CN104744935B - A kind of Long carbon chain Heat conduction nylon composite material and preparation method thereof - Google Patents
A kind of Long carbon chain Heat conduction nylon composite material and preparation method thereof Download PDFInfo
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- 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
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
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- C—CHEMISTRY; METALLURGY
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- 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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- C—CHEMISTRY; METALLURGY
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- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The present invention relates to technical field of polymer composite materials, and in particular to a kind of Long carbon chain Heat conduction nylon composite material, mainly includes：Long carbon chain nylon resin 20 40%, heat filling 30 50%, reinforcer 5 20%, halogen-free flame retardants 5 20%, coupling agent 0.1 0.5%, lubricant 0.4 1.0%, antioxidant 0.1 0.5%, toner 0.1 5%, raw material is weighed by composition of raw materials mass percent, long carbon chain nylon resin and coupling agent are mixed in mixed cylinder, antioxidant is then added and remixes, add heat filling, halogen-free flame retardants, lubricant, toner to remix, last melting extrusion.The composite of the present invention prepared can be tested by the thermal shock of more than 1000 hours at 40 DEG C ~ 120 DEG C, low-gravity, low water absorption, high tenacity, is not separated out, dimensionally stable, viscosity is relatively low, reduces equipment attrition, article surface does not whiten when particularly doing grey product.
Description
Technical field
The present invention relates to technical field of polymer composite materials, and in particular to a kind of Long carbon chain Heat conduction nylon composite material and
Its preparation method.
Background technology
Existing power-type LED illumination is general to use conventional aluminum alloy heat-sink shell, with good heat conductivity, efficiency of thermal transfer
High the advantages of, also there are quality big, electrical insulating property and corrosion resistance is poor, manufacturing procedure complexity, low production efficiency, electroplating surface pollute
The shortcomings of.In the every field of the modern life, polymer composite product is with its light weight, electric insulation, corrosion-resistant, Yi Jia
Work, production efficiency is high, without the unique advantages such as spray treatment progressively substituted metal material.Therefore it is compound with heat-conducting polymer
The traditional aluminium alloy of material substitution, meets environmental protection and sustainable development requirement as LED illumination radiator shell.
As LED radiator shell, in addition to requiring material and there is high thermal conductivity, polymer composite energy is also required
The thermal shock for passing through more than 1000 hours at -40 DEG C ~ 120 DEG C is tested, and can be made into various colors to meet different Gus
The demand of visitor, good electrical insulating property is to eliminate consumer's electric shock hidden danger, and excellent halogen-free flameproof performance is to avoid LED electronics zero
Part causes fire hazard and poison gas dangerous when short circuit, current overload.
《The reply climate change development in science and technology ad hoc planning of " 12 " country》Clearly propose, to promote China to slow down and fit
Climate change technological innovation and application are answered, low-carbon economy development is supported, supported during " 12 " and the year two thousand twenty per GDP dioxy
Change the target of carbon emission.Therefore, the carbon emission of polymer composite is reduced as much as possible, meets national industrial policies requirement.
To ensure that heat-conductive composite material reaches certain thermal conductivity, it is necessary to add substantial amounts of heat filling, necessarily bring toughness of material tight
Decline again, proportion is increased substantially, variation is unfavorable for the negative effect such as processing to mobility rapidly.
The B of patent of invention CN 102408710 are using raw material systems such as nylon66 fiber, boron nitride, carborundum, aluminium nitride, aluminum oxide
For high heat conduction nylon 66 composite material, the B of patent of invention CN 102775767 are prepared using nylon 6, graphite powder, aluminum fiber etc.
