃；Two area's temperature：240℃；Three area's temperature：
240℃；Four area's temperature：250℃；Five 240 DEG C of area's temperature；Six area's temperature：230℃；Seven 230 DEG C of area's temperature；
Eight area's temperature：235℃；Nine area's temperature：245℃；Screw speed is：380r/min；
(4) heat conduction, scratch-resistant master batch and 150g APPs, 150g magnesium hydroxides and 15g antioxidant are mixed
Close uniform, mixtures II is made；
(5) by mixtures II by double screw extruder melting extrusion, granulation, shock resistance scratch-resistant is made and leads
Hot nylon composite materials；The process conditions of double screw extruder are：One area's temperature：230℃；Two area's temperature：
240℃；Three area's temperature：250℃；Four area's temperature：255℃；Five 240 DEG C of area's temperature；Six area's temperature：230℃；
Seven 230 DEG C of area's temperature；Eight area's temperature：235℃；Nine area's temperature：245℃；Screw speed is：350r/min.
Using the structure of Heat conduction nylon composite material made from scanning electron microscopic observation, as a result as shown in Figure 1.
Obtained Heat conduction nylon composite material is made by standard batten using injection molding equipment, and to its progressive
It can test, the results are shown in Table 1.
Comparative example 1：Two step melt-blending processes prepare Heat conduction nylon composite material
(1) by 1200g ball-aluminium oxides and 9g KH550 be added to can hot type mix pot in, regulation mix
The temperature of pot is 60 DEG C, high-speed uniform mixing 3min, and pretreatment thing is made；
(2) added into pretreatment thing 1500g nylon 6 (relative viscosity is 2.5, and number-average molecular weight is 15000,
Molecular weight distributing index is 1.6) high-speed uniform mixing 3min, and mixture I is made；
(3) heat conduction, scratch-resistant master batch is made by double screw extruder melting extrusion, granulation in mixture I；
The process conditions of double screw extruder are：One area's temperature：220℃；Two area's temperature：240℃；Three area's temperature：
240℃；Four area's temperature：250℃；Five 240 DEG C of area's temperature；Six area's temperature：230℃；Seven 230 DEG C of area's temperature；
Eight area's temperature：235℃；Nine area's temperature：245℃；Screw speed is：380r/min；
(4) heat conduction, scratch-resistant master batch and 150g APPs, 150g magnesium hydroxides and 15g antioxidant are mixed
Close uniform, mixtures II is made；
(5) by mixtures II by double screw extruder melting extrusion, granulation, shock resistance scratch-resistant is made and leads
Hot nylon composite materials；The process conditions of double screw extruder are：One area's temperature：230℃；Two area's temperature：
240℃；Three area's temperature：250℃；Four area's temperature：255℃；Five 240 DEG C of area's temperature；Six area's temperature：230℃；
Seven 230 DEG C of area's temperature；Eight area's temperature：235℃；Nine area's temperature：245℃；Screw speed is：350r/min.
Obtained Heat conduction nylon composite material is made by standard batten using injection molding equipment, and to its progressive
It can test, the results are shown in Table 1.
Comparative example 2：Two step melt-blending processes prepare Heat conduction nylon composite material
(1) being added to 300g boron nitride, 900g ball-aluminium oxides and 9g KH550 can the mixed pot of hot type
In, the temperature that regulation mixes pot is 60 DEG C, high-speed uniform mixing 3min, and pretreatment thing is made；
(2) added into pretreatment thing 1500g nylon66 fibers (relative viscosity is 2.4, and number-average molecular weight is 15000,
Molecular weight distributing index is 2.0) high-speed uniform mixing 3min, and mixture I is made；
(3) heat conduction, scratch-resistant master batch is made by double screw extruder melting extrusion, granulation in mixture I；
The process conditions of double screw extruder are：One area's temperature：220℃；Two area's temperature：240℃；Three area's temperature：
240℃；Four area's temperature：250℃；Five 240 DEG C of area's temperature；Six area's temperature：230℃；Seven 230 DEG C of area's temperature；
Eight area's temperature：235℃；Nine area's temperature：245℃；Screw speed is：380r/min；
(4) heat conduction, scratch-resistant master batch and 150g APPs, 150g magnesium hydroxides and 15g antioxidant are mixed
Close uniform, mixtures II is made；
(5) by mixtures II by double screw extruder melting extrusion, granulation, shock resistance scratch-resistant is made and leads
Hot nylon composite materials；The process conditions of double screw extruder are：One area's temperature：230℃；Two area's temperature：
240℃；Three area's temperature：250℃；Four area's temperature：255℃；Five 240 DEG C of area's temperature；Six area's temperature：230℃；
Seven 230 DEG C of area's temperature；Eight area's temperature：235℃；Nine area's temperature：245℃；Screw speed is：350r/min.
