CN109897284A - A kind of carbon nanotube and silicon nitride composite modified polypropylene composite material and preparation method and application - Google Patents
A kind of carbon nanotube and silicon nitride composite modified polypropylene composite material and preparation method and application Download PDFInfo
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- CN109897284A CN109897284A CN201910267130.4A CN201910267130A CN109897284A CN 109897284 A CN109897284 A CN 109897284A CN 201910267130 A CN201910267130 A CN 201910267130A CN 109897284 A CN109897284 A CN 109897284A
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Abstract
The invention discloses a kind of carbon nanotube and silicon nitride composite modified polypropylene composite material and preparation method and applications.The carbon nanotube of carboxyl-functional is prepared first, then it combines the carbon nanotube of carboxyl-functional and silicon nitride to obtain carbon nanotube/silicon nitride composite material of multidimensional network shape using the hydrogen bond physical action between carboxyl and silicon nitride, and carbon nanotube/silicon nitride composite material is modified by ethyl acrylate, then it being carried out with polypropylene to mixing internally mix, carbon nanotube and silicon nitride composite modified polypropylene composite material can be obtained.Its Young's modulus, tensile strength and thermal conductivity coefficient with higher.When being used as the component materials of heat exchanger, it is remarkably improved the heat exchange efficiency of heat exchanger.
Description
Technical field
The invention belongs to technical field of polymer materials, and in particular to a kind of carbon nanotube and silicon nitride composite modified poly- third
Alkene composite material and preparation method and application.
Background technique
Polypropylene (PP) is one of maximum general-purpose plastics of current dosage, is widely used in chemical industry, mechanical, automobile,
The every field such as daily necessities.Although PP has excellent mechanical performance, his tensile strength is lower and impact strength vulnerable to
The influence of temperature, and heating conduction is poor, is not able to satisfy heat exchange material when being applied to heat exchange material for heat transfer
The requirement of coefficient.
Summary of the invention
The purpose of the present invention is to provide a kind of carbon nanotube and silicon nitride composite modified polypropylene composite material and its systems
Preparation Method and application.Polypropylene is carried out by carbon nanotube and silicon nitride it is composite modified, obtain with higher mechanical strength and
The modified polypropylene composite material of the coefficient of heat transfer.
The technical scheme adopted by the invention is as follows:
A kind of preparation method of carbon nanotube and silicon nitride composite modified polypropylene composite material, comprising the following steps:
(1) carbon nanotube of carboxyl-functional and nitridation pasc reaction are generated into carbon nanotube/silicon nitride composite material；
(2) carbon nanotube/silicon nitride composite material is coupled with silane coupling agent, obtains being coated with silane coupling agent
Carbon nanotube/silicon nitride composite material；
(3) carbon nanotube/silicon nitride composite material for being coated with silane coupling agent for obtaining step (2) and acrylic acid second
After ester and initiator mixing, in 70~90 DEG C of 24~36h of ball milling；Product after water and ethanol washing, is dried in vacuo respectively
Obtain the modified carbon nanotube/silicon nitride composite material of ethyl acrylate；
(4) carbon nanotube/silicon nitride composite material and polypropylene that the ethyl acrylate for obtaining step (3) is modified are simultaneously
Be added in mixer, 170~190 DEG C of 3~6min of internally mix, then proceed to be added antioxidant, lubricant continue internally mix 7~
Carbon nanotube and silicon nitride composite modified polypropylene can be obtained in 10min.
Further, the carboxyl function carbon nano tube the preparation method comprises the following steps: carbon nanotube is dispersed in concentrated nitric acid,
30~50min of ultrasound, then 100~120 DEG C of 2~3h of heating reflux reaction, after water and ethanol washing, then are dispersed in dense
In sulfuric acid, 30~50min of ultrasound, then 100~120 DEG C of 2~3h of heating reflux reaction, through water and ethanol washing, vacuum drying
After carboxyl function carbon nano tube can be obtained.
Further, the mass fraction of the concentrated nitric acid is 68%, and the mass fraction of the concentrated sulfuric acid is 75~85%.
