CN102757640A - 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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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 the thermally conductive material technical field, particularly, relate to a kind of heat conduction nylon composite materials and preparation method thereof.
Background technology
Mostly conventional plastic is thermal insulation material, and the heat-conducting plastic of CoolPoly company exploitation brings new opportunity for this field.The commercial applications of CoolPoly company heat-conducting plastic starts from 1998; Having made about this product of product up to a million succeeds in a plurality of fields; Be widely used in various consumer electronics, power electronics, automobile, motorcycle, illumination, medical equipment and other apparatus etc.The CoolPoly heat-conducting plastic is a base material with engineering plastics and general-purpose plastics, like 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 approximately is 5-100 times of conventional plastic, and general thermal conductivity has only 0.2W/m-K.This conductivity is also worked as with some metallographic phase, is 15W/m-K like stainless thermal conductivity, and the thermal conductivity of some cast aluminium alloys is 50-100W/m-K.
Compare with traditional material, heat-conducting plastic has higher flexible resistance and tensile rigidity, but resistance to impact shock is relatively poor.Heat-conducting plastic mainly can be used for replacing some the product size to be had the metal or the ceramic objects of micromodule, optical module, mechanical component and the medical component of strict demand.When being base material, can be used as packing ring, vibroshock or contact material with the elastomerics.Heat-conducting plastic combines the simplification of plastic shaping with excellent heat conductivity, can realize some metal or the same thermal heat transfer capability of pottery through injection molding.Simultaneously, this type material can provide more design freedom for the tDesigners, and the weight of product has only the half the of aluminum products.Utilizing heat-conducting plastic processing can shortening shaping cycle 20% ~ 50% and its inherent low thermal coefficient of expansion can effectively reduce product shrinks.
Yet heat-conducting plastic is difficult to have concurrently simultaneously high with the excellent mechanical property of heat conductivility, is difficult to satisfy the use properties of actual needs, thereby has limited the widespread use of heat-conducting plastic.
Summary of the invention
In order to address the above problem, the invention provides a kind of heat conduction nylon composite materials and preparation method thereof, it has high heat-conducting property and excellent mechanical property, has promoted the widespread use of heat-conducting plastic.
Technical scheme of the present invention is following: a kind of heat conduction nylon composite materials comprises that the quality percentage composition of component and each component is following:
Said thermoplastic polymer is selected from a kind of in PA6, PA66, PA612, PA11, PA12, PA1010, PPA, PA46, PA6T, PA9T and the PA6/66 multipolymer or several compsn; Said compatilizer is maleic anhydride grafted ethene-1-octene copolymer (POE-g-MAH), maleic anhydride graft thermoplastic elastomer (TPE-g-MAH), maleic anhydride grafted ethene-propylene-dicyclopentadiene terpolymers (terpolymer EP rubber) one or more the mixture in (EPDM-g-MAH); Said high heat conducting fiber is carbon nanotube, thomel or the mixture of the two; Said high heat conductive filler is one or more the mixture in Graphene, nano aluminium oxide, aluminium nitride AlN, SP 1, silit, the flakey highly-conductive hot carbon powder; Said auxiliary agent comprises heatproof inhibitor, lubricant, nucleator, branching agent and chainextender.
The mass percent of following each component in said heat conduction nylon composite materials total amount is:
Said heatproof inhibitor is a Hinered phenols antioxidant, the mixture of one or more in phosphite ester kind antioxidant and the alkali metal halide.
Said lubricant is a calcium stearate, ethylene bis stearic acid amide, silicone powder or its arbitrary composition.
Said nucleator is selected from talcum powder.
Said branching agent chemical structural formula is:
Wherein, R is aromatic series segment, aliphatics segment or alicyclic segment, amino, carboxyl, epoxy group(ing) or the hydroxy functional group of R ' for reacting with the nylon end group, R ' number of functional groups >=3.
Said branching agent is one or more the mixture in three carboxyl Phenylsulfonic acids, triaminotriphenyl-methane or the trihydroxy-propylene oxide.
Said chainextender is selected from one or more the mixture in BASF ADR-4370, Brueggemann M1251, the maleic anhydride graft nylon 6.