Obtained Heat conduction nylon composite material is made by standard batten using injection molding equipment, and to its progressive
It can test, the results are shown in Table 1.
Comparative example 3：Two step melt-blending processes prepare Heat conduction nylon composite material
(1) being added to 300g boron nitride, 900g ball-aluminium oxides, 60g calcirm-fluoride and 9g KH550 can
Hot type is mixed in pot, and the temperature that regulation mixes pot is 60 DEG C, and pretreatment is made in high-speed uniform mixing 3min
Thing；
(2) added into pretreatment thing 1440g nylon 6 (relative viscosity is 2.5, and number-average molecular weight is 15000,
Molecular weight distributing index is 1.6) high-speed uniform mixing 3min, and mixture I is made；
(3) heat conduction, scratch-resistant master batch is made by double screw extruder melting extrusion, granulation in mixture I；
The process conditions of double screw extruder are：One area's temperature：220℃；Two area's temperature：240℃；Three area's temperature：
240℃；Four area's temperature：250℃；Five 240 DEG C of area's temperature；Six area's temperature：230℃；Seven 230 DEG C of area's temperature；
Eight area's temperature：235℃；Nine area's temperature：245℃；Screw speed is：380r/min；
(4) heat conduction, scratch-resistant master batch and 150g APPs, 150g magnesium hydroxides and 15g antioxidant are mixed
Close uniform, mixtures II is made；
(5) by mixtures II by double screw extruder melting extrusion, granulation, shock resistance scratch-resistant is made and leads
Hot nylon composite materials；The process conditions of double screw extruder are：One area's temperature：230℃；Two area's temperature：
240℃；Three area's temperature：250℃；Four area's temperature：255℃；Five 240 DEG C of area's temperature；Six area's temperature：230℃；
Seven 230 DEG C of area's temperature；Eight area's temperature：235℃；Nine area's temperature：245℃；Screw speed is：350r/min.
Obtained Heat conduction nylon composite material is made by standard batten using injection molding equipment, and to its progressive
It can test, the results are shown in Table 1.
Comparative example 4：One step melt-blending process prepares Heat conduction nylon composite material
(1) 300g boron nitride, 900g ball-aluminium oxides and 9g KH550 are added in high-speed mixer,
High-speed uniform mixing 3min, is made pretreatment thing；
(2) to addition 1440g copolymer nylons in thing are pre-processed, (relative viscosity is 3.5, and number-average molecular weight is
20000, molecular weight distributing index is 2.5, the construction unit of nylon 6 and nylon66 fiber construction unit in copolymer nylon
Mol ratio be 4:1), 60g calcirm-fluoride, 150g APPs, 150g magnesium hydroxides and 15g antioxidant fill
Divide uniform mixing 3min, mixture is made；
(3) Heat conduction nylon composite material is made by double screw extruder melting extrusion, granulation in mixture；
The process conditions of double screw extruder are：One area's temperature：220℃；Two area's temperature：240℃；Three area's temperature：
240℃；Four area's temperature：250℃；Five 240 DEG C of area's temperature；Six area's temperature：230℃；Seven 230 DEG C of area's temperature；
Eight area's temperature：235℃；Nine area's temperature：245℃；Screw speed is：380r/min；
Obtained Heat conduction nylon composite material is made by standard batten using injection molding equipment, and to its progressive
It can test, the results are shown in Table 1.
The Heat conduction nylon composite material properties of sample test result of table 1
As can be seen that stratiform heat conduction from the stereoscan photograph of the Heat conduction nylon composite material sample shown in Fig. 1
Filler can interact with spherical heat filling, and be uniformly distributed in resin matrix.
It can be seen from the data of table 1 by embodiments of the invention 1 with contrast 1 compared with, embodiment 2 with contrast
Example 2 is compared, embodiment 3 compared with comparative example 3, the Heat conduction nylon composite material sample in the embodiment of the present invention
Impact property and low-temperature flexibility improve more than 10%；The case hardness of composite is lower, scratch resistance
Can be more preferably.The contrast embodiment of the present invention 3 can be seen that with comparative example 4 and compare " a step melt-blending process ",
" two step melt-blending processes " is more beneficial for " the expansion layer " of stratiform heat filling and its scattered in resin matrix,
So as to promote the formation of heat conduction network chain in matrix, macro manifestations are that composite possesses higher thermal conductivity factor, more
Excellent mechanical property, heat resistance and fire resistance.
