CN102757640B - Heat conduction nylon composite material and preparation method thereof - Google Patents
Heat conduction nylon composite material and preparation method thereof Download PDFInfo
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- CN102757640B CN102757640B CN201210260475.5A CN201210260475A CN102757640B CN 102757640 B CN102757640 B CN 102757640B CN 201210260475 A CN201210260475 A CN 201210260475A CN 102757640 B CN102757640 B CN 102757640B
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Abstract
The invention provides a heat conduction nylon composite material and a preparation method thereof. The heat conduction nylon composite material comprises the following components by mass: 20-60 percent of nylon, 3-10 percent of a compatilizer, 5-10 percent of high thermal conductivity fiber, 30-50 percent of a high thermal conductivity filling material and 0.5-16 percent of assistants. The heat conduction nylon composite material has the advantages as follows: through the addition proportion control of a branching agent and a chain extendor, the effect that slight crosslinking occurs in the modification process of the material and deep crosslinking is conducted in the processing process of injection moulding in a later period is achieved, so that the material is directly changed from a thermoplastic material into a thermoset product, and the physical and mechanical properties of the product are greatly improved, so as to solve the problem of over large impact on the physical properties of the product caused by high filling amount of heat conduction ingredients.
Description
Technical field
The present invention relates to thermally conductive material technical field, particularly, relate to a kind of Heat conduction nylon composite material and preparation method thereof.
Background technology
Traditional plastics mostly are thermal insulation material, and the heat-conducting plastic of CoolPoly company exploitation is that new opportunity is brought in this field.The commercial applications of CoolPoly company heat-conducting plastic starts from 1998, manufacture about this product of product up to a million to succeed in multiple field, be widely used in various consumer electronics, power electronics, automobile, motorcycle, illumination, medical equipment and other apparatus etc.CoolPoly heat-conducting plastic with engineering plastics and general-purpose plastics for base material, as PP, ABS, PC, PA, LCP, PPS, PEEK etc.Typical heat-conducting plastic thermal conductivity scope is 1-20W/m-K, and some grade can reach 100W/m-K.This numerical value is approximately 5-100 times of conventional plastic, and general thermal conductivity only has 0.2W/m-K.This conductivity is also worked as with some metallographic phase, and if stainless thermal conductivity is 15W/m-K, the thermal conductivity of some cast aluminium alloys is 50-100W/m-K.
Compared with traditional material, heat-conducting plastic has higher flexible resistance and tensile rigidity, but resistance to impact shock is poor.Heat-conducting plastic mainly can be used for replacing some to have metal or the ceramic objects of the micromodule of strict demand, optical module, mechanical component and medical component to product size.When taking elastomerics as base material, can be used as packing ring, vibroshock or contact material.Heat-conducting plastic combines the simplification of plastic shaping with excellent heat conductivity, can realize some metal or pottery thermal heat transfer capability equally by injection molding.Meanwhile, this type material can provide more design freedom for Designers, and the weight of product only has the half of aluminum products.Utilize heat-conducting plastic process can shorten shaping cycle 20% ~ 50% and its intrinsic low thermal coefficient of expansion can effectively reduce product shrink.
But heat-conducting plastic is difficult to have the high and excellent mechanical property of heat conductivility concurrently, is difficult to the use properties meeting actual needs, thus limits the widespread use of heat-conducting plastic simultaneously.
Summary of the invention
In order to solve the problem, the invention provides a kind of Heat conduction nylon composite material and preparation method thereof, it has higher heat conductivility and excellent mechanical property, has promoted the widespread use of heat-conducting plastic.
Technical scheme of the present invention is as follows: a kind of Heat conduction nylon composite material, is made up of each component of following mass percentage:
Described thermoplastic polymer is selected from the composition of one or several in PA6, PA66, PA612, PA11, PA12, PA1010, PPA, PA46, PA6T, PA9T and PA6/66 multipolymer; Described compatilizer is one or more the mixture in maleic anhydride grafted ethene-1-octene copolymer (POE-g-MAH), Maleic Anhydride Grafted Thermoplastic Elastomer (TPE-g-MAH), maleic anhydride grafted ethene-propylene-dicyclopentadiene terpolymers (terpolymer EP rubber) (EPDM-g-MAH); Described high heat conducting fiber is carbon nanotube, carbon fiber or the mixture of the two; Described high heat conductive filler is one or more the mixture in Graphene, nano aluminium oxide, aluminium nitride, boron nitride, silicon carbide, flakey highly-conductive hot carbon powder; Described auxiliary agent comprises heatproof antiaging agent, lubricant, nucleator, branching agent and chainextender.