The preparation method of said heat-conductive composite material comprises following concrete steps:
Steps A: by prescription weighing nylon, compatilizer, high heat conducting fiber, high heat conductive filler and auxiliary agent; With thermoplastic polymer, the compatilizer of weighing, high heat conducting fiber and auxiliary agent drop into low speed mixer, splash into dispersed oil after, mixed 5～10 minutes;
Step B: high heat conductive filler is added the low speed mixer, mixed 5～10 minutes, get the blend material;
Step C: with step B) gained blend material drops into the TE-75 twin screw extruder, behind the mixing, melt extrudes, and temperature is being 170 ℃～285 ℃, and rotating speed is 200～400r/min;
Step D) cooling back pelletizing screening;
Step e) packing.
Compare with prior art, the present invention has following advantage:
1) effect through branching agent; It is netted that the matrix resin molecular structure is changed into by the straight chain shape, promoted the products machinery performance greatly, because unique star-branched agent is to the effect of molecular structure; Molecule is the roller motion in the material plasticizing process; The matrix resin flowability significantly promotes, and the dispersion of heat conducting fiber and heat-conducting filler is had remarkable effect, helps the stability of modification and injection moulding processing.
2) the present invention introduces chainextender; Adding proportion control through chainextender; It is slightly crosslinked to have realized that material has occurred in modifying process, and carries out the crosslinked effect of the degree of depth in the injection moulding course of processing in later stage, can make material directly change thermoset articles into by thermoplastic material; Improved the physical and mechanical properties of goods greatly, thereby solved because heat conduction composition high filler loading capacity influences too big problem to material property.
3) heat conduction nylon composite materials according to the invention, material is cheap and easy to get, and it has high heat-conducting property 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 materials comprises that the quality percentage composition of component and each component is following:
Said nylon is selected from PA6; Said compatilizer is maleic anhydride grafted ethene-1-octene copolymer (POE-g-MAH); Said high heat conducting fiber is a thomel; Said high heat conductive filler is the mixture of Graphene and nano aluminium oxide; Said auxiliary agent comprises heatproof inhibitor, lubricant, nucleator, branching agent and chainextender.The mass percent of each component of said auxiliary agent in said heat conduction nylon composite materials total amount is:
Said heatproof inhibitor is the mixture of Hinered phenols antioxidant and cupric chloride.
Said lubricant is a calcium stearate.
Said nucleator is a talcum powder.
Said branching agent chemical structural formula is:
Wherein, R is aromatic series segment, aliphatics segment or alicyclic segment, amino, carboxyl, epoxy group(ing) or the hydroxy functional group of R ' for reacting with the nylon end group, R ' number of functional groups >=3.Said branching agent is three carboxyl Phenylsulfonic acids.
Said chainextender is the mixture of BASF ADR-4370 and Brueggemann M1251.
Embodiment 2:
A kind of heat conduction nylon composite materials comprises that the quality percentage composition of component and each component is following:
Said nylon is selected from the mixture of PA6 and PA66; Said compatilizer is maleic anhydride graft thermoplastic elastomer (TPE-g-MAH) and maleic anhydride grafted ethene-propylene-dicyclopentadiene terpolymers (terpolymer EP rubber) mixture (EPDM-g-MAH); Said high heat conducting fiber is a carbon nanotube; Said high heat conductive filler is the mixture of aluminium nitride AlN and silit; Said auxiliary agent comprises heatproof inhibitor, lubricant, nucleator, branching agent and chainextender.
The mass percent of each component of said auxiliary agent in said heat conduction nylon composite materials total amount is:
Said heatproof inhibitor is a phosphite ester kind antioxidant.
Said lubricant is the mixture of ethylene bis stearic acid amide and silicone powder.
Said nucleator is selected from talcum powder.
Said branching agent is the mixture of triaminotriphenyl-methane and trihydroxy-propylene oxide.
Said chainextender is Brueggemann M1251.
Embodiment 3
A kind of heat conduction nylon composite materials comprises that the quality percentage composition of component and each component is following:
Said nylon is selected from the mixture of PA612 and PA1010; Said compatilizer be maleic anhydride grafted ethene-propylene-dicyclopentadiene terpolymers (terpolymer EP rubber) (EPDM-g-MAH); Said high heat conducting fiber is a thomel; Said high heat conductive filler is the mixture of SP 1 and flakey highly-conductive hot carbon powder; Said auxiliary agent comprises heatproof inhibitor, lubricant, nucleator, branching agent and chainextender.
