CN106189165B - A kind of preparation method of high heat conductive insulating hexagonal boron nitride/polycarbonate composite material - Google Patents
A kind of preparation method of high heat conductive insulating hexagonal boron nitride/polycarbonate composite material Download PDFInfo
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Abstract
The present invention is a kind of preparation method of high heat conductive insulating hexagonal boron nitride/polycarbonate composite material.This method comprises the following steps：Hexagonal boron nitride and distilled water are added in reactor, then cation polymethacrylamide solution is added dropwise, and stirring reaction, after miillpore filter filters, solid residue is dried, obtain cation polymethacrylamide modification hexagonal boron nitride, by its with makrolon the melt blending in torque rheometer, finally obtain high heat conductive insulating hexagonal boron nitride/polycarbonate composite material；The present invention is modified for non-covalent bond, and medium used is water in modified, green non-pollution, and whole modifying process is simple and easy, nontoxic, low for equipment requirements.
Description
Technical field：
The present invention relates to the preparation field of high-heat-conductive composite material, the specially surface of hexagonal boron nitride is modified, Yi Jiliu
The preparation method of square boron nitride/polycarbonate composite material.
Background technology：
With industry and the rapid development of technology, electronic equipment is just towards miniaturization, portability, highly integrated direction hair
Exhibition, heat, which dissipates, to be become can not be ignored.If heat can not be dissipated in time, service efficiency and the use of device certainly will be influenceed
Life-span.The features such as makrolon (Polycarbonate, PC) is because of its excellent electrical insulating property, mechanical performance, extensively should
Relatively low field of LED illumination is required for heat conduction, but pure PC heat conductivilitys are poor, limit it and require answering for field in high heat conduction
With.Therefore, on the premise of PC Good All-around Properties itself are ensured, improve its heat conductivility and caused in academic and engineering field
Extensive interest.
It is to prepare heat-conducting polymer material main stream approach at present that heat filling is added in resin matrix.It is existing at present a variety of
Filler is added in resin matrix, such as metal, graphite, CNT, aluminum oxide, but is answered using prepared by these fillers
Condensation material material has the shortcomings that electrical conductivity is too high or thermal conductivity is relatively low, can not meet the application in heat conductive insulating field.Six side's nitrogen
Change boron be it is a kind of there is high-termal conductivity, low-k, inorganic particulate resistant to chemical etching and inoxidizability, be to prepare
The ideal filler of high heat conduction, insulating polymer composite.Existing much study improves the heat of matrix by adding BN at present
Conductance.
Xie et al. handles boron nitride using 30% aqueous hydrogen peroxide solution in autoclave, then will be treated
Boron nitride, which adds, is made heat-conductive composite material in polyvinyl alcohol (PVA), treated boron nitride surface hydroxyl increases, with matrix
Interface bond strength increase, in 10wt% loadings, thermal conductivity reaches 3.92W/mK.(Xie B H,Huang X,Zhang G
J.High thermal conductive polyvinyl alcohol composites with hexagonal boron
nitride microplatelets as fillers.Compos Sci Technol 2013；85(9):98-103.).This article
Although offer realizes higher thermal conductivity under relatively low loading, the processing to BN is needed in strong hydrogen peroxide solution and high pressure
Carried out in kettle, it is not only dangerous, and do not have general applicability, it is higher to equipment requirement.
Increase wettability by first handling boron nitride with nitration mixture in dawn swallow et al., recycle diisocyanate to be modified and be made
Amidized boron nitride.Amidized boron nitride and base polyamide imines (PI) compatibility are more preferable, may participate in polyimides
Polymerisation in, play crosslinking points effect, in 30wt% loadings, thermal conductivity 0.5189W/mK.(CN
104892968A).This preparation method is modified boron nitride with nitration mixture and diisocyanate, not only dangerous, and two isocyanides
Acid esters toxicity is larger, does not meet the theory of Green Chemistry.