The carbon nanotube is preferably single-walled carbon nanotube, and single-walled carbon nanotube thermal coefficient with higher is thermally conductive
Property is significantly better than multi-walled carbon nanotube.
Further, the step (1) is specifically includes the following steps: by the carbon nanotube of carboxyl-functional, silicon nitride point
It is dispersed in methanol solvate, after being uniformly dispersed, 16~20h of back flow reaction under heating condition, through centrifugation, washing, dry after natural cooling
It is dry, carbon nanotube/silicon nitride composite material can be obtained.
Further, the carbon nanotube of the carboxyl-functional, the mass ratio of silicon nitride are 1:3~6；The carboxyl function
The carbon nanotube of energyization is 0.5~1.0mg/mL relative to the concentration of methanol.
The step (2) is specifically includes the following steps: be dispersed in 75~85% for carbon nanotube/silicon nitride composite material
In ethanol water, silane coupling agent is then added, is stirred to react 15~20h, product is dried in vacuo after ethanol washing
Obtain the carbon nanotube/silicon nitride composite material for being coated with silane coupling agent.
The quality of the silane coupling agent is carbon nanotube/silicon nitride composite material quality 1.5~2.0%；The carbon
Nanotube/silicon nitride composite material is 0.1~0.5g/mL relative to the concentration of ethanol water；The silane coupling agent is
KH560 or KH570.
In step (3), the carbon nanotube/silicon nitride composite material for being coated with silane coupling agent, draws ethyl acrylate
The mass ratio for sending out agent is 1:0.1~0.15:0.03~0.05.
In step (4), the modified carbon nanotube/silicon nitride composite material quality of the ethyl acrylate is polypropylene matter
The 10~20% of amount.Although composite wood can be improved in the modified carbon nanotube/silicon nitride composite material addition of ethyl acrylate
The thermal coefficient and mechanical strength of material, but adding the more mechanical strength that will lead to PP composite material reduces, therefore, this
Its additive amount is limited in 10~20% by invention.
In step (4), the antioxidant is antioxidant 1010, antioxidant 1076, antioxidant 300, antioxidant 1790, antioxygen
One of agent 1290 is a variety of；The lubricant is calcium stearate, EBO or polypropylene wax；The matter of the antioxidant, lubricant
Amount is the 0.5~1.0% of polypropylene quality.
The present invention also provides the carbon nanotubes and silicon nitride that are prepared according to above-mentioned preparation method composite modified poly- third
Alkene composite material.
The present invention also provides the carbon nanotubes and silicon nitride composite modified polypropylene composite material as heat exchange equipment
The application of material.
In carbon nanotube provided by the invention and the preparation method of silicon nitride composite modified polypropylene composite material, make first
The carbon nanotube of standby carboxyl-functional, then using the hydrogen bond physical action between carboxyl and silicon nitride by the carbon of carboxyl-functional
Nanotube and silicon nitride combine to obtain carbon nanotube/silicon nitride composite material.Carbon nanotube is to be batched to be formed by graphite
The one-dimensional tubulose carbon material of nanoscale, the excellent properties high with intensity, modulus is high, thermal coefficient is high；And silicon nitride is six
Prismatic crystal system is in hexahedron structure, and has excellent thermal conduction characteristic, by keeping carbon nanotube and silicon nitride logical after heating reaction
The bridging for crossing hydrogen bond forms the reticular structure of multidimensional, and after it is with polypropylene composite materials, this reticular structure can enhance compound
The mechanical strength of material, and enable heat cracking by composite material, and then refer to the thermal conductivity of composite material.
Carbon nanotube/silicon nitride composite material and the compatibility of polypropylene direct combination are poor, in order to increase carbon nanotube/
Silicon nitride composite material and polyacrylic compatibility, change carbon nanotube/silicon nitride composite material by ethyl acrylate
Property, after modified, the two can be preferably compatible, and the polypropylene through carbon nanotube/silicon nitride composite material after modified relatively changes
Young's modulus with higher, tensile strength and thermal conductivity coefficient before property.When being used as the component materials of heat exchanger, it can show
Write the heat exchange efficiency for improving heat exchanger.
