CN108659523A - A kind of highly-conductive hot carbon fiber PA6 composite material and preparation methods - Google Patents
A kind of highly-conductive hot carbon fiber PA6 composite material and preparation methods Download PDFInfo
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Abstract
The present invention relates to a kind of highly-conductive hot carbon fiber PA6 composite material and preparation methods.Group including following weight percent content is grouped as:PA6:15%‑45%;Carbon fiber:5%‑30%;Dispersant:1%‑3%;Phase solvent:1%‑3%;Thermal conducting agent:15%‑55%;Insulating heat-conductive powder:5%‑15%;Antioxidant:0.7%;Coupling agent:1%.The present invention is added to thermal conducting agent and insulating heat-conductive powder in the composite, and carbon fiber is modified, make carbon fiber that there is better intermiscibility with PA6, make finally obtained composite material that not only there is the good capacity of heat transmission, but also it is made to obtain superior mechanical property, the preparation method extruding pelletization of the present invention is once formed, preparation method is simple for process, easy to operate, high efficiency, it is at low cost, it is suitble to industrialized production.
Description
Technical field
The present invention relates to technical field of composite materials, and in particular to a kind of highly-conductive hot carbon fiber PA6 composite materials and its system
Preparation Method.
Background technology
Carbon fiber has many excellent performances, and the axial strength and modulus of carbon fiber are high, and density is low, higher than performance, without compacted
Become, superhigh temperature resistant under non-oxidizing atmosphere, fatigue durability is good, and specific heat and electric conductivity between metal, thermally expand system between nonmetallic
Number is small and has the features such as anisotropy, good corrosion resistance, X-ray transparent is good, has good electrical and thermal conductivity performance, electromagnetism
Shielding is good etc., has been widely used in space flight and aviation, new textile machinery, petrochemical industry, medicine instrument, automobile, machinery system
Make, building trade, stationery sports goods, telecommunications, the high-technology fields such as electrical heating.
Carbon fiber excellent in mechanical performance at present also essentially consists of carbon fiber research emphasis the power for how improving carbon fiber
Performance is learned, and for how to improve the heat conductivility of carbon fiber, and utilize its superior mechanical property high-new for heat conduction equipment
The research in field is but essentially blank.Although PA6 has superior comprehensive performance at present, in addition good insulating capacity and resistance toization
The property learned, application is very extensive, but its thermal conductivity but only has 0.30W/m.k, limits it in heat conduction, the application of field of radiating.
Invention content
In order to overcome the shortcomings of background technology, a kind of highly-conductive hot carbon fiber PA6 composite materials of present invention offer and its preparation
Method.
The technical solution adopted in the present invention is:A kind of highly-conductive hot carbon fiber PA6 composite materials, the composite material by with
The group of lower weight percent content is grouped as:
PA6:15%-45%;
Carbon fiber:5%-30%;
Dispersant:1%-3%;
Phase solvent:1%-3%;
Thermal conducting agent:15%-55%;
Insulating heat-conductive powder:5%-15%;
Antioxidant:0.7%;
Coupling agent:1%.
Wherein, the thermal conducting agent is graphite, described coupled to be connected in KH550.
Wherein, the carbon fiber is modified carbon fiber, and wherein the method for modifying of carbon fiber is to be immersed in carbon fiber to change
Property agent dilution in, and nitric acid is added in dilution, impregnates 1-2h, alcohol is then added, and be heated to handling at 120 DEG C
3h-5h。
Wherein, a concentration of 40%-60% of the nitric acid, the alcohol concentration are 30%-50%.
Wherein, the modifying agent is epoxy resin modification agent, and in dilution, the weight percent content of modifying agent is
30%-60%。
Wherein, diluent used in the dilution is one or two kinds of in water, methanol, formaldehyde;
The antioxidant is four [β-(3,5- di-t-butyl -4- hydroxy phenyls) propionic acid] pentaerythritol esters and/or three
[2.4- di-tert-butyl-phenyls] phosphite ester;
The coupling agent is amino triethoxysilane coupling agent and/or amino trimethoxysilane coupling agent.
Wherein, the insulating heat-conductive powder is silicon carbide or boron nitride.