The mass percent of following ingredients in described Heat conduction nylon composite material total amount is:
Described heatproof antiaging agent is Hinered phenols antioxidant, one or more the mixture in phosphite ester kind antioxidant and alkali metal halide.
Described lubricant is calcium stearate, ethylene bis stearic acid amide, silicone powder or its arbitrary composition.
Described nucleator is selected from talcum powder.
Described branching agent chemical structural formula is:
Wherein, R is aromatic series segment, aliphatics segment or alicyclic segment, and R ' is amino, carboxyl, epoxy group(ing) or the hydroxy functional group that can react with nylon end group, R ' number of functional groups >=3.
Described branching agent is one or more the mixture in three carboxyl Phenylsulfonic acids, triaminotriphenyl-methane or trihydroxy-propylene oxide.
Described chainextender is selected from one or more the mixture in BASF ADR-4370, Brueggemann M1251, maleic anhydride graft nylon 6.
The preparation method of described heat-conductive composite material, comprises following concrete steps:
Steps A: weigh nylon by formula, compatilizer, high heat conducting fiber, high heat conductive filler and auxiliary agent; By the thermoplastic polymer, the compatilizer that weigh, high heat conducting fiber and auxiliary agent drop into low speed mixer, after instillation dispersed oil, mix 5 ~ 10 minutes;
Step B: high heat conductive filler is added low speed mixer, mixes 5 ~ 10 minutes, obtains blended material;
Step C: by step B) gained blended material input TE-75 twin screw extruder, after mixing, melt extrude, temperature is being 170 DEG C ~ 285 DEG C, and rotating speed is 200 ~ 400r/min;
Step D) the rear pelletizing screening of cooling;
Step e) packaging.
Compared with the existing technology, tool of the present invention has the following advantages:
1) by the effect of branching agent, matrix resin molecular structure can be made to be changed into by straight-chain netted, greatly improve products machinery performance, because the star-branched agent of uniqueness is to the effect of molecular structure, plasticize process Middle molecule is roller motion, matrix resin mobility significantly promotes, and has remarkable effect to the dispersion of heat conducting fiber and heat-conducting filler, is conducive to the stability of modification and injection molding.
2) the present invention introduces chainextender, controlled by the adding proportion of chainextender, achieve material has occurred slight crosslinked in modifying process, and the effect of deep-crosslinked is carried out in the injection moulding course of processing in later stage, material can be made directly to change thermoset articles into by thermoplastic material, substantially increase the physical and mechanical properties of goods, thus solve because heat conduction composition high filler loading capacity affects too large problem to material property.
3) Heat conduction nylon composite material of the present invention, material is cheap and easy to get, and it has higher heat conductivility and excellent mechanical property, has promoted the widespread use of heat-conducting plastic, and its preparation method is simple, is suitable for applying.
Embodiment
Embodiment 1:
A kind of Heat conduction nylon composite material, is made up of each component of following mass percentage:
Described nylon is selected from PA6; Described compatilizer is maleic anhydride grafted ethene-1-octene copolymer (POE-g-MAH); Described high heat conducting fiber is carbon fiber; Described high heat conductive filler is the mixture of Graphene and nano aluminium oxide; Described auxiliary agent comprises heatproof antiaging agent, lubricant, nucleator, branching agent and chainextender.The mass percent of each component of described auxiliary agent in described Heat conduction nylon composite material total amount is:
Described heatproof antiaging agent is the mixture of Hinered phenols antioxidant and cupric chloride.
Described lubricant is calcium stearate.
Described nucleator is talcum powder.
Described branching agent chemical structural formula is:
Wherein, R is aromatic series segment, aliphatics segment or alicyclic segment, and R ' is amino, carboxyl, epoxy group(ing) or the hydroxy functional group that can react with nylon end group, R ' number of functional groups >=3.Described branching agent is three carboxyl Phenylsulfonic acids.
Described chainextender is the mixture of BASF ADR-4370 and Brueggemann M1251.
Embodiment 2:
A kind of Heat conduction nylon composite material, is made up of each component of following mass percentage:
Described nylon is selected from the mixture of PA6 and PA66; Described compatilizer is the mixture of Maleic Anhydride Grafted Thermoplastic Elastomer (TPE-g-MAH) and maleic anhydride grafted ethene-propylene-dicyclopentadiene terpolymers (terpolymer EP rubber) (EPDM-g-MAH); Described high heat conducting fiber is carbon nanotube; Described high heat conductive filler is the mixture of aluminium nitride and silicon carbide; Described auxiliary agent comprises heatproof antiaging agent, lubricant, nucleator, branching agent and chainextender.
The mass percent of each component of described auxiliary agent in described Heat conduction nylon composite material total amount is:
Described heatproof antiaging agent is phosphite ester kind antioxidant.