It is an object of the invention to provide a kind of side for preparing high heat conductive insulating hexagonal boron nitride/polycarbonate composite material
Method.Hexagonal boron nitride surface chemistry group is few, and reactivity is low, and matrix poor compatibility, if hexagonal boron nitride is without place
Reason is just added to resin matrix, and hexagonal boron nitride can not be disperseed well, and thermal conductivity improves relatively low.Therefore, to six side's nitrogen
Change the surface modification of boron, it is its emphasis and difficult point in field of compound material application to improve its dispersiveness with constructing thermal conducting path.
The invention provides a kind of non-covalent bond method of modifying of hexagonal boron nitride, make hexagonal boron nitride and mineral filler
Improved, constructed effective thermal conducting path, final composite heat conductivility, heat resistance significantly improves.
The content of the invention
The present invention is for deficiency present in current techniques, there is provided a kind of high heat conductive insulating hexagonal boron nitride/poly- carbonic acid
The preparation method of ester composite.This method is ultrasonically treated to the aqueous solution of hexagonal boron nitride first, is increased its surface and is born
Electrically, then mainly adsorbed using modifying agent cation polymethacrylamide by electrostatic interaction on hexagonal boron nitride surface,
The crystal structure of boron nitride is not interfered with.The present invention is modified for non-covalent bond, and medium used is water in modified, and green is without dirt
Dye, whole modifying process are simple and easy, nontoxic, low for equipment requirements.Modified hexagonal boron nitride can be in polycarbonate matrix
In align, form orientation texture, the heat conductivity and heat resistance finally given be obtained for large increase.
The technical scheme is that：
A kind of preparation method of high heat conductive insulating hexagonal boron nitride/polycarbonate composite material, this method include following step
Suddenly：
The first step：Hexagonal boron nitride and distilled water are added in reactor, it is mass ratio that it, which is matched, hexagonal boron nitride:
Distilled water=1:100~400,30~40h of ultrasonic disperse；
Second step：By the cation polymethacrylamide aqueous solution that mass fraction is 0.1~1%, the first step is added drop-wise to
In the solution of preparation, solution starts to be layered in dropwise addition, stops that cation polymethacrylamide is added dropwise when upper solution is clarified
Solution, continue 5~30min of stirring, obtain mixed liquor；
3rd step：The miillpore filter that above-mentioned mixed liquor is passed through filters, and then does solid residue at 35~50 DEG C
Dry 20~24h, the hexagonal boron nitride of cation polymethacrylamide modification is obtained, is designated as m-BN；
4th step：Hexagonal boron nitride (m-BN) and makrolon melt blending in torque rheometer will be modified, m-BN's
Mass fraction is 5~20%；Melt blending temperature is 230~250 DEG C, and rotor speed be 30~50rpm, the blending time for 6~
10min；Finally obtain high heat conductive insulating hexagonal boron nitride/polycarbonate composite material.
Ultrasound condition in the described first step is：100kW, 25~60 DEG C.
Cation polymethacrylamide in described second step is acrylyl oxy-ethyl-trimethyl salmiac and methyl
The copolymer of acrylamide；The mol ratio of the two is acrylyl oxy-ethyl-trimethyl salmiac：Methacrylamide=1:1~4.
Described hexagonal boron nitride be industrial goods high-purity micron order hexagonal boron nitride, 3~5 μm of piece footpath, purity ＞
99.0%.
The aperture of described miillpore filter is 0.15~0.45 μm.
The present invention substantive distinguishing features be：
In current techniques, the method for modifying to hexagonal boron nitride is mostly covalent bond chemical modification, not only dangerous poisonous, yield
It is low, and it is possible to destroy the crystal structure of hexagonal boron nitride, and hexagonal boron nitride perfection of crystal is to thermal conductivity in future
Influence is very big, if crystal structure is destroyed, thermal conductivity will improve little.Increase as Hou Jun et al. handles boron nitride by nitration mixture
Surface hydroxyl, then grafted silane coupling agent be modified hexagonal boron nitride (Hou J.Preparation and
Characterization of Surface Modified Boron Nitride Epoxy Composites with
Enhanced Thermal Conductivity.Rsc Adv 2014；4(83):44282-44290.).In this method of modifying
The nitration mixture used is dangerous, high poison reagent with toluene, harmful, and treated boron nitride crystal structure can be sent out
Changing.And the present invention is modified for non-covalent bond, modifying agent cation polymethacrylamide is mainly adsorbed by electrostatic interaction
On hexagonal boron nitride surface, the crystal structure of boron nitride is not interfered with, medium used is water in modified, and green non-pollution is whole
Individual modifying process is simple and easy, nontoxic, low for equipment requirements.