The nylon 6 composite material of high heat conduction, patent of invention CN 103602060 A are led using nylon 6, fibrous heat filling, insulation
Hot powder, heat conduction abrasion-resistant powder etc. are prepared for heat conduction abrasion-proof insulating nylon 6 composite material, and the A of patent of invention CN 103613923 use Buddhist nun
Imperial resin, magnesia, aluminum oxide, aluminium nitride, boron nitride, silicon nitride, multi-walled carbon nanotube, natural graphite flakes, graphene particles
High heat conduction nylon composite materials are prepared for, the A of patent of invention CN 103483809 use nylon resin, heat filling magnesia, nitrogen
Change magnesium, ball-aluminium oxide, spherical aluminum oxide, aluminium nitride, boron nitride, pitch fibers, galapectite, CNT, graphite, carbonization
Silicon, boehmite etc., Non-halogen Flame Retardant Melamine-Quadrafos（MP）, melamine-polyphosphate（MP）, melamine
Amine-focusing phosphate, alkyl hypophosphites, alkyl metaphosphate, alkyl phosphite, APP（APP）, aluminium hydroxide,
Magnesium hydroxide, expanded graphites, epsom salt and molybdenum oxide etc. are prepared for high-fluidity polyamide base halogen-free flame-retarded heat-conducting and answered
Condensation material, patent of invention CN1926192A, as the filling-modified polyamide of fire retardant, is prepared for fire-retardant polyamides using phosphinic acids aluminium
Amine composite, patent of invention CN101157798A discloses a kind of imperial 6/ nano montmorillonite composite material of high whiteness super-dispersed nylon 6
High-efficiency and continuous polymerization, patent of invention ZL200910193532.0 discloses a kind of filling-modified heat conduction of inorganic heat filling
Electric-insulating polyphenyl thioether and polyamide blended alloy, patent of invention CN103087389A disclose a kind of high heat conduction high tenacity composite wood
Material and preparation method thereof, the patent mixes filling PET with granulated filler using graphite and prepares thermal conductivity
Up to 1.6 W/m K composite.
Above-mentioned technical proposal is blending type heat-conducting plastic technology, and use is all conventional nylon resin, above-mentioned skill
The characteristics of art scheme is to must be added to substantial amounts of inorganic heat filling, and this make it that the mobility and toughness of material are particularly poor.Flowing
Property difference cause to produce gas line during injection the problems such as whiten, poor toughness can make the position of bone bending displacement of final finished small, frangibility, no
Beneficial to assembling.Common elastic body toughening agent only can allow the mobility of material worse.Therefore the material obtained is in the grey system of making
Easily whiten during part, and cold-resistant thermal shock resistance properties is poor, and equipment is easily worn and torn.
The content of the invention
The purpose of the present invention is that there is provided a kind of Long carbon chain heat conduction nylon composite wood for above-mentioned deficiency of the prior art
Material, the material can pass through the thermal shock test of more than 1000 hours at -40 DEG C ~ 120 DEG C, low-gravity, low water absorption, high-ductility
Property, do not separate out, dimensionally stable, viscosity is relatively low, reduce equipment attrition, article surface does not whiten when particularly doing grey product.
Another goal of the invention of the present invention is to provide a kind of preparation method of Long carbon chain Heat conduction nylon composite material, and it has
Material blended characteristic is good, can improve the mobility and toughness of material, the characteristics of obtained quality of materials is high.
The purpose of the present invention is achieved through the following technical solutions：A kind of Long carbon chain Heat conduction nylon composite material, mainly includes
The raw material of following mass percent：
Long carbon chain nylon resin 20-40%
Heat filling 30-50%
Reinforcer 5-20%
Halogen-free flame retardants 5-20%
Coupling agent 0.1-0.5%
Lubricant 0.4-1.0%
Antioxidant 0.1-0.5%
Toner 0.1-5%；
The mass percent sum of above-mentioned raw materials is 100%.
Further, a kind of Long carbon chain Heat conduction nylon composite material, includes the raw material of following mass percent：
Long carbon chain nylon resin 20-30%
Heat filling 40-50%
Reinforcer 10-20%
Halogen-free flame retardants 10-20%
Coupling agent 0.3-0.5%
Lubricant 0.8-1.0%
Antioxidant 0.1-0.3%
Toner 0.2-4%.
Further, a kind of Long carbon chain Heat conduction nylon composite material, includes the raw material of following mass percent：
Long carbon chain nylon resin 30-40%
Heat filling 30-40%
Reinforcer 13-17%
Halogen-free flame retardants 15-20%
Coupling agent 0.2-0.4%
Lubricant 0.7-0.9%
Antioxidant 0.2-0.4%
Toner 0.2-4%.
This composite can also add appropriate toner, and preferably addition is 0.1-5%, and toner is matched colors according to needs
Species carries out ratio selection, and toner is black smoke, titanium dioxide, the mixture of nigrosine；
Wherein, the long carbon chain nylon resin is PA610, PA612, PA1010, PA1012, PA11, PA12 nylon resin
In one or more, relative viscosity is between 1.3 ~ 2.5.It is preferred that carbon chain range is 11 ~ 22 carbon.Long carbon chain nylon resin is comprehensive
Excellent performance is closed, compared with nylon 6, nylon66 fiber, its proportion is lower, water absorption rate is lower, toughness is more preferable, resistance to low temperature is more preferable,
The advantages of size is more stable, intensity is higher, more resistant, viscosity is relatively low.