A kind of preparation method of highly-conductive hot carbon fiber PA6 composite materials, includes the following steps:
(1)Graphite is added according to the ratio in the carbon fiber obtained through claim 4 modification, and coupling agent is added wherein,
Then 5h is handled at 150 DEG C, last kept dry obtains dry carbon fiber mixture;
(2)By above-mentioned steps(1)In obtained carbon fiber mixture be ground into powder;
(3)PA6, dispersant, phase solvent, insulating heat-conductive powder, antioxidant and coupling agent are mixed according to the ratio, obtain mixed material.
(4)Mixed material is placed in double screw extruder, meanwhile, the carbon fiber mixture that step 2 is obtained is according to the ratio
It is added in extruder, squeezes out, is granulated the highly-conductive hot carbon fiber PA6 composite materials described in obtaining.
Wherein, 220 DEG C -240 DEG C of one area's temperature of twin-screw, two area's temperature are 240 DEG C -250 DEG C, three area's temperature
250 DEG C -270 DEG C of degree, four 240 DEG C -250 DEG C of area's temperature, five 230 DEG C -240 DEG C of area's temperature, six 220 DEG C of area's temperature -
230 DEG C, seven 220 DEG C -230 DEG C of area's temperature, die head temperature is 250 DEG C, and extruded velocity is 200~230KG/H.
The beneficial effects of the invention are as follows:The present invention is added to thermal conducting agent and insulating heat-conductive powder in the composite, and to carbon
Fiber is modified, and carbon fiber is made to have better intermiscibility with PA6, and making finally obtained composite material not only has well
The capacity of heat transmission, and it is made to obtain superior mechanical property, preparation method extruding pelletization of the invention is once formed, preparation side
Method is simple for process, easy to operate, and high efficiency is at low cost, is suitble to industrialized production.
Specific implementation mode
Embodiment 1:A kind of highly-conductive hot carbon fiber PA6 composite materials, the composite material is by following weight percent content
Group be grouped as:
PA6: 39%;
Carbon fiber: 30%;
Dispersant:2%;
Phase solvent:2%;
Thermal conducting agent:15%;
Insulating heat-conductive powder:10.3%;
Antioxidant:0.7%;
Coupling agent:1%.
Wherein, the thermal conducting agent is graphite, described coupled to be connected in KH550.
Wherein, the carbon fiber is modified carbon fiber, and wherein the method for modifying of carbon fiber is to be immersed in carbon fiber to change
Property agent dilution in, and nitric acid is added in dilution, impregnates 2h, alcohol is then added, and be heated to handling at 120 DEG C
5h。
Wherein, a concentration of the 60% of the nitric acid, the alcohol concentration are 50%.
Wherein, the modifying agent is epoxy resin modification agent, and in dilution, the weight percent content of modifying agent is
60%。
Wherein, diluent used in the dilution is methanol;
The antioxidant is four [β-(3,5- di-t-butyl -4- hydroxy phenyls) propionic acid] pentaerythritol esters;
The coupling agent is amino triethoxysilane coupling agent.
Wherein, the insulating heat-conductive powder is boron nitride.
A kind of preparation method of highly-conductive hot carbon fiber PA6 composite materials, includes the following steps:
(1)Graphite is added according to the ratio in the carbon fiber obtained through claim 4 modification, and coupling agent is added wherein,
Then 5h is handled at 150 DEG C, last kept dry obtains dry carbon fiber mixture;
(2)By above-mentioned steps(1)In obtained carbon fiber mixture be ground into powder;
(3)PA6, dispersant, phase solvent, insulating heat-conductive powder, antioxidant and coupling agent are mixed according to the ratio, obtain mixed material.
(4)Mixed material is placed in double screw extruder, meanwhile, the carbon fiber mixture that step 2 is obtained is according to the ratio
It is added in extruder, squeezes out, is granulated the highly-conductive hot carbon fiber PA6 composite materials described in obtaining.
Wherein, one 220 DEG C DEG C of area's temperature of twin-screw, two area's temperature are 240 DEG C, three 250 DEG C of area's temperature, four
240 DEG C of area's temperature, five 240 DEG C of area's temperature, six 230 DEG C of area's temperature, seven 220 DEG C of area's temperature, die head temperature are 250 DEG C, are squeezed
It is 200KG/H to go out speed.