Specific embodiment
The following describes the present invention in detail with reference to examples.
Embodiment 1
A kind of preparation method of carbon nanotube and silicon nitride composite modified polypropylene composite material, comprising the following steps:
(1) single-walled carbon nanotube is dispersed in 68% concentrated nitric acid, single-walled carbon nanotube is relative to the concentration of concentrated nitric acid
10mg/mL, ultrasonic 30min, then 120 DEG C of heating reflux reaction 2h, after water and ethanol washing, then are dispersed in 75%
In the concentrated sulfuric acid, single-walled carbon nanotube is 10mg/mL, ultrasonic 40min relative to the concentration of the concentrated sulfuric acid, is then heated to reflux for 120 DEG C
2h is reacted, carboxyl function carbon nano tube can be obtained after water and ethanol washing, vacuum drying；
The carbon nanotube of carboxyl-functional, silicon nitride are dispersed in methanol solvate, the carbon nanotube of carboxyl-functional, nitrogen
The mass ratio of SiClx is 1:3, and the carbon nanotube of carboxyl-functional is 0.6mg/mL relative to the concentration of methanol, is uniformly dispersed
Afterwards, carbon nanotube/nitridation can be obtained through centrifugation, washing, drying after natural cooling in back flow reaction 20h under 65 DEG C of heating conditions
Silicon composite；
(2) carbon nanotube/silicon nitride composite material is dispersed in 75% ethanol water, is then added silane coupled
Agent KH560, the quality of silane coupling agent are carbon nanotube/silicon nitride composite material quality 1.5%；Carbon nanotube/the nitrogen
SiClx composite material is 0.2g/mL relative to the concentration of ethanol water；It is stirred to react 20h, product vacuum after the pure washing of second
It is dry, the carbon nanotube/silicon nitride composite material for being coated with silane coupling agent can be obtained；
(3) carbon nanotube/silicon nitride composite material for being coated with silane coupling agent for obtaining step (2) and acrylic acid second
After ester and initiator are mixed according to mass ratio 1:0.1:0.03, in 70 DEG C of ball milling 36h, product is respectively after water, ethanol washing, very
Sky is dry, and the modified carbon nanotube/silicon nitride composite material of ethyl acrylate can be obtained；
(4) carbon nanotube/silicon nitride composite material and polypropylene that the ethyl acrylate for obtaining step (3) is modified are simultaneously
It is added in mixer, the modified carbon nanotube/silicon nitride composite material quality of ethyl acrylate is polyacrylic quality
10%, 170 DEG C of internally mix 6min, then proceed to antioxidant 1010 is added, calcium stearate continues internally mix 10min, antioxidant 1010, hard
The quality of resin acid calcium is the 0.5% of polypropylene quality, and carbon nanotube and silicon nitride composite modified polypropylene composite wood can be obtained
Material.