It is preferred that, the relative viscosity of the long carbon chain nylon resin is 1.8,2.5 using mass ratio as 1:1 mixture.
Wherein, the heat filling is one or more of mixtures in boron nitride, magnesia, aluminum oxide.
Wherein, the reinforcer is one or more of mixtures in glass fibre, wollastonite, ZnOw.
It is preferred that, the reinforcer is made up of glass fibre and ZnOw, glass fibre and ZnOw
Mass ratio is 2:1.
Wherein, the halogen-free flame retardants is one in melamine cyanurate, magnesium hydroxide, aluminium hydroxide, Firebrake ZB
Plant or several mixtures.
It is preferred that, the halogen-free flame retardants is that inorganic compound fire retardant magnesium hydroxide, aluminium hydroxide and Firebrake ZB press matter
Amount is than being 5:5:The mixture of 1 ratio mixing.
It is preferred that, inorganic compound fire retardant is melamine cyanurate and magnesium hydroxide using mass ratio as 1:2 mixing
Mixture.
It is preferred that, the halogen-free flame retardants is inorganic compound fire retardant magnesium hydroxide, melamine cyanurate and boron
Sour zinc is 7 in mass ratio:3:The mixture of 1 ratio mixing.
Wherein, the coupling agent is silane coupling agent KH-550, is moulded in thermosetting and the thermoplasticity of glass fiber reinforcement
Used in material, bending strength, tensile strength and the interlayer that silane coupling agent KH-550 can be increased substantially under dry and wet state are cut
Shearing stress, and significantly improve hygrometric state electric property.When using this coupling agent in the case of dry and wet state, glass fiber reinforcement is answered
Condensation material rose before immersion with later flexural strength and tensile strength.
Wherein, the lubricant is mixture one or more of in ethylene acrylic acid co polymer ester type waxes, OP waxes.
It is preferred that, the lubricant is ethylene-acrylic acid copolymer and OP waxes using mass ratio as 1:The mixture of 2 mixing
Wherein, the antioxidant is N, N'- couples-(3- (3,5- di-tert-butyl-hydroxy phenyl) propiono) hexamethylene diamine.
Long carbon chain nylon commonly has superelevation elongation at break, by controlling molecular weight to synthesize the tree of different viscosities
Fat, the mobility and toughness of material can be lifted simultaneously, and long carbon chain nylon water absorption rate is low, and organic solvent-resistant is conducive to Injection moulded part
Dimensionally stable, will not cause after oil spout because of solvent cracking.Also, long carbon chain nylon can be biological Geordie dragon, be hindered with Halogen
Combustion agent makes the composite of the present invention have more low-carbon characteristic together.
A kind of preparation method of Long carbon chain Heat conduction nylon composite material of the present invention, mainly including following preparation process：
Step a. presses composition of raw materials mass percent, by long carbon chain nylon resin and coupling agent at 100-150 revs/min
Mixed 30-60 seconds in mixed cylinder under speed.
Step b. presses composition of raw materials mass percent, adds antioxidant, remixes 30-60 seconds.
Step c. presses composition of raw materials mass percent, adds heat filling, halogen-free flame retardants, lubricant, toner, then mix
Close 2-5 minutes.
Step d. melts at 160 DEG C -220 DEG C the compound in step c by meshing co rotating twin screw extrusion,
Mixing, extrusion；Meanwhile, reinforcer is fed in Section 6 gun barrel using side drawing-in device.
By the material strip extruded in step d through transmission belt is air-cooled, pelleter pelletizing, air knife dry, you can packaging.
The beneficial effects of the present invention are：LED lamp cup is poor fluidity with the maximum shortcoming of Heat Conduction Material, can cause injection
The problems such as whiting, gas line occurs in the parts surface processed, poor toughness, elongation at break is low, bending displacement is small.It is tough to solve
Property difference the problem of, conventional method be addition toughener, but addition toughener can make it that the mobility of material is worse.Usual PA6,
The viscosity of PA66 resins is between 2.0 ~ 3.0, and the viscosity of long carbon chain nylon resin is between 1.3 ~ 2.8, the lower flowing of viscosity
Property is better.Long carbon chain resin highest elongation at break is up to 350%, and the elongation at break highest 200% of PA6 resins, PA66
Highest 50%.Thus, mobility and tough sex chromosome mosaicism can be solved simultaneously using long carbon chain nylon resin, increased which overcome currently common
Tough dose can only improve toughness of material and can not be while improving the shortcoming of material flowability.