Embodiment 2:
A kind of highly-conductive hot carbon fiber PA6 composite materials, the composite material are grouped as by the group of following weight percent content:
PA6: 34%;
Carbon fiber: 25%;
Dispersant:2%;
Phase solvent:2%;
Thermal conducting agent:25%;
Insulating heat-conductive powder:10.3%;
Antioxidant:0.7%;
Coupling agent:1%.
Wherein, the thermal conducting agent is graphite, described coupled to be connected in KH550.
Wherein, the carbon fiber is modified carbon fiber, and wherein the method for modifying of carbon fiber is to be immersed in carbon fiber to change
Property agent dilution in, and nitric acid is added in dilution, impregnates 2h, alcohol is then added, and be heated to handling at 120 DEG C
5h。
Wherein, a concentration of the 60% of the nitric acid, the alcohol concentration are 50%.
Wherein, the modifying agent is epoxy resin modification agent, and in dilution, the weight percent content of modifying agent is
60%。
Wherein, diluent used in the dilution is methanol;
The antioxidant is four [β-(3,5- di-t-butyl -4- hydroxy phenyls) propionic acid] pentaerythritol esters;
The coupling agent is amino triethoxysilane coupling agent.
Wherein, the insulating heat-conductive powder is boron nitride.
A kind of preparation method of highly-conductive hot carbon fiber PA6 composite materials, includes the following steps:
(1)Graphite is added according to the ratio in the carbon fiber obtained through claim 4 modification, and coupling agent is added wherein,
Then 5h is handled at 150 DEG C, last kept dry obtains dry carbon fiber mixture;
(2)By above-mentioned steps(1)In obtained carbon fiber mixture be ground into powder;
(3)PA6, dispersant, phase solvent, insulating heat-conductive powder, antioxidant and coupling agent are mixed according to the ratio, obtain mixed material.
(4)Mixed material is placed in double screw extruder, meanwhile, the carbon fiber mixture that step 2 is obtained is according to the ratio
It is added in extruder, squeezes out, is granulated the highly-conductive hot carbon fiber PA6 composite materials described in obtaining.
Wherein, one 220 DEG C DEG C of area's temperature of twin-screw, two area's temperature are 240 DEG C, three 250 DEG C of area's temperature, four
240 DEG C of area's temperature, five 240 DEG C of area's temperature, six 230 DEG C of area's temperature, seven 220 DEG C of area's temperature, die head temperature are 250 DEG C, are squeezed
It is 200KG/H to go out speed.
Embodiment 3:
A kind of highly-conductive hot carbon fiber PA6 composite materials, the composite material are grouped as by the group of following weight percent content:
PA6: 29%;
Carbon fiber: 20%;
Dispersant:2%;
Phase solvent:2%;
Thermal conducting agent:35%;
Insulating heat-conductive powder:10.3%;
Antioxidant:0.7%;
Coupling agent:1%.
Wherein, the thermal conducting agent is graphite, described coupled to be connected in KH550.
Wherein, the carbon fiber is modified carbon fiber, and wherein the method for modifying of carbon fiber is to be immersed in carbon fiber to change
Property agent dilution in, and nitric acid is added in dilution, impregnates 2h, alcohol is then added, and be heated to handling at 120 DEG C
5h。
Wherein, a concentration of the 60% of the nitric acid, the alcohol concentration are 50%.
Wherein, the modifying agent is epoxy resin modification agent, and in dilution, the weight percent content of modifying agent is
60%。
Wherein, diluent used in the dilution is methanol;
The antioxidant is four [β-(3,5- di-t-butyl -4- hydroxy phenyls) propionic acid] pentaerythritol esters;
The coupling agent is amino triethoxysilane coupling agent.
Wherein, the insulating heat-conductive powder is boron nitride.