The mass percent of each component of said auxiliary agent in said heat conduction nylon composite materials total amount is:
Said heatproof inhibitor is an alkali metal halide.
Said lubricant is the mixture of calcium stearate and ethylene bis stearic acid amide.
Said nucleator is selected from talcum powder.
Said branching agent is the trihydroxy-propylene oxide.
Said chainextender is the mixture of Brueggemann M1251 and maleic anhydride graft nylon 6.
Embodiment 4
A kind of heat conduction nylon composite materials comprises that the quality percentage composition of component and each component is following:
Said nylon is selected from the mixture of PA46 and PA9T; Said compatilizer is the mixture of maleic anhydride grafted ethene-1-octene copolymer (POE-g-MAH) and maleic anhydride graft thermoplastic elastomer (TPE-g-MAH); Said high heat conducting fiber is carbon nanotube, thomel or the mixture of the two; Said high heat conductive filler is the mixture of Graphene and flakey highly-conductive hot carbon powder; Said auxiliary agent comprises heatproof inhibitor, lubricant, nucleator, branching agent and chainextender.
The mass percent of following each component in said heat conduction nylon composite materials total amount is:
Said heatproof inhibitor is a phosphite ester kind antioxidant.
Said lubricant is an ethylene bis stearic acid amide.
Said nucleator is selected from talcum powder.
Said branching agent is the mixture of three carboxyl Phenylsulfonic acids and triaminotriphenyl-methane.
Said chainextender is BASF ADR-4370.
Embodiment 5
A kind of heat conduction nylon composite materials comprises that the quality percentage composition of component and each component is following:
Said nylon selects the mixture of PA46 and PA6; Said compatilizer is maleic anhydride graft thermoplastic elastomer (TPE-g-MAH); Said high heat conducting fiber is the mixture of carbon nanotube and thomel; Said high heat conductive filler is the mixture of nano aluminium oxide and SP 1 and silit; Said auxiliary agent comprises heatproof inhibitor, lubricant, nucleator, branching agent and chainextender.
The mass percent of following each component in said heat conduction nylon composite materials total amount is:
Said heatproof inhibitor is a Hinered phenols antioxidant.
Said lubricant is the mixture of calcium stearate and silicone powder.
Said nucleator is selected from talcum powder.
Said branching agent triaminotriphenyl-methane.
Said chainextender is the mixture of BASF ADR-4370 and maleic anhydride graft nylon 6.
Embodiment 6
A kind of heat conduction nylon composite materials comprises that the quality percentage composition of component and each component is following:
Said nylon is selected from the PA6/66 multipolymer; Said compatilizer is maleic anhydride grafted ethene-1-octene copolymer (POE-g-MAH); Said high heat conducting fiber is a carbon nanotube; Said high heat conductive filler is SP 1 and flakey highly-conductive hot carbon powder; Said auxiliary agent comprises heatproof inhibitor, lubricant, nucleator, branching agent and chainextender.
The mass percent of following each component in said heat conduction nylon composite materials total amount is:
Heatproof inhibitor 3%;
Said heatproof inhibitor is the mixture of phosphite ester kind antioxidant and alkali metal halide.
Said lubricant is the mixture of calcium stearate and silicone powder.
Said nucleator is selected from talcum powder.
Said branching agent is the mixture of three carboxyl Phenylsulfonic acids, triaminotriphenyl-methane and trihydroxy-propylene oxide.
Said chainextender is Brueggemann M1251, BASF ADR-4370 and maleic anhydride graft nylon 6 threes' a mixture.
Embodiment 7
The preparation method of the said heat conduction nylon composite materials of embodiment 1-6 comprises following concrete steps:
Steps A: by prescription weighing nylon, compatilizer, high heat conducting fiber, high heat conductive filler and auxiliary agent; With thermoplastic polymer, the compatilizer of weighing, high heat conducting fiber and auxiliary agent drop into low speed mixer, splash into dispersed oil after, mixed 5～10 minutes;
Step B: high heat conductive filler is added the low speed mixer, mixed 5～10 minutes, get the blend material;
Step C: with step B) gained blend material drops into the TE-75 twin screw extruder, behind the mixing, melt extrudes, and temperature is being 170 ℃～285 ℃, and rotating speed is 200～400r/min;
Step D) cooling back pelletizing screening;
Step e) packing.