The present invention substitutes traditional nylon resin by using long carbon chain nylon, and overall technical scheme is matched somebody with somebody again
Close and improve, the normal direction thermal conductivity of obtained composite of the invention is in more than 1.0W/m K, and volume resistance is 1x1014-
1x1015 Ω cm, UL94 flame retardant rating are V2 grades of 0.8mm thickness, can pass through at -40 DEG C ~ 120 DEG C more than 1000 hours cold and hot
Shock-testing.Long carbon chain nylon resin used in the present invention can completely or partially use organism-based raw material castor oil, big
Soya-bean oil etc. is synthesized, and compared with petroleum base nylon, it is possible to decrease the consumption to petroleum resources, the emission reduction of carbon dioxide is realized, to environment
It is more friendly, it is new ep-type material.
The present invention another advantage is that：The preparation method of the present invention can improve the blended characteristic of various components, energy
Improve the mobility and toughness of material, the characteristics of obtained quality of materials is high.
Embodiment
For the ease of the understanding of those skilled in the art, with reference to embodiment, the present invention is further illustrated, real
The content that the mode of applying is referred to not limitation of the invention.
Embodiment 1
By composition of raw materials mass percent：Long carbon chain nylon resin 25.0%, heat filling 45%, reinforcer 10%, Halogen
Fire retardant 18%, coupling agent 0.4%, lubricant 1%, antioxidant 0.3%, toner 0.3%.By load weighted long carbon chain nylon resin and
Mixed 30 seconds in mixed cylinder of the coupling agent under 100 revs/min of speed, then add antioxidant, remix 30 seconds, add and lead
Hot filler, halogen-free flame retardants, lubricant, toner are remixed 3 minutes.The raw material mixed is passed through into intermeshing co rotating twin screw extrusion
Machine melting, mixing, extrusion, meanwhile, reinforcer is fed in Section 6 gun barrel using side drawing-in device.
The temperature control of double screw extruder is as follows：160 DEG C ~ 180 DEG C of first paragraph, 180 DEG C ~ 200 DEG C, the 3rd section of second segment
200 DEG C ~ 220 DEG C, the 4th section 200 DEG C ~ 220 DEG C, the 5th section 200 DEG C ~ 220 DEG C, the 6th section 180 DEG C ~ 200 DEG C, the 7th section 180 DEG C
~ 200 DEG C, the 8th section 180 DEG C ~ 200 DEG C, head and die temperature control are at 200 DEG C ~ 220 DEG C, 350 revs/min of screw speed,
Head pressure is 14 ~ 18MPa.The material strip of extrusion is through transmission belt is air-cooled, pelleter pelletizing, air knife are dried, and finally packs.
Wherein, the reinforcer is glass fibre；Color matching is that the toner of grey single selection is nigrosine and titanium dioxide, with matter
Amount is than being 1:The mixture of 2 mixing；The halogen-free flame retardants is inorganic compound fire retardant magnesium hydroxide, aluminium hydroxide and boric acid
Zinc is 5 in mass ratio:5:The mixture of 1 ratio mixing；The antioxidant is N, N'- couples-(3- (3,5- di-t-butyl -4- hydroxyls
Base phenyl) propiono) hexamethylene diamine；The relative viscosity of the long carbon chain nylon resin is 1.8；The coupling agent is γ-(2,3-
The oxygen of epoxy third) propyl trimethoxy silicane；The lubricant is ethylene-acrylic acid copolymer ester sodium.
Embodiment 2
By composition of raw materials mass percent：Long carbon chain nylon resin 30.0%, heat filling 40%, reinforcer 13%, Halogen
Fire retardant 15.5%, coupling agent 0.3%, lubricant 0.8%, antioxidant 0.2%, toner 0.2%.By load weighted long carbon chain nylon tree
Mixed 30 seconds in the mixed cylinder of fat and coupling agent under 100 revs/min of speed, then add antioxidant, remix 30 seconds, then added
Enter heat filling, halogen-free flame retardants, lubricant, toner to remix 3 minutes.The raw material mixed is passed through into intermeshing co-rotating twin-screw
Extruder melting, mixing, extrusion, meanwhile, reinforcer is fed in Section 6 gun barrel using side drawing-in device.
