CN105778427A - Method for synergistically modifying epoxy resin through nitride-carbon nano tube nanocomposite - Google Patents
Method for synergistically modifying epoxy resin through nitride-carbon nano tube nanocomposite Download PDFInfo
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- CN105778427A CN105778427A CN201610352308.1A CN201610352308A CN105778427A CN 105778427 A CN105778427 A CN 105778427A CN 201610352308 A CN201610352308 A CN 201610352308A CN 105778427 A CN105778427 A CN 105778427A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5033—Amines aromatic
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
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- C08K7/24—Expanded, porous or hollow particles inorganic
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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Abstract
The invention discloses a method for synergistically modifying epoxy resin through a nitride-carbon nano tube nanocomposite.The method comprises the following steps that 1, a carbon nano tube is subjected to carboxylation through concentrated sulfuric acid and concentrated nitric acid; 2, boron nitride ultrasonic stripping is carried out in a liquid phase assisted mode, and then a silane coupling agent is utilized for modifying boron nitride; 3 heatign reflux is carried out to prepare the nitride-carbon nano tube nanocomposite; 4, a nitride-carbon nano tube/epoxy resin composite material is prepared in a in-situ polymerization mode.By means of the method, the dispersity of the carbon nano tube in the epoxy resin is effectively improved, and the mechanical property and heat-conducting property of the epoxy resin are improved.
Description
One, technical field
The method that the present invention relates to a kind of boron nitride-carbon nanotube nanocomposite modified synergic epoxy resin, belongs to high molecular nanometer multiple
Condensation material field.
Two, background technology
Epoxy resin has a feature of the excellences such as excellent hot property, corrosion resistance and intensity are high, adhesive property is good, thus extensively
The general field of electronic materials that is applied to, but epoxy resin thermal property is poor, and so limiting its use, and epoxy resin is solid
After change, property is crisp, so the application of epoxy resin is had great significance by the mechanical property of raising epoxy resin and heat conductivility.Mesh
Before, improve the heat conductivility of epoxy resin and the main path of mechanical strength is to carry out it with high heat conduction and high strength filler respectively
Modified.
Nm-class boron nitride heat conductivity is high, is commonly used to improve the heat conductivity of polymer.Generally utilize organic molecule such as 18-amine.,
Silane couplers etc. carry out surface modification to nm-class boron nitride, can improve the compatibility of itself and polymeric matrix, promote nano silicon nitride
Boron dispersion in the polymer.But nm-class boron nitride is a kind of stratified nano materials, even if it is also difficult to be uniformly dispersed during a small amount of interpolation
To form thermal conducting path in the polymer, the heat conductivity significantly improving polymer during the highest addition, could be compared.
CNT is a kind of monodimension nanometer material with relatively high length-diameter ratio, has high intensity and high thermal conductivity, is a kind of excellent
Different polymers function filler.When being uniformly dispersed, CNT can form three-dimensional net structure in polymeric matrix, builds good
Conduction and heat conduction network.But, the most modified carbon nano tube surface can be high, easily reunites, cause after adding polymer
It is the most notable to the modified effect of polymer.
Three, summary of the invention
It is desirable to provide the method for a kind of boron nitride-carbon nanotube nanocomposite modified synergic epoxy resin, on the one hand improve
CNT dispersibility in the epoxy, it is achieved the raising of epoxy resin mechanical property；The most auxiliary by CNT
Help nm-class boron nitride to form thermal conducting path in the epoxy, improve its heat conductivity.
The method of boron nitride of the present invention-carbon nanotube nanocomposite modified synergic epoxy resin, comprises the steps:
1, CNT is carboxylated: weigh 0.2g CNT, adds 75ml concentrated sulphuric acid (98wt%) and 25ml concentrated nitric acid
(65wt%) mixed solution, magnetic agitation 10h under the water bath condition of 40 DEG C, stay after high speed centrifugation under 10000rpm rotating speed
Take off a layer material, the pH value of lower floor's material is adjusted to 7, obtains carboxylic carbon nano-tube；
2, boron nitride is peeled off: weigh 0.5g boron nitride, adds 100ml isopropanol, ultrasonic 48h, low-speed centrifugal after stirring
Leave and take upper solution；
3, boron nitride is modified: add silane coupler in the upper solution that step 2 obtains and alcohol water obtains mixed solution, heats up
It is stirred at reflux reaction 4 hours to 75 DEG C, then dialyses 48h with bag filter, after lyophilization, obtain modified boron nitride；
4, carboxylic carbon nano-tube prepared by step 1 is distributed in isopropanol, within ultrasonic 1 hour, obtains carbon nano tube dispersion liquid；
Modified boron nitride step 3 prepared is distributed in isopropanol, within ultrasonic 1 hour, obtains boron nitride dispersion；CNT is divided
Dissipate liquid and boron nitride dispersion mixing, be stirred at reflux reaction 10 hours at 70 DEG C, obtain boron nitride-carbon nanotube after drying
Complex；
5, weigh 3g epoxy resin and add in 10ml DMF, stir 30min at 60 DEG C, obtain epoxy resin
Solution；
6, boron nitride step 4 prepared-carbon nanotube nanocomposite adds in 20ml DMF, the most again
Adding 0.75g firming agent, ultrasonic disperse adds in the epoxy resin solution of step 5 preparation the most afterwards, continues ultrasonic 2.5 hours,
Rotation is evaporated off solvent, pours into solidify in Teflon mould and i.e. obtains modified epoxy.
It is by adding substantial amounts of water that the pH value of lower floor's material is adjusted in step 17, repeats and changes what the method for water realized.