Embodiment 2
A kind of preparation method of carbon nanotube and silicon nitride composite modified polypropylene composite material, comprising the following steps:
(1) single-walled carbon nanotube is dispersed in 68% concentrated nitric acid, single-walled carbon nanotube is relative to the concentration of concentrated nitric acid
10mg/mL, ultrasonic 30min, then 100 DEG C of heating reflux reaction 3h, after water and ethanol washing, then are dispersed in 80%
In the concentrated sulfuric acid, single-walled carbon nanotube is 10mg/mL, ultrasonic 30min relative to the concentration of the concentrated sulfuric acid, is then heated to reflux for 100 DEG C
3h is reacted, carboxyl function carbon nano tube can be obtained after water and ethanol washing, vacuum drying；
The carbon nanotube of carboxyl-functional, silicon nitride are dispersed in methanol solvate, the carbon nanotube of carboxyl-functional, nitrogen
The mass ratio of SiClx is 1:5, and the carbon nanotube of carboxyl-functional is 0.8mg/mL relative to the concentration of methanol, is uniformly dispersed
Afterwards, carbon nanotube/nitridation can be obtained through centrifugation, washing, drying after natural cooling in back flow reaction 16h under 70 DEG C of heating conditions
Silicon composite；
(2) carbon nanotube/silicon nitride composite material is dispersed in 80% ethanol water, is then added silane coupled
Agent KH570, the quality of silane coupling agent are carbon nanotube/silicon nitride composite material quality 1.8%；Carbon nanotube/the nitrogen
SiClx composite material is 0.3g/mL relative to the concentration of ethanol water；It is stirred to react 17h, product vacuum after the pure washing of second
It is dry, the carbon nanotube/silicon nitride composite material for being coated with silane coupling agent can be obtained；
(3) carbon nanotube/silicon nitride composite material for being coated with silane coupling agent for obtaining step (2) and acrylic acid second
After ester and initiator are mixed according to mass ratio 1:0.12:0.04, in 80 DEG C of ball milling 30h, product respectively after water, ethanol washing,
Modified carbon nanotube/the silicon nitride composite material of ethyl acrylate can be obtained in vacuum drying；
(4) carbon nanotube/silicon nitride composite material and polypropylene that the ethyl acrylate for obtaining step (3) is modified are simultaneously
It is added in mixer, the modified carbon nanotube/silicon nitride composite material quality of ethyl acrylate is polyacrylic quality
15%, 180 DEG C of internally mix 5min then proceed to that antioxidant 1790, EBO continuation internally mix 8min, the matter of antioxidant 1790, EBO is added
Amount is the 0.8% of polypropylene quality, and carbon nanotube and silicon nitride composite modified polypropylene composite material can be obtained.
Embodiment 3
A kind of preparation method of carbon nanotube and silicon nitride composite modified polypropylene composite material, comprising the following steps:
(1) single-walled carbon nanotube is dispersed in 68% concentrated nitric acid, single-walled carbon nanotube is relative to the concentration of concentrated nitric acid
10mg/mL, ultrasonic 50min, then 110 DEG C of heating reflux reaction 2.5h, after water and ethanol washing, then are dispersed in 85%
The concentrated sulfuric acid in, single-walled carbon nanotube relative to the concentrated sulfuric acid concentration be 10mg/mL, ultrasonic 30min, then heat back for 110 DEG C
Stream reaction 2.5h, can be obtained carboxyl function carbon nano tube after water and ethanol washing, vacuum drying；
The carbon nanotube of carboxyl-functional, silicon nitride are dispersed in methanol solvate, the carbon nanotube of carboxyl-functional, nitrogen
The mass ratio of SiClx is 1:6；The carbon nanotube of the carboxyl-functional is 1.0mg/mL relative to the concentration of methanol, and dispersion is equal
After even, carbon nanotube/nitrogen is can be obtained through centrifugation, washing, drying after natural cooling in back flow reaction 16h under 70 DEG C of heating conditions
SiClx composite material；
(2) carbon nanotube/silicon nitride composite material is dispersed in 85% ethanol water, is then added silane coupled
Agent KH570, the quality of silane coupling agent are carbon nanotube/silicon nitride composite material quality 2.0%；Carbon nanotube/the nitrogen
SiClx composite material is 0.5g/mL relative to the concentration of ethanol water；It is stirred to react 20h, product vacuum after the pure washing of second
It is dry, the carbon nanotube/silicon nitride composite material for being coated with silane coupling agent can be obtained；
(3) carbon nanotube/silicon nitride composite material for being coated with silane coupling agent for obtaining step (2) and acrylic acid second
After ester and initiator are mixed according to mass ratio 1:0.15:0.05,90 DEG C of ball millings for 24 hours, product respectively after water, ethanol washing,
Modified carbon nanotube/the silicon nitride composite material of ethyl acrylate can be obtained in vacuum drying；
(4) carbon nanotube/silicon nitride composite material and polypropylene that the ethyl acrylate for obtaining step (3) is modified are simultaneously
It is added in mixer, the modified carbon nanotube/silicon nitride composite material quality of ethyl acrylate is polyacrylic quality
20%, 190 DEG C of internally mix 3min then proceed to that antioxidant 1290, polypropylene wax continuation internally mix 10min is added, and antioxidant 1290 gathers
The quality of propylene wax is the 1.0% of polypropylene quality, and carbon nanotube and silicon nitride composite modified polypropylene composite wood can be obtained
Material.