Described lubricant is the mixture of ethylene bis stearic acid amide and silicone powder.
Described nucleator is selected from talcum powder.
Described branching agent is the mixture of triaminotriphenyl-methane and trihydroxy-propylene oxide.
Described chainextender is Brueggemann M1251.
Embodiment 3
A kind of Heat conduction nylon composite material, is made up of each component of following mass percentage:
Described nylon is selected from the mixture of PA612 and PA1010; Described compatilizer is maleic anhydride grafted ethene-propylene-dicyclopentadiene terpolymers (terpolymer EP rubber) (EPDM-g-MAH); Described high heat conducting fiber is carbon fiber; Described high heat conductive filler is the mixture of boron nitride and flakey highly-conductive hot carbon powder; Described auxiliary agent comprises heatproof antiaging agent, lubricant, nucleator, branching agent and chainextender.
The mass percent of each component of described auxiliary agent in described Heat conduction nylon composite material total amount is:
Described heatproof antiaging agent is alkali metal halide.
Described lubricant is the mixture of calcium stearate and ethylene bis stearic acid amide.
Described nucleator is selected from talcum powder.
Described branching agent is trihydroxy-propylene oxide.
Described chainextender is the mixture of Brueggemann M1251 and maleic anhydride graft nylon 6.
Embodiment 4
A kind of Heat conduction nylon composite material, is made up of each component of following mass percentage:
Described nylon is selected from the mixture of PA46 and PA9T; Described compatilizer is the mixture of maleic anhydride grafted ethene-1-octene copolymer (POE-g-MAH) and Maleic Anhydride Grafted Thermoplastic Elastomer (TPE-g-MAH); Described high heat conducting fiber is carbon nanotube, carbon fiber or the mixture of the two; Described high heat conductive filler is the mixture of Graphene and flakey highly-conductive hot carbon powder; Described auxiliary agent comprises heatproof antiaging agent, lubricant, nucleator, branching agent and chainextender.
The mass percent of following ingredients in described Heat conduction nylon composite material total amount is:
Described heatproof antiaging agent is phosphite ester kind antioxidant.
Described lubricant is ethylene bis stearic acid amide.
Described nucleator is selected from talcum powder.
Described branching agent is the mixture of three carboxyl Phenylsulfonic acids and triaminotriphenyl-methane.
Described chainextender is BASF ADR-4370.
Embodiment 5
A kind of Heat conduction nylon composite material, is made up of each component of following mass percentage:
Described nylon selects the mixture of PA46 and PA6; Described compatilizer is Maleic Anhydride Grafted Thermoplastic Elastomer (TPE-g-MAH); Described high heat conducting fiber is the mixture of carbon nanotube and carbon fiber; Described high heat conductive filler is the mixture of nano aluminium oxide and boron nitride and silicon carbide; Described auxiliary agent comprises heatproof antiaging agent, lubricant, nucleator, branching agent and chainextender.
The mass percent of following ingredients in described Heat conduction nylon composite material total amount is:
Described heatproof antiaging agent is Hinered phenols antioxidant.
Described lubricant is the mixture of calcium stearate and silicone powder.
Described nucleator is selected from talcum powder.
Described branching agent triaminotriphenyl-methane.
Described chainextender is the mixture of BASF ADR-4370 and maleic anhydride graft nylon 6.
Embodiment 6
A kind of Heat conduction nylon composite material, is made up of each component of following mass percentage:
Described nylon is selected from PA6/66 multipolymer; Described compatilizer is maleic anhydride grafted ethene-1-octene copolymer (POE-g-MAH); Described high heat conducting fiber is carbon nanotube; Described high heat conductive filler is boron nitride and flakey highly-conductive hot carbon powder; Described auxiliary agent comprises heatproof antiaging agent, lubricant, nucleator, branching agent and chainextender.
The mass percent of following ingredients in described Heat conduction nylon composite material total amount is:
Described heatproof antiaging agent is the mixture of phosphite ester kind antioxidant and alkali metal halide.
Described lubricant is the mixture of calcium stearate and silicone powder.
Described nucleator is selected from talcum powder.
Described branching agent is the mixture of three carboxyl Phenylsulfonic acids, triaminotriphenyl-methane and trihydroxy-propylene oxide.
Described chainextender is the mixture of Brueggemann M1251, BASF ADR-4370 and maleic anhydride graft nylon 6 three.