A kind of preparation method of highly-conductive hot carbon fiber PA6 composite materials, includes the following steps:
(1)Graphite is added according to the ratio in the carbon fiber obtained through claim 4 modification, and coupling agent is added wherein,
Then 5h is handled at 150 DEG C, last kept dry obtains dry carbon fiber mixture;
(2)By above-mentioned steps(1)In obtained carbon fiber mixture be ground into powder;
(3)PA6, dispersant, phase solvent, insulating heat-conductive powder, antioxidant and coupling agent are mixed according to the ratio, obtain mixed material.
(4)Mixed material is placed in double screw extruder, meanwhile, the carbon fiber mixture that step 2 is obtained is according to the ratio
It is added in extruder, squeezes out, is granulated the highly-conductive hot carbon fiber PA6 composite materials described in obtaining.
Wherein, one 220 DEG C DEG C of area's temperature of twin-screw, two area's temperature are 240 DEG C, three 250 DEG C of area's temperature, four
240 DEG C of area's temperature, five 240 DEG C of area's temperature, six 230 DEG C of area's temperature, seven 220 DEG C of area's temperature, die head temperature are 250 DEG C, are squeezed
It is 200KG/H to go out speed.
Embodiment 4:
A kind of highly-conductive hot carbon fiber PA6 composite materials, the composite material are grouped as by the group of following weight percent content:
PA6: 24%;
Carbon fiber: 15%;
Dispersant:2%;
Phase solvent:2%;
Thermal conducting agent:45%;
Insulating heat-conductive powder:10.3%;
Antioxidant:0.7%;
Coupling agent:1%.
Wherein, the thermal conducting agent is graphite, described coupled to be connected in KH550.
Wherein, the carbon fiber is modified carbon fiber, and wherein the method for modifying of carbon fiber is to be immersed in carbon fiber to change
Property agent dilution in, and nitric acid is added in dilution, impregnates 2h, alcohol is then added, and be heated to handling at 120 DEG C
5h。
Wherein, a concentration of the 60% of the nitric acid, the alcohol concentration are 50%.
Wherein, the modifying agent is epoxy resin modification agent, and in dilution, the weight percent content of modifying agent is
60%。
Wherein, diluent used in the dilution is methanol;
The antioxidant is four [β-(3,5- di-t-butyl -4- hydroxy phenyls) propionic acid] pentaerythritol esters;
The coupling agent is amino triethoxysilane coupling agent.
Wherein, the insulating heat-conductive powder is boron nitride.
A kind of preparation method of highly-conductive hot carbon fiber PA6 composite materials, includes the following steps:
(1)Graphite is added according to the ratio in the carbon fiber obtained through claim 4 modification, and coupling agent is added wherein,
Then 5h is handled at 150 DEG C, last kept dry obtains dry carbon fiber mixture;
(2)By above-mentioned steps(1)In obtained carbon fiber mixture be ground into powder;
(3)PA6, dispersant, phase solvent, insulating heat-conductive powder, antioxidant and coupling agent are mixed according to the ratio, obtain mixed material.
(4)Mixed material is placed in double screw extruder, meanwhile, the carbon fiber mixture that step 2 is obtained is according to the ratio
It is added in extruder, squeezes out, is granulated the highly-conductive hot carbon fiber PA6 composite materials described in obtaining.
Wherein, one 220 DEG C DEG C of area's temperature of twin-screw, two area's temperature are 240 DEG C, three 250 DEG C of area's temperature, four
240 DEG C of area's temperature, five 240 DEG C of area's temperature, six 230 DEG C of area's temperature, seven 220 DEG C of area's temperature, die head temperature are 250 DEG C, are squeezed
It is 200KG/H to go out speed.
Embodiment 5:
A kind of highly-conductive hot carbon fiber PA6 composite materials, the composite material are grouped as by the group of following weight percent content:
PA6: 19%;
Carbon fiber: 15%;
Dispersant:2%;
Phase solvent:2%;
Thermal conducting agent:55%;
Insulating heat-conductive powder:5.3%;
Antioxidant:0.7%;
Coupling agent:1%.
Wherein, the thermal conducting agent is graphite, described coupled to be connected in KH550.