Comparative example 1
A kind of preparation method of polypropylene material, comprising the following steps: add carbon nanotube, silicon nitride, polypropylene simultaneously
Enter into mixer, carbon nanotube, the mass ratio of silicon nitride are 1:3, and carbon nanotube+silicon nitride quality sum is polypropylene
Quality 10%, 170 DEG C of internally mix 6min, then proceed to be added antioxidant, lubricant continue internally mix 10min, modification can be obtained
PP composite material.
Comparative example 2
Other are only omitted step (2) and step (3) with embodiment 1, and the carbon nanotube for directly obtaining step (1)/
Silicon nitride composite material mixes internally mix with polypropylene according to the step (4) in embodiment 1.
Comparative example 3
Other are with embodiment 1, the only modified carbon nanotube/silicon nitride composite material of ethyl acrylate in step (4)
Quality is polyacrylic quality 5%.
Comparative example 4
Other are with embodiment 1, the only modified carbon nanotube/silicon nitride composite material of ethyl acrylate in step (4)
Quality is polyacrylic quality 25%.
The composite wood that each embodiment and comparative example are obtained using compression molding instrument and mold under 190 DEG C and 15.0MPa
Material carries out hot pressing 10min, tests sample, the results are shown in Table 1.
Table 1
| Tensile strength (MPa) | Young's modulus (MPa) | Thermal coefficient (W/mK) | |
| Embodiment 1 | 39.7 | 1550 | 3.1 |
| Embodiment 2 | 32.7 | 1532 | 3.3 |
| Embodiment 3 | 30.4 | 1528 | 3.6 |
| Comparative example 1 | 20.3 | 1231 | 1.8 |
| Comparative example 2 | 25.9 | 1368 | 2.0 |
| Comparative example 3 | 27.1 | 1426 | 2.8 |
| Comparative example 4 | 22.4 | 1209 | 3.9 |
As can be seen that carbon nanotube and silicon nitride composite modified polypropylene that the present invention is prepared are multiple from above-mentioned table 1
Condensation material have good mechanical performance and thermal coefficient, therefore can conventionally be prepared into flat pipes of heat exchanger, fin, on
Next part plate, upper lower chamber, side plate, each component of constrictor, and it is conventionally assembled into heat exchanger, heat exchanger can be promoted
Heat exchange efficiency compares the heat exchanger that the component of pure PP machine-shaping assembles, and heat exchanger effectiveness of the invention is opposite to be mentioned
It is high by 45% or more.
Above-mentioned reference embodiment is to a kind of carbon nanotube and silicon nitride composite modified polypropylene composite material and its preparation side
The detailed description that method and application carry out, is illustrative without being restrictive, can enumerate several according to limited range
Embodiment, therefore the change and modification in the case where not departing from present general inventive concept, should belong within protection scope of the present invention.
Claims (10)
1. the preparation method of a kind of carbon nanotube and silicon nitride composite modified polypropylene composite material, which is characterized in that including with
Lower step:
(1) carbon nanotube of carboxyl-functional and nitridation pasc reaction are generated into carbon nanotube/silicon nitride composite material；
(2) carbon nanotube/silicon nitride composite material is coupled with silane coupling agent, obtains the carbon for being coated with silane coupling agent
Nanotube/silicon nitride composite material；
(3) carbon nanotube/silicon nitride composite material for being coated with silane coupling agent for obtaining step (2) and ethyl acrylate and
After initiator mixing, in 70~90 DEG C of 24~36h of ball milling；Respectively after water and ethanol washing, vacuum drying can be obtained product
Modified carbon nanotube/the silicon nitride composite material of ethyl acrylate；
(4) the modified carbon nanotube/silicon nitride composite material of the ethyl acrylate that step (3) obtains is added simultaneously with polypropylene
Into mixer, 170~190 DEG C of 3~6min of internally mix then proceed to that antioxidant, lubricant continuation 7~10min of internally mix is added, i.e.,
Carbon nanotube and silicon nitride composite modified polypropylene can be obtained.