Embodiment 7
The preparation method of Heat conduction nylon composite material described in embodiment 1-6, comprises following concrete steps:
Steps A: weigh nylon by formula, compatilizer, high heat conducting fiber, high heat conductive filler and auxiliary agent; By the thermoplastic polymer, the compatilizer that weigh, high heat conducting fiber and auxiliary agent drop into low speed mixer, after instillation dispersed oil, mix 5 ~ 10 minutes;
Step B: high heat conductive filler is added low speed mixer, mixes 5 ~ 10 minutes, obtains blended material;
Step C: by step B) gained blended material input TE-75 twin screw extruder, after mixing, melt extrude, temperature is being 170 DEG C ~ 285 DEG C, and rotating speed is 200 ~ 400r/min;
Step D) the rear pelletizing screening of cooling;
Step e) packaging.
In order to further illustrate the performance of Heat conduction nylon composite material of the present invention, applicant has carried out Performance Detection to the heat-conductive composite material prepared by enforcement 7, test item and result as shown in table 1.
The Performance Detection of Heat conduction nylon composite material described in table 1 embodiment 1-6
| Thermally conductive material | Thermal conductivity (W/mk) | Tensile strength | Unnotched impact strength |
| Embodiment 1 | 2.2 | 90 | 5.5 |
| Embodiment 2 | 2.8 | 110 | 6.0 |
| Embodiment 3 | 2.7 | 110 | 6.5 |
| Embodiment 4 | 2.6 | 100 | 4.5 |
| Embodiment 5 | 2.3 | 90 | 5.0 |
| Embodiment 6 | 2.2 | 95 | 6.8 |
Above content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, its framework form can be flexible and changeable, can subseries product.Just make some simple deduction or replace, all should be considered as belonging to the scope of patent protection that the present invention is determined by submitted to claims.
Claims (8)
1. a Heat conduction nylon composite material, is characterized in that, is made up of each component of following mass percentage:
Described nylon is selected from the composition of one or several in PA6, PA66, PA612, PA11, PA12, PA1010, PA46, PA6T, PA9T and PA6/66 multipolymer; Described compatilizer is one or more the mixture in maleic anhydride grafted ethene-1-octene copolymer (POE-g-MAH), Maleic Anhydride Grafted Thermoplastic Elastomer (TPE-g-MAH), maleic anhydride grafted ethene-propylene-dicyclopentadiene terpolymers (terpolymer EP rubber) (EPDM-g-MAH); Described high heat conducting fiber is carbon nanotube, carbon fiber or the mixture of the two; Described high heat conductive filler is one or more the mixture in Graphene, nano aluminium oxide, aluminium nitride, boron nitride, silicon carbide, flakey highly-conductive hot carbon powder; Described auxiliary agent comprises heatproof antiaging agent, lubricant, nucleator, branching agent and chainextender.
2. Heat conduction nylon composite material as claimed in claim 1, it is characterized in that, the mass percent of following ingredients in described Heat conduction nylon composite material total amount is:
3. Heat conduction nylon composite material as claimed in claim 1, it is characterized in that, described heatproof antiaging agent is Hinered phenols antioxidant, one or more the mixture in phosphite ester kind antioxidant and alkali metal halide.
4. Heat conduction nylon composite material as claimed in claim 1, it is characterized in that, described lubricant is calcium stearate, ethylene bis stearic acid amide, silicone powder or its arbitrary composition.
5. Heat conduction nylon composite material as claimed in claim 1, it is characterized in that, described nucleator is selected from talcum powder.
6. Heat conduction nylon composite material as claimed in claim 1, it is characterized in that, described branching agent chemical structural formula is:
Wherein, R is aromatic series segment, aliphatics segment or alicyclic segment; Amino, carboxyl, hydroxyl or the epoxy group(ing) of R ' for reacting with nylon end group, and R ' number of functional groups >=3.
7. Heat conduction nylon composite material as claimed in claim 1, it is characterized in that, described chainextender is selected from one or more the mixture in BASF ADR-4370, Brueggemann M1251, maleic anhydride graft nylon 6.
8. the preparation method of the Heat conduction nylon composite material as described in any one of claim 1-7, is characterized in that, comprises following concrete steps:
Steps A: weigh nylon by formula, compatilizer, high heat conducting fiber, high heat conductive filler and auxiliary agent; By the thermoplastic polymer, the compatilizer that weigh, high heat conducting fiber and auxiliary agent drop into low speed mixer, after instillation dispersed oil, mix 5 ~ 10 minutes;
Step B: high heat conductive filler is added low speed mixer, mixes 5 ~ 10 minutes, obtains blended material;
Step C: by step B) gained blended material input TE-75 twin screw extruder, after mixing, melt extrude, temperature is being 170 DEG C ~ 285 DEG C, and rotating speed is 200 ~ 400r/min;
Step D) the rear pelletizing screening of cooling;
Step e) packaging.
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| CN201210260475.5A CN102757640B (en) | 2012-07-25 | 2012-07-25 | Heat conduction nylon composite material and preparation method thereof |
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