In addition, patent before or document are directed generally to nitrogen in the research of resin heat conduction is improved using boron nitride
Change the modification of boron surface, the distribution of boron nitride in the base is not designed, and this patent passes through the poly- methyl-prop of cation
The restriction effect of acrylamide makes boron nitride align in the base, is more beneficial for thermal conductivity raising.
The beneficial effects of the invention are as follows：
1. the modifying agent used in the present invention is cation polymethacrylamide, green non-poisonous, being modified six sides with it nitrogenizes
The method of boron has no report.The method of modifying used is simple and easy to do for non-covalent bond method, will not change the crystal of hexagonal boron nitride
Structure, compared to other chemical modification methods, not only safety, and production demand can be met.
2. modified hexagonal boron nitride (m-BN) meeting orientations in polycarbonate matrix in the present invention, make obtained
Thermal conductivity, the heat resistance of composite significantly improve, while electrical insulating property is maintained.In embodiment 4, add 20wt% and change
During hexagonal boron nitride after property, the thermal conductivity of composite is 0.73W/ (mK), is 3.1 times of pure makrolon, and compound
Temperature when material thermal weight loss is 5% reaches 498 DEG C, and purer makrolon improves 77 DEG C；Filling-modified hexagonal boron nitride
Composite volume resistivity remain at 1016Ω cm, electric field requirement can be met.
Brief description of the drawings：
Fig. 1 be the embodiment of the present invention 1 provide hexagonal boron nitride before modified after infared spectrum comparison diagram；
Fig. 2 be the embodiment of the present invention 1~4 provide modification hexagonal boron nitride/polycarbonate composite material, comparative example 1 carries
The thermal conductivity curve comparison for hexagonal boron nitride/polycarbonate composite material that the polycarbonate resin and comparative example 2~5 of confession provide
Figure；
Fig. 3 is that modification hexagonal boron nitride/polycarbonate composite material that the embodiment of the present invention 1~4 provides and comparative example 1 carry
The thermogravimetric curve comparison diagram of the polycarbonate resin of confession；
Fig. 4 is that modification hexagonal boron nitride/polycarbonate composite material that the embodiment of the present invention 1~4 provides and comparative example 1 carry
The specific insulation comparison diagram of the polycarbonate resin of confession；
Embodiment
The present invention is further described with reference to the accompanying drawings and examples.It should be noted that following instance of the present invention is only
It is the proof and evidence to technical scheme, does not limit protection domain and be only limitted to this.
The polycarbonate pellet that following examples are related to is the makrolon of South Korea's Samsung SC-1100R models.
The cation polymethacrylamide that following examples are related to is acrylyl oxy-ethyl-trimethyl salmiac and methyl
The copolymer of acrylamide；The mol ratio of the two is acrylyl oxy-ethyl-trimethyl salmiac：Methacrylamide=1:4.
Embodiment 1
1st, surface is modified the preparation of hexagonal boron nitride
(1) 3g BN and 300ml distilled water is added in 500ml round-bottomed flask, be stirred with 300rpm, and
35 DEG C, ultrasonic 40h under 100kW.
(2) configuration quality fraction is 0.5wt% cation polymethacrylamide aqueous solution 20g, is added dropwise
In first step solution, solution starts to be layered in dropwise addition, and stopping dropwise addition when upper solution is just clarified, (process control, which is added dropwise, is
2min), continue stirring 20min at 100 rpm to be allowed to fully react.