It should be noted that embodiment described above is only used for explaining the present invention, do not constitute to the present invention's
Any limitation.By referring to exemplary embodiments, invention has been described, it should be appreciated that wherein used
Word is descriptive and explanatory vocabulary, rather than limited vocabulary.Can be by regulation in the claims in the present invention
In the range of the present invention is modified, and in without departing substantially from scope and spirit of the present invention to the present invention progress
Revision.Although the present invention described in it is related to specific method, material and embodiment, it is not intended that
The present invention is limited to wherein disclosed particular case, on the contrary, to can be extended to other all with identical function by the present invention
Methods and applications, resin matrix, binding resin matrix are used as example with the nylon composite comprising copolymer nylon
And the preparation method set by the characteristic of heat filling, there is universal applicability to filled-type thermally conductive system.
Claims (10)
1. a kind of shock resistance scratch-resistant Heat conduction nylon composite material, it is based on component a-c and optional component d
Gross weight meter include following component：
2. composite according to claim 1, it is characterised in that
The nylon resin is the nylon composite comprising copolymer nylon；
The copolymer nylon is the copolymer comprising the construction unit of nylon 6 Yu nylon66 fiber construction unit；It is described common
The relative viscosity of poly- nylon is 2.8-3.5；The number-average molecular weight of the copolymer nylon is 15000-20000；It is described
The molecular weight distributing index of copolymer nylon is 1.7-2.5；The construction unit of nylon 6 and nylon66 fiber in the copolymer nylon
The mol ratio of construction unit is 4:1.
3. composite according to claim 1 or 2, it is characterised in that the heat conduction component is stratiform
Heat filling and/or needle-like heat filling and spherical heat filling and/or the compound of spherical heat filling；Base
In the gross weight meter of heat conduction component, content≤30wt% of layered heat filling and/or needle-like heat filling.
4. the composite according to any one in claim 1-3, it is characterised in that layered to lead
Hot filler includes hexahedron type boron nitride and/or expanded graphites；The needle-like heat filling include carbon fiber and/
Or halloysite nanotubes；The spherical heat filling includes ball-aluminium oxide and/or spherical alumina magnesium.
5. the composite according to any one in claim 1-4, it is characterised in that the fire retardant
For halogen-free flame retardants；The halogen-free flame retardants includes phosphorus nitrogen fire-retardant agent and/or inorganic fire-retardant agent；It is described
The agent of phosphorus nitrogen fire-retardant includes melamine-Quadrafos, melamine-polyphosphate, melamine-cyanogen urea
One or more in hydrochlorate and melamine-focusing phosphate；The inorganic fire-retardant agent includes polyphosphoric acid
One or more in ammonium, aluminium hydroxide and magnesium hydroxide.
6. the composite according to any one in claim 1-5, it is characterised in that the scratch-resistant
Agent includes the one or more in calcirm-fluoride, molybdenum disulfide and polytetrafluoroethylene (PTFE)；It is preferred that the scratch resistance liniment is fluorine
Change calcium；
The antioxidant includes Hinered phenols antioxidant and/or phosphite ester kind antioxidant；
The coupling agent includes silane coupler and/or epoxy radicals aliphatic polyester.
7. the preparation method of composite as described in any one in a kind of 1-6 such as claim, it includes：
Step A, heat conduction component, coupling agent and optional scratch resistance liniment are well mixed, and pretreatment thing is made；
Step B, pretreatment thing is well mixed with nylon resin, mixture I is made；
Step C, using melt-blending process, by mixture I by double screw extruder melting extrusion, granulation,
Master batch is made；
Step D, master batch is well mixed with fire retardant and antioxidant, and mixtures II is made；
Step E, using melt-blending process, by mixtures II by double screw extruder melting extrusion, granulation,
Shock resistance scratch-resistant Heat conduction nylon composite material is made.
8. preparation method according to claim 7, it is characterised in that in step, the mixing
Temperature be 50-70 DEG C；The time of the mixing is 2-3min.
9. the preparation method according to claim 7 or 8, it is characterised in that in step C, described double
The process conditions of screw extruder are：One area's temperature：200-220℃；Two area's temperature：240-260℃；3rd area
Temperature：240-260℃；Four area's temperature：250-270℃；Five 240-260 DEG C of area's temperature；Six area's temperature：230-250℃；
Seven 230-250 DEG C of area's temperature；Eight area's temperature：235-250℃；Nine area's temperature：230-245℃；Screw speed is：
350-400r/min。
10. the preparation method according to any one in claim 7-9, it is characterised in that in step E
In, the process conditions of the double screw extruder are：One area's temperature：210-230℃；Two area's temperature：240-260℃；
Three area's temperature：250-270℃；Four area's temperature：255-270℃；Five 240-260 DEG C of area's temperature；Six area's temperature：
230-250℃；Seven 230-250 DEG C of area's temperature；Eight area's temperature：235-250℃；Nine area's temperature：230-245℃；
Screw speed is：300-350r/min.
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