The temperature control of double screw extruder is as follows：160 DEG C ~ 180 DEG C of first paragraph, 180 DEG C ~ 200 DEG C, the 3rd section of second segment
200 DEG C ~ 220 DEG C, the 4th section 200 DEG C ~ 220 DEG C, the 5th section 200 DEG C ~ 220 DEG C, the 6th section 180 DEG C ~ 200 DEG C, the 7th section 180 DEG C
~ 200 DEG C, the 8th section 180 DEG C ~ 200 DEG C, head and die temperature control are at 200 DEG C ~ 220 DEG C, 350 revs/min of screw speed,
Head pressure is 14 ~ 18MPa.The material strip of extrusion is through transmission belt is air-cooled, pelleter pelletizing, air knife are dried, and finally packs.
Wherein, the reinforcer is made up of glass fibre and ZnOw, the matter of glass fibre and ZnOw
Amount is than being 2:1；The toner is selected according to the species for needing to match colors, and color matching is that the toner of grey single selection is black smoke and titanium
White powder is using mass ratio as 1:The mixture of 2 mixing；The halogen-free flame retardants is inorganic compound fire retardant, inorganic compound resistance
Combustion agent is MCA and magnesium hydroxide is using mass ratio as 1:The mixture of 2 mixing；The antioxidant is N, N'- couples-(3- (uncles of 3,5- bis-
Butyl -4- hydroxy phenyls) propiono) hexamethylene diamine；The relative viscosity of the long carbon chain nylon resin is 2.0；The coupling agent is
γ-(oxygen of 2,3- epoxies third) propyl trimethoxy silicane；The lubricant is ethylene-acrylic acid copolymer and OP waxes with quality
Than for 1:The mixture of 2 mixing.
Embodiment 3
By composition of raw materials mass percent：Long carbon chain nylon resin 33.7%, heat filling 35%, reinforcer 16%, Halogen
Fire retardant 14%, coupling agent 0.2%, lubricant 0.6%, antioxidant 0.4%, toner 0.1%.By load weighted long carbon chain nylon resin
Mixed 30 seconds with mixed cylinder of the coupling agent under 100 revs/min of speed, then add antioxidant, remix 30 seconds, add
Heat filling, halogen-free flame retardants, lubricant, toner are remixed 3 minutes.The raw material mixed is squeezed by intermeshing co-rotating twin-screw
Go out machine melting, mixing, extrusion, meanwhile, reinforcer is fed in Section 6 gun barrel using side drawing-in device.
The temperature control of double screw extruder is as follows：160 DEG C ~ 180 DEG C of first paragraph, 180 DEG C ~ 200 DEG C, the 3rd section of second segment
200 DEG C ~ 220 DEG C, the 4th section 200 DEG C ~ 220 DEG C, the 5th section 200 DEG C ~ 220 DEG C, the 6th section 180 DEG C ~ 200 DEG C, the 7th section 180 DEG C
~ 200 DEG C, the 8th section 180 DEG C ~ 200 DEG C, head and die temperature control are at 200 DEG C ~ 220 DEG C, 350 revs/min of screw speed,
Head pressure is 14 ~ 18MPa.The material strip of extrusion is through transmission belt is air-cooled, pelleter pelletizing, air knife are dried, and finally packs.
Wherein, the reinforcer is made up of wollastonite and ZnOw, the mass ratio of wollastonite and ZnOw
For 2:1；The toner is selected according to the species for needing to match colors, and the toner is black smoke, titanium dioxide, iron oxide red, phthalein green grass or young crops
The mixture of one or both of green, silver powder and pearl essence；Color matching is that the toner of red selection is iron oxide red；The nothing
Halogen fire retardant is inorganic compound fire retardant, and inorganic compound fire retardant is aluminium hydroxide；The antioxidant is N, N'- couples-(3-
(3,5- di-tert-butyl-hydroxy phenyls) propiono) hexamethylene diamine；The relative viscosity of the long carbon chain nylon resin is 1.8,2.5
Using mass ratio as 1:1 mixture；The coupling agent is γ-(oxygen of 2,3- epoxies third) propyl trimethoxy silicane；The lubrication
Agent is ethylene-acrylic acid copolymer.