2. preparation method according to claim 1, which is characterized in that the step (1) is specifically includes the following steps: by carboxylic
The carbon nanotube of base functionalization, silicon nitride are dispersed in methanol solvate, after being uniformly dispersed, back flow reaction 16 under heating condition~
Carbon nanotube/silicon nitride composite material can be obtained through centrifugation, washing, drying after natural cooling in 20h.
3. preparation method according to claim 2, which is characterized in that the carbon nanotube of the carboxyl-functional, silicon nitride
Mass ratio be 1:3~6；The carbon nanotube of the carboxyl-functional is 0.5~1.0mg/mL relative to the concentration of methanol.
4. preparation method according to claim 1 or 2, which is characterized in that the step (2) specifically includes the following steps:
Carbon nanotube/silicon nitride composite material is dispersed in 75~85% ethanol water, silane coupling agent is then added, is stirred
15~20h is reacted, product is dried in vacuo after ethanol washing, and the carbon nanotube/nitridation for being coated with silane coupling agent can be obtained
Silicon composite.
5. the preparation method according to claim 4, which is characterized in that the quality of the silane coupling agent be carbon nanotube/
The 1.5~2.0% of silicon nitride composite material quality；Carbon nanotube/the silicon nitride composite material is relative to ethanol water
Concentration is 0.1~0.5g/mL；The silane coupling agent is KH560 or KH570.
6. preparation method according to claim 1 or 2, which is characterized in that in step (3), it is described be coated with it is silane coupled
Carbon nanotube/silicon nitride composite material of agent, ethyl acrylate, initiator mass ratio be 1:0.1~0.15:0.03~
0.05。
7. preparation method according to claim 1 or 2, which is characterized in that in step (4), the ethyl acrylate is modified
Carbon nanotube/silicon nitride composite material quality be polyacrylic quality 10~20%.
8. preparation method according to claim 1 or 2, which is characterized in that in step (4), the antioxidant is antioxidant
1010, one of antioxidant 1076, antioxidant 300, antioxidant 1790, antioxidant 1290 or a variety of；The lubricant is hard
Resin acid calcium, EBO or polypropylene wax；The antioxidant, lubricant quality be polypropylene quality 0.5~1.0%.
9. the carbon nanotube and silicon nitride that preparation method according to any one of claims 1 to 8 is prepared are composite modified
PP composite material.
10. carbon nanotube and silicon nitride composite modified polypropylene composite material are as heat exchanger materials according to claim 9
Application.
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| CN104861298A (en) * | 2015-05-26 | 2015-08-26 | 西南大学 | Heat-conducting and insulated composite material based on carbon nanotubes and preparation method for composite material |
| CN106633369A (en) * | 2016-09-18 | 2017-05-10 | 中山大学 | Preparation method of bi-component modified glass fiber filled composite polypropylene material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101575096A (en) * | 2009-06-02 | 2009-11-11 | 桂林电子科技大学 | Method for preparing carbon nanotube grafted with vinyl macromolecular chain on the surface |
| CN101824238A (en) * | 2009-12-09 | 2010-09-08 | 广州市创至峰塑料制品科技有限公司 | Surface treatment method for powder composition of optical diffusion plastic |
| CN104861298A (en) * | 2015-05-26 | 2015-08-26 | 西南大学 | Heat-conducting and insulated composite material based on carbon nanotubes and preparation method for composite material |
| CN106633369A (en) * | 2016-09-18 | 2017-05-10 | 中山大学 | Preparation method of bi-component modified glass fiber filled composite polypropylene material |
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