Wherein, the carbon fiber is modified carbon fiber, and wherein the method for modifying of carbon fiber is to be immersed in carbon fiber to change
Property agent dilution in, and nitric acid is added in dilution, impregnates 2h, alcohol is then added, and be heated to handling at 120 DEG C
5h。
Wherein, a concentration of the 60% of the nitric acid, the alcohol concentration are 50%.
Wherein, the modifying agent is epoxy resin modification agent, and in dilution, the weight percent content of modifying agent is
60%。
Wherein, diluent used in the dilution is methanol;
The antioxidant is four [β-(3,5- di-t-butyl -4- hydroxy phenyls) propionic acid] pentaerythritol esters;
The coupling agent is amino triethoxysilane coupling agent.
Wherein, the insulating heat-conductive powder is boron nitride.
A kind of preparation method of highly-conductive hot carbon fiber PA6 composite materials, includes the following steps:
(1)Graphite is added according to the ratio in the carbon fiber obtained through claim 4 modification, and coupling agent is added wherein,
Then 5h is handled at 150 DEG C, last kept dry obtains dry carbon fiber mixture;
(2)By above-mentioned steps(1)In obtained carbon fiber mixture be ground into powder;
(3)PA6, dispersant, phase solvent, insulating heat-conductive powder, antioxidant and coupling agent are mixed according to the ratio, obtain mixed material.
(4)Mixed material is placed in double screw extruder, meanwhile, the carbon fiber mixture that step 2 is obtained is according to the ratio
It is added in extruder, squeezes out, is granulated the highly-conductive hot carbon fiber PA6 composite materials described in obtaining.
Wherein, one 220 DEG C DEG C of area's temperature of twin-screw, two area's temperature are 240 DEG C, three 250 DEG C of area's temperature, four
240 DEG C of area's temperature, five 240 DEG C of area's temperature, six 230 DEG C of area's temperature, seven 220 DEG C of area's temperature, die head temperature are 250 DEG C, are squeezed
It is 200KG/H to go out speed.
Melt mass flow rate(g/10min) | Impact strength(KJ/M²) | Tensile strength(MPa) | Bending strength(MPa) | Thermal coefficient(W/m*k) | |
Embodiment 1 | 5.3 | 6.8 | 230 | 9886 | 0.98 |
Embodiment 2 | 3.2 | 7.2 | 220 | 8964 | 3.43 |
Embodiment 3 | 1.8 | 3.3 | 190 | 12680 | 4.76 |
Embodiment 4 | 0.7 | 1.9 | 150 | 8653 | 5.54 |
Embodiment 5 | 0.05 | 1.7 | 120 | 6023 | 7.63 |
In order to which data are more convincing, the experimental data in preparation method in embodiment 1-5 is used into unified standard,
Only the percentage of graphite, PA6, carbon fiber and insulating heat-conductive powder is adjusted, it was found from above-mentioned analysis of experimental data:
1, after graphite is added, obvious variation is will produce to melt mass flow rate, graphite reach 55% it
Afterwards, melt mass flow rate is essentially 0, the main reason is that graphite is organic filler, in rigidity, is added in polymer
Necessarily mobility is caused to decline;On the other hand, graphite has good lubricating action, and after nitric acid treatment, coupling agent is being added
Processing, allows to be coated well by PA6.
2, after the content increase of graphite, mechanical properties decrease is apparent, although wherein embodiment 1 is opposite with embodiment 2
Although shock resistance is risen, the main reason is that reducing the content of carbon fiber, certain impact resistance is increased
Energy(The influence that carbon fiber increases to shock resistance is more apparent).
3, addition graphite can effectively improve the thermal coefficient of composite material, when the degree of graphite reaches 55%, carbon
When the degree 15% of fiber, the thermal coefficient of composite material may be up to 7.63.But mechanical properties decrease is more apparent,
It can be applied to the industry that do not done to mechanical property requirements.
4, it is 3.43 to coefficient when the degree of 2 graphite of embodiment is 25%, not only has good
Heat conductivility, while there is good mechanical property.
The present invention is added to thermal conducting agent and insulating heat-conductive powder in the composite, and is modified to carbon fiber, makes carbon fiber
Dimension has better intermiscibility with PA6, so that finally obtained composite material is not only had the good capacity of heat transmission, but also it is made to obtain
Superior mechanical property is obtained, preparation method extruding pelletization of the invention is once formed, and preparation method is simple for process, operation side
Just, high efficiency, it is at low cost, it is suitble to industrialized production.