Embodiment 4
By composition of raw materials mass percent：Long carbon chain nylon resin 20%, heat filling 50%, reinforcer 18.5%, Halogen
Fire retardant 10%, coupling agent 0.1%, lubricant 0.4%, antioxidant 0.5%, toner 0.5%.By load weighted long carbon chain nylon resin
Mixed 30 seconds with mixed cylinder of the coupling agent under 100 revs/min of speed, then add antioxidant, remix 30 seconds, add
Heat filling, halogen-free flame retardants, lubricant, toner are remixed 3 minutes.The raw material mixed is squeezed by intermeshing co-rotating twin-screw
Go out machine melting, mixing, extrusion, meanwhile, reinforcer is fed in Section 6 gun barrel using side drawing-in device.
The temperature control of double screw extruder is as follows：160 DEG C ~ 180 DEG C of first paragraph, 180 DEG C ~ 200 DEG C, the 3rd section of second segment
200 DEG C ~ 220 DEG C, the 4th section 200 DEG C ~ 220 DEG C, the 5th section 200 DEG C ~ 220 DEG C, the 6th section 180 DEG C ~ 200 DEG C, the 7th section 180 DEG C
~ 200 DEG C, the 8th section 180 DEG C ~ 200 DEG C, head and die temperature control are at 200 DEG C ~ 220 DEG C, 350 revs/min of screw speed,
Head pressure is 14 ~ 18MPa.The material strip of extrusion is through transmission belt is air-cooled, pelleter pelletizing, air knife are dried, and finally packs.
Wherein, the reinforcer is glass fibre, wollastonite, ZnOw using mass ratio as 1:1:1 ratio
Mixture；The toner is selected according to the species for needing to match colors, and color matching is that the toner of metallochrome selection is silver powder and pearl
Light powder is using mass ratio as 2:The mixture of 3 mixing；The halogen-free flame retardants be inorganic compound fire retardant magnesium hydroxide, MCA and
Firebrake ZB is 7 in mass ratio:3:The mixture of 1 ratio mixing；The antioxidant is N, N'- is double-(3- (3,5- di-t-butyls-
4- hydroxy phenyls) propiono) hexamethylene diamine；The relative viscosity of the long carbon chain nylon resin is 1.3；The coupling agent be γ-
(oxygen of 2,3- epoxies third) propyl trimethoxy silicane；The lubricant is ethylene-acrylic acid copolymer.
The material characteristic of novel nylon composite is as follows made from embodiments of the invention 1-4：
Performance test：
Proportion is tested by ASTM D792 plastic densities and relative density test method.
Water absorption rate is tested by the test method of ASTM D570 plastic ink absorption rates.
Bending displacement strengthens the test method survey with no reinforced plastics and electrically insulating material bending property by ASTM D790
Examination.
The standard test method that thermal conductivity determines solid conductive heat by ASTM E1461 flicker methods is tested.
Volume resistance is tested by ASTM D257 insulating materials D.C. resistances and conductivity test method.
Flame retardant rating is tested by UL94 plastic material combustion testing standards.
Thermal shock is tested：By material injection into LED lamp cup, place half an hour, then turned in 3 minutes at -40 DEG C
It is changed into placing half an hour at 120 DEG C, so circulation 1000 times.
Whiting test：By grey material injection into LED lamp cup, observation surface whether there is whiting.
Separate out and dimensional stability test：By the LED lamp cup of injection molding in 80 DEG C and the constant temperature and humidity of relative humidity 80%
Placed 720 hours in case, taking-up sees whether to exist and separated out and metaboly.
The normal direction thermal conductivity of nylon composite materials produced by the present invention is 1x1014- in more than 1.0W/m K, volume resistance
1x1015 Ω cm, UL94 flame retardant rating are V2 grades of 0.8mm thickness, can pass through at -40 DEG C ~ 120 DEG C more than 1000 hours cold and hot
Shock-testing, low-gravity, low water absorption, high tenacity is not separated out, and dimensionally stable, viscosity is relatively low, reduces equipment attrition, especially
It is that article surface does not whiten when doing grey product.Because the long carbon chain nylon such as PA610, PA1010, PA1012, PA11 resin can be with complete
Complete or part is using the synthesis such as organism-based raw material castor oil, soybean oil, compared with petroleum base nylon, it is possible to decrease to petroleum resources
Consumption, realize the emission reduction of carbon dioxide.