(3) above-mentioned mixed liquor is filtered into the miillpore filter by 0.22 μm, filtration residue solids is dried at 40 DEG C
24h, obtain the hexagonal boron nitride (m-BN) of cation polymethacrylamide modification.
2nd, the preparation of modified hexagonal boron nitride/polycarbonate composite material
2.737g m-BN and 52g polycarbonate pellets are weighed respectively, pour into melt blending in Haake torque rheometer, altogether
Mixed temperature is 235 DEG C, rotor speed 30rpm, and the blending time is 10min.Shred (particle diameter 3cm while hot after blending terminates
Left and right).The material shredded is put into grinding tool, heat pressing process is：Hot pressing temperature be 230 DEG C, successively pressure be 0,100kgf,
Hot pressing 5 minutes under 200kgf, after hot pressing terminates, take out grinding tool and be put into cold press device, cooling pressurize 10 minutes, obtained 5wt% changes
The polycarbonate composite material of property hexagonal boron nitride content.
The specific steps of embodiment 2~4 with embodiment 1, but in embodiment 2~4 m-BN dosage it is different, specific dosage such as table
Shown in 1.
M-BN dosages in the embodiment 1~4 of table 1
The preparation of comparative example：
Comparative example 1
52g polycarbonate pellets are weighed, pours into and stirring is melted in Haake torque rheometer, cavity temperature is 235 DEG C, rotor
Rotating speed is 30rpm, mixing time 10min.Shredded while hot after end to be mixed.The material shredded is put into grinding tool, hot pressing
Technique is：Hot pressing temperature is 230 DEG C, and successively hot pressing 5 minutes in the case where pressure is 0,100kgf, 200kgf, after hot pressing terminates, take out
Grinding tool is put into cold press device, cooling pressurize 10 minutes, pure polycarbonate plate is made.
Comparative example 2
2.737g unmodified hexagonal boron nitride and 52g polycarbonate pellets is weighed respectively, pours into Haake torque rheometer
Middle melt blending, blending temperature are 235 DEG C, rotor speed 30rpm, and the blending time is 10min.Cut while hot after blending terminates
It is broken.The material shredded is put into grinding tool, heat pressing process is：Hot pressing temperature be 230 DEG C, successively pressure be 0,100kgf,
Hot pressing 5 minutes under 200kgf, after hot pressing terminates, take out grinding tool and be put into cold press device, cooling pressurize 10 minutes, 5wt% is made not
The polycarbonate composite material of modified hexagonal boron nitride content.
Filler used is unmodified hexagonal boron nitride in comparative example, and the specific steps of comparative example 3~5 are with comparative example 2, but BN
Dosage is different, and specific dosage is as shown in table 2.
Unmodified hexagonal boron nitride dosage in the comparative example 1~5 of table 2
To being characterized as below for the hexagonal boron nitride after before modified and polycarbonate composite material：
(1) before modified after hexagonal boron nitride
Referring to accompanying drawing 1, it be provided in embodiment 1 before modified after hexagonal boron nitride infared spectrum, 1375cm-1With
818cm-1Peak be hexagonal boron nitride characteristic peak, correspond respectively to B-N stretching vibration peaks and B-N-B flexural vibrations peaks.By
Cation polymethacrylamide is modified, in addition to there are two characteristic peaks of foregoing hexagonal boron nitride, have also appeared
New peak, as shown in modified hexagonal boron nitride curve, 3445cm-1Locate as N-H peaks, 2957cm-1And 2871cm-1For-CH3It is flexible
Vibration, 2929cm-1For-CH2Stretching vibration, 1734cm-1Locate as-COOCH2Middle C=O stretching vibration, 1648-1601cm-1
It is amide Ⅰ and acid amides II with characteristic peak, 953cm-1For quaternary ammonium group characteristic peak.Thus illustrate, cation polymethacrylamide
Hexagonal boron nitride surface is successfully adsorbed in.