Every technical staff's notice:Although the present invention is described according to above-mentioned specific implementation mode, of the invention
Invention thought be not limited in the invention, any repacking with inventive concept will all be included in this patent protection of the patent right
In range.
Claims (10)
1. a kind of highly-conductive hot carbon fiber PA6 composite materials, it is characterised in that:The composite material is by following weight percent content
Group be grouped as:
PA6:15%-45%;
Carbon fiber:5%-30%;
Dispersant:1%-3%;
Phase solvent:1%-3%;
Thermal conducting agent:15%-55%;
Insulating heat-conductive powder:5%-15%;
Antioxidant:0.7%;
Coupling agent:1%.
2. a kind of highly-conductive hot carbon fiber PA6 composite materials according to claim 1, it is characterised in that:The thermal conducting agent
For graphite.
3. a kind of highly-conductive hot carbon fiber PA6 composite materials according to claim 1, it is characterised in that:It is described coupled to connect
For KH550.
4. a kind of highly-conductive hot carbon fiber PA6 composite materials according to claim 1, it is characterised in that:The carbon fiber
For modified carbon fiber, wherein the method for modifying of carbon fiber is that carbon fiber is immersed in the dilution of modifying agent, and in dilution
Middle addition nitric acid impregnates 1-2h, alcohol is then added, and be heated to handling 3h-5h at 120 DEG C.
5. a kind of highly-conductive hot carbon fiber PA6 composite materials according to claim 4, it is characterised in that:The nitric acid
A concentration of 40%-60%, the alcohol concentration are 30%-50%.
6. a kind of highly-conductive hot carbon fiber PA6 composite materials according to claim 4 or 5, it is characterised in that:The modification
Agent is epoxy resin modification agent, and in dilution, the weight percent content of modifying agent is 30%-60%.
7. a kind of highly-conductive hot carbon fiber PA6 composite materials according to claim 6, it is characterised in that:The dilution
Used in diluent be water, methanol, it is one or two kinds of in formaldehyde;
The antioxidant is four [β-(3,5- di-t-butyl -4- hydroxy phenyls) propionic acid] pentaerythritol esters and/or three
[2.4- di-tert-butyl-phenyls] phosphite ester;
The coupling agent is amino triethoxysilane coupling agent and/or amino trimethoxysilane coupling agent.
8. a kind of highly-conductive hot carbon fiber PA6 composite materials according to claim 1, it is characterised in that:The insulation is led
Hot powder is silicon carbide or boron nitride.
9. a kind of preparation method of highly-conductive hot carbon fiber PA6 composite materials, it is characterised in that:Include the following steps:
(1)Graphite is added according to the ratio in the carbon fiber obtained through claim 4 modification, and coupling agent is added wherein,
Then 5h is handled at 150 DEG C, last kept dry obtains dry carbon fiber mixture;
(2)By above-mentioned steps(1)In obtained carbon fiber mixture be ground into powder;
(3)PA6, dispersant, phase solvent, insulating heat-conductive powder, antioxidant and coupling agent are mixed according to the ratio, obtain mixed material;
(4)Mixed material is placed in double screw extruder, meanwhile, the carbon fiber mixture that step 2 obtains is added according to the ratio
Into extruder, squeezes out, is granulated the highly-conductive hot carbon fiber PA6 composite materials described in obtaining.
10. a kind of preparation method of highly-conductive hot carbon fiber PA6 composite materials according to claim 9, it is characterised in that:Institute
220 DEG C -240 DEG C of the one area's temperature of twin-screw stated, two area's temperature are 240 DEG C -250 DEG C, three 250 DEG C -270 DEG C of area's temperature,
Four 240 DEG C -250 DEG C of area's temperature, five 230 DEG C -240 DEG C of area's temperature, six 220 DEG C -230 DEG C of area's temperature, seven area's temperature
220 DEG C -230 DEG C, die head temperature is 250 DEG C, and extruded velocity is 200~230KG/H.
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