Above-described embodiment is the present invention preferably implementation, and in addition, the present invention can be realized with other manner,
Any obvious replacement is within protection scope of the present invention on the premise of not departing from present inventive concept.
Claims (6)
1. a kind of Long carbon chain Heat conduction nylon composite material, it is characterised in that：Mainly include the raw material of following mass percent：
Long carbon chain nylon resin 20-40%
Heat filling 30-50%
Reinforcer 5-20%
Halogen-free flame retardants 5-20%
Coupling agent 0.1-0.5%
Lubricant 0.4-1.0%
Antioxidant 0.1-0.5%
Toner 0.1-5%；
The mass percent sum of above-mentioned raw materials be 100%, wherein, the long carbon chain nylon resin be PA610, PA612,
One or more in PA1010, PA1012, PA11, PA12 nylon resin, relative viscosity is between 1.3 ~ 2.5；The enhancing
Filler is made up of wollastonite and ZnOw, and the heat filling is the one or more in boron nitride, magnesia, aluminum oxide
Mixture, the halogen-free flame retardants be at least one of metal hydroxides or melamine cyanurate, Firebrake ZB with
The mixture of metal hydroxides, the metal hydroxides is magnesium hydroxide and/or aluminium hydroxide.
2. a kind of Long carbon chain Heat conduction nylon composite material according to claim 1, it is characterised in that：Including following quality hundred
Divide the raw material of ratio：
Long carbon chain nylon resin 20-30%
Heat filling 40-50%
Reinforcer 10-20%
Halogen-free flame retardants 10-20%
Coupling agent 0.3-0.5%
Lubricant 0.8-1.0%
Antioxidant 0.1-0.3%
Toner 0.2-4%.
3. a kind of Long carbon chain Heat conduction nylon composite material according to claim 1, it is characterised in that：Including following quality hundred
Divide the raw material of ratio：
Long carbon chain nylon resin 30-40%
Heat filling 30-40%
Reinforcer 13-17%
Halogen-free flame retardants 15-20%
Coupling agent 0.2-0.4%
Lubricant 0.7-0.9%
Antioxidant 0.2-0.4%
Toner 0.2-4%.
4. a kind of Long carbon chain Heat conduction nylon composite material according to claim 1, it is characterised in that：The lubricant is second
One or more of mixture in allyl olefin(e) acid copolymer ester type waxes, OP waxes.
5. a kind of Long carbon chain Heat conduction nylon composite material according to claim 1, it is characterised in that：The coupling agent is silicon
Alkanes coupling agent KH-550；The antioxidant is N, N'- is double-(3- (3,5- di-tert-butyl-hydroxy phenyls) propiono) oneself two
Amine.
6. a kind of preparation method of Long carbon chain Heat conduction nylon composite material described in claim any one of 1-5, it is characterised in that：
Mainly include following preparation process：
Step a. presses composition of raw materials mass percent, by long carbon chain nylon resin and coupling agent in 100-150 revs/min of speed
Under mixed cylinder in mix 30-60 seconds；
Step b. presses composition of raw materials mass percent, adds antioxidant, remixes 30-60 seconds；
Step c. presses composition of raw materials mass percent, adds heat filling, halogen-free flame retardants, lubricant, toner, remixes 2-5
Minute；
Compound in step c melted at 160 DEG C -220 DEG C, kneaded by step d. by meshing co rotating twin screw extrusion,
Extrusion；Meanwhile, reinforcer is fed in Section 6 gun barrel using side drawing-in device.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102108204A (en) * | 2009-12-24 | 2011-06-29 | 合肥杰事杰新材料有限公司 | Plastic case material for breaker and preparation method thereof |
| CN103059565A (en) * | 2013-01-25 | 2013-04-24 | 本松工程塑料（杭州）有限公司 | Heat-conducting nylon composite material, preparation method and application thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2324734T3 (en) * | 2007-02-07 | 2009-08-13 | Ems-Chemie Ag | POLYAMIDE MOLDING COMPOUNDS FILLED WITH REDUCED WATER ABSORPTION. |
-
2015
- 2015-04-03 CN CN201510157303.9A patent/CN104744935B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102108204A (en) * | 2009-12-24 | 2011-06-29 | 合肥杰事杰新材料有限公司 | Plastic case material for breaker and preparation method thereof |
| CN103059565A (en) * | 2013-01-25 | 2013-04-24 | 本松工程塑料（杭州）有限公司 | Heat-conducting nylon composite material, preparation method and application thereof |
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