(2) polycarbonate composite material
Referring to accompanying drawing 2, it be the embodiment of the present invention 1~4 provide modification hexagonal boron nitride/polycarbonate composite material,
Unmodified hexagonal boron nitride/polycarbonate composite material that the polycarbonate resin and comparative example 2~5 that comparative example 1 provides provide
Thermal conductivity curve comparison figure (abscissa is that 5~20wt% section be directed to embodiment 1~4 wherein in curve 2, horizontal stroke in curve 1
The section that coordinate is 5-20wt% is directed to comparative example 2~5, and abscissa is that the point at 0 is directed to comparative example 1).There is provided with comparative example 1
Polycarbonate resin compare, the thermal conductivity for the composite that embodiment 1~4 and comparative example 2~5 provide increases,
Moreover, the addition of filler is more, the thermal conductivity raising of composite is more obvious.Meanwhile the filler that embodiment 1~4 provides is
The filler that the thermal conductivity of the composite of modified hexagonal boron nitride is respectively higher than the offer of comparative example 2~5 nitrogenizes for unmodified six side
The heat conductivity value of the composite of boron.In embodiment 4, when adding 20wt% modification hexagonal boron nitrides, heat conductivity is
0.73W/ (mK), it is 3.1 times of pure makrolon.This is because, by cation polymethacrylamide it is modified six
Square boron nitride, when being blended with polycarbonate melt, motion is restricted, and the orientation in big face is formd in polycarbonate matrix
Structure, hot-fluid transmission efficiency are improved, and final thermal conductivity improves；On the other hand, adsorb hexagonal boron nitride surface sun from
Sub- polymethacrylamide can improve hexagonal boron nitride and the interface bond strength of polycarbonate matrix, and interface resistance reduces,
Thermal conductivity can be improved.
Referring to accompanying drawing 3, it be the embodiment of the present invention 1~4 provide modification hexagonal boron nitride/polycarbonate composite material,
(wherein curve 1 is directed to comparative example 1 to the thermogravimetric curve comparison diagram for the polycarbonate resin that comparative example 1 provides, and curve 2~5 is successively
For embodiment 1~4).With comparative example 1 provide polycarbonate resin compared with, embodiment 1~4 provide composite it is resistance to
Hot property increases, moreover, the addition of filler is more, the heat resistance raising of composite is more obvious.Embodiment 4
In, when adding 20wt% modification hexagonal boron nitrides, the temperature of composite thermal weight loss 5% reaches 498 DEG C, and purer makrolon carries
It is high 77 DEG C.
Referring to accompanying drawing 4, it be the embodiment of the present invention 1~4 provide modification hexagonal boron nitride/polycarbonate composite material,
(wherein abscissa is 5~20wt% section to the specific insulation comparison diagram for the polycarbonate resin that comparative example 1 provides, hollow
The post of filling is directed to embodiment 1~4, and the post of hatching solid is directed to comparative example 2~5, and abscissa is to be directed to comparative example 1 at 0).With
The polycarbonate resin that comparative example 1 provides is compared, the volume electricity for the composite that embodiment 1~4 and comparative example 2~5 provide
Though resistance rate decreases, 10 are remained at16Ω cm, it is sufficient to meet the requirement in electric field.
Result above shows to add the polycarbonate composite material that cation polymethacrylamide is modified hexagonal boron nitride
On the premise of excellent electrical insulation capability is kept, thermal conductivity and heat resistance are greatly improved.
Unaccomplished matter of the present invention is known technology.