In order to further specify the performance of heat conduction nylon composite materials according to the invention, the applicant has carried out Performance Detection to implementing 7 prepared heat-conductive composite materials, and test item and result are as shown in table 1.
The Performance Detection of the said heat conduction nylon composite materials of 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 to combine concrete preferred implementation to the further explain that the present invention did, and can not assert that practical implementation of the present invention is confined to these explanations.For the those of ordinary skill of technical field under the present invention, under the prerequisite that does not break away from the present invention's design, its framework form can be flexible and changeable, can the subseries product.Just make some simple deduction or replace, all should be regarded as belonging to the scope of patent protection that the present invention is confirmed by claims of being submitted to.
Claims (8)
1. a heat conduction nylon composite materials is characterized in that, comprises that the quality percentage composition of component and each component is following:
Said thermoplastic polymer is selected from a kind of in PA6, PA66, PA612, PA11, PA12, PA1010, PPA, PA46, PA6T, PA9T and the PA6/66 multipolymer or several compsn; Said compatilizer is maleic anhydride grafted ethene-1-octene copolymer (POE-g-MAH), maleic anhydride graft thermoplastic elastomer (TPE-g-MAH), maleic anhydride grafted ethene-propylene-dicyclopentadiene terpolymers (terpolymer EP rubber) one or more the mixture in (EPDM-g-MAH); Said high heat conducting fiber is carbon nanotube, thomel or the mixture of the two; Said high heat conductive filler is one or more the mixture in Graphene, nano aluminium oxide, aluminium nitride AlN, SP 1, silit, the flakey highly-conductive hot carbon powder; Said auxiliary agent comprises heatproof inhibitor, lubricant, nucleator, branching agent and chainextender.
2. heat conduction nylon composite materials as claimed in claim 1 is characterized in that, the mass percent of following each component in said heat-conductive composite material total amount is:
3. heat-conductive composite material as claimed in claim 1 is characterized in that, said heatproof inhibitor is a Hinered phenols antioxidant, the mixture of one or more in phosphite ester kind antioxidant and the alkali metal halide.
4. heat-conductive composite material as claimed in claim 1 is characterized in that, said lubricant is a calcium stearate, ethylene bis stearic acid amide, silicone powder or its arbitrary composition.
5. heat-conductive composite material as claimed in claim 1 is characterized in that said nucleator is selected from talcum powder.
6. heat-conductive composite material as claimed in claim 1 is characterized in that, said 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 the nylon end group, and R ' number of functional groups >=3.
7. heat-conductive composite material as claimed in claim 1 is characterized in that, said chainextender is selected from one or more the mixture in BASF ADR-4370, Brueggemann M1251, the maleic anhydride graft nylon 6.
8. like the preparation method of each described heat-conductive composite material of claim 1-7, it is characterized in that, comprise following concrete steps:
Steps A: by prescription weighing thermoplastic polymer, compatilizer, high heat conducting fiber, high heat conductive filler and auxiliary agent; With thermoplastic polymer, the compatilizer of weighing, high heat conducting fiber and auxiliary agent drop into low speed mixer, splash into dispersed oil after, mixed 5～10 minutes;
Step B: high heat conductive filler is added the low speed mixer, mixed 5～10 minutes, get the blend material;
Step C: with step B) gained blend material drops into the TE-75 twin screw extruder, behind the mixing, melt extrudes, and temperature is being 170 ℃～285 ℃, and rotating speed is 200～400r/min;
Step D) cooling back pelletizing screening;
Step e) packing.
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Address after: Room 312, ITT plant, No.5, Gongye North 4th Road, Songshanhu high tech Industrial Development Zone, Dongguan City, Guangdong Province Patentee after: Chendong Yipuwan New Materials (Guangdong) Co., Ltd. Address before: Park Songshan Lake Science and Technology Industrial Park in the northern industrial city of Guangdong Province, 523000 small enterprises of science and technology of Dongguan city building 4 Dongguan epone nylon Polytron Technologies Inc Patentee before: Dongguan Epone Nylon Sci & Tech Co., Ltd. |