Claims (5)
- A kind of 1. preparation method of high heat conductive insulating hexagonal boron nitride/polycarbonate composite material, it is characterized in that this method includes Following steps：The first step：Hexagonal boron nitride and distilled water are added in reactor, it is mass ratio that it, which is matched, hexagonal boron nitride:Distillation Water=1:100~400,30~40h of ultrasonic disperse；Second step：By the cation polymethacrylamide aqueous solution that mass fraction is 0.1~1%, first step preparation is added drop-wise to Solution in, solution starts to be layered in dropwise addition, when upper solution is clarified stop be added dropwise cation polymethacrylamide solution, Continue 5~30min of stirring, obtain mixed liquor；3rd step：Above-mentioned mixed liquor is filtered by miillpore filter, then by solid residue at 35~50 DEG C dry 20~ 24h, the hexagonal boron nitride of cation polymethacrylamide modification is obtained, is designated as m-BN；4th step：Will modified hexagonal boron nitride (m-BN) and makrolon melt blending in torque rheometer, m-BN quality Fraction is 5~20%；Melt blending temperature is 230~250 DEG C, and rotor speed be 30~50rpm, the blending time for 6~ 10min；Finally obtain high heat conductive insulating hexagonal boron nitride/polycarbonate composite material.
- 2. the preparation method of high heat conductive insulating hexagonal boron nitride/polycarbonate composite material as claimed in claim 1, its feature It is for the ultrasound condition in the described first step：100kW, 25~60 DEG C.
- 3. the preparation method of high heat conductive insulating hexagonal boron nitride/polycarbonate composite material as claimed in claim 1, its feature It is acrylyl oxy-ethyl-trimethyl salmiac and methacryl for the cation polymethacrylamide in described second step The copolymer of amine；The mol ratio of the two is acrylyl oxy-ethyl-trimethyl salmiac：Methacrylamide=1:1~4.
- 4. the preparation method of high heat conductive insulating hexagonal boron nitride/polycarbonate composite material as claimed in claim 1, its feature For high-purity micron order hexagonal boron nitride that described hexagonal boron nitride is industrial goods, 3~5 μm of piece footpath, purity ＞ 99.0%.
- 5. the preparation method of high heat conductive insulating hexagonal boron nitride/polycarbonate composite material as claimed in claim 1, its feature Aperture for described miillpore filter is 0.15~0.45 μm.
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| CN108219426A (en) * | 2018-01-05 | 2018-06-29 | 广东纳路纳米科技有限公司 | A kind of PC master batches being modified based on white graphite alkene and preparation method thereof |
| CN108264765B (en) * | 2018-01-23 | 2020-04-28 | 河北工业大学 | Preparation method of toughened heat-conducting insulating cyanate resin-based composite material |
| CN108264735B (en) * | 2018-01-23 | 2020-06-09 | 河北工业大学 | Preparation method of toughened, heat-conducting and insulating epoxy resin-based composite material |
| CN108819400B (en) * | 2018-06-26 | 2021-05-04 | 青岛科技大学 | Method for preparing anisotropic heat-conducting block material by utilizing Gibbs free energy induction |
| CN109810544A (en) * | 2018-12-29 | 2019-05-28 | 厦门大学 | A kind of amination hexagonal boron nitride and its preparation method and application |
| CN110105603B (en) * | 2019-05-06 | 2021-05-25 | 南京林业大学 | Hydroxylated hexagonal boron nitride/polyvinyl alcohol/lignin nanoparticle heat-conducting composite film material and preparation method thereof |
| CN110437600A (en) * | 2019-09-06 | 2019-11-12 | 安徽赛福电子有限公司 | A kind of durable capacitor film and preparation method thereof |
| CN115678240A (en) * | 2022-11-08 | 2023-02-03 | 湖北合聚高分子材料有限公司 | MMT/hBN composite modified PC wear-resistant material and preparation method thereof |
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| CN104892968A (en) * | 2015-07-02 | 2015-09-09 | 河北工业大学 | Preparation method of high-heat-conduction hexagonal boron nitride/polyimide composite material |
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| High thermal conductive polyvinyl alcohol composites with hexagonal boron nitride microplatelets as fillers;Xie, Bin-Huan;《COMPOSITES SCIENCE AND TECHNOLOGY》;20130821;第85卷;98-103 * |
| Preparation and characterization of surface modified boron nitride epoxy composites with enhanced thermal conductivity;Hou, Jun;《RSC ADVANCES》;20140910;第4卷(第83期);44282-44290 * |
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