Being centrifuged in step 2 and leaving and taking upper solution is for obtaining the preferable boron nitride of peeling effect.
In step 2, the rotating speed of low-speed centrifugal is 4000 revs/min.
In step 3 mixed solution, the mass volume ratio of boron nitride, silane coupler and alcohol water is 1g:3g:1000mL, wherein alcohol
Water is isopropyl alcohol and water, and both volume ratios are 3:1.Alcohol water when herein calculating proportional quantity refers to the total isopropanol in mixed solution
And water, and not merely refer to the alcohol water added in step 3.
The weight average molecular weight of the bag filter used during dialysis in step 3 is 14000.
In step 3, cryodesiccated baking temperature is-50 DEG C, and drying time is 48 hours.
CNT and the mass ratio of boron nitride in step 4 are 5:1.
In step 6, the quality of boron nitride-carbon nanotube nanocomposite is the 0.2-1% of epoxy resin quality.
Firming agent described in step 6 is 4,4-MDA.
In step 6, cure parameter is: first solidify 2h at 80 DEG C, then raises temperature to 120 DEG C of solidification 2h, finally in 160 DEG C
Solidification 4h.
Cooperative effect is applied to catalytic field the earliest, and it refers to the catalytic performance of two or more metal generation higher than any one
Performance during component individualism.In the polymer-modified field of nano composite material, utilize one of cooperative effect the earliest is graphite
Alkene/carbon mano-tube composite, mixes with monomer after compound for the CNT of graphene oxide and functionalization, then carries out polycondensation anti-
Should obtain composite masterbatch, then obtain Graphene and multi-walled carbon nano-tubes works in coordination with enhanced polymer fiber (CN through melt extruding
104357941 B)。
The present invention uses suitable method to build the boron nitride-carbon nanotube nanocomposite with three-dimensional net structure, utilizes modification
Nm-class boron nitride and the excellent compatibility of polymer promote CNT in the polymer dispersed, simultaneously by CNT
Interconnection function aided nano boron nitride form thermal conducting path in the polymer, play CNT and two kinds of nanometers of nm-class boron nitride
The advantage of material, collaborative mechanics and the heat conductivility improving epoxy resin.
Four, accompanying drawing explanation
Fig. 1 is the TEM picture of boron nitride-carbon mano-tube composite.
Fig. 2 is carbon nano tube/epoxy resin thin film macrograph.
Fig. 3 is boron nitride-carbon nano tube/epoxy resin thin film macrograph.
Fig. 4 is the picture of the heat conductivity of epoxy resin and the epoxy resin thin film adding different filler.
Fig. 5 is the DMA picture of epoxy resin and the epoxy resin thin film adding different filler.
Five, detailed description of the invention
Term used in the present invention, unless otherwise specified, typically have that those of ordinary skill in the art are generally understood that contains
Justice.
The specific descriptions present invention carried out below by embodiment, it is necessary to it is pointed out here that be following example be served only for this
Invention is further described, it is impossible to be interpreted as limiting the scope of the invention, and the person skilled in the art in this field can root
According to foregoing, the present invention made some nonessential improvement and adjustment.
Embodiment 1:
1, CNT is carboxylated: weigh 0.2g CNT, adds 75ml concentrated sulphuric acid (98wt%) and 25ml concentrated nitric acid
(65wt%) mixed solution, magnetic agitation 10h under the water bath condition of 40 DEG C, stay after high speed centrifugation under 10000rpm rotating speed
Take off a layer material, the pH value of lower floor's material is adjusted to 7, obtains carboxylic carbon nano-tube；
2, boron nitride is peeled off: weigh 0.5g boron nitride, adds 100ml isopropanol, and ultrasonic 48h after stirring, with 4000
Rev/min rotating speed be centrifuged and leave and take upper solution；
3, boron nitride is modified: add silane coupler in the upper solution that step 2 obtains and alcohol water obtains mixed solution, heats up
It is stirred at reflux reaction 4 hours to 75 DEG C, then with bag filter that weight average molecular weight is 14000 dialysis 48h, lyophilization at-50 DEG C
48h, obtains modified boron nitride；
In mixed solution, the mass volume ratio of boron nitride, silane coupler and alcohol water is 1g:3g:1000mL, and wherein alcohol water is different
Third alcohol and water, both volume ratios are 3:1.Alcohol water when herein calculating proportional quantity refers to the total isopropyl alcohol and water in mixed solution,
And not merely refer to the alcohol water added in step 3.
4, carboxylic carbon nano-tube prepared by 0.02g step 1 is distributed in 100mL isopropanol, within ultrasonic 1 hour, obtains carbon and receive
Mitron dispersion liquid；Modified boron nitride 0.1g step 3 prepared is distributed in 100mL isopropanol, within ultrasonic 1 hour, is nitrogenized
Boron dispersion liquid；Carbon nano tube dispersion liquid and boron nitride dispersion are mixed, is stirred at reflux at 70 DEG C and reacts 10 hours, dried
To boron nitride-carbon nanotube nanocomposite.
Shown in the transmission electron microscope Fig. 1 of boron nitride-carbon mano-tube composite that the present embodiment obtains, CNT uniform load is in nitridation
Boron surface or interlayer.
Embodiment 2:
1, CNT is carboxylated: weigh 0.2g CNT, adds 75ml concentrated sulphuric acid (98wt%) and 25ml concentrated nitric acid
(65wt%) mixed solution, magnetic agitation 10h under the water bath condition of 40 DEG C, stay after high speed centrifugation under 10000rpm rotating speed
Take off a layer material, the pH value of lower floor's material is adjusted to 7, obtains carboxylic carbon nano-tube；
2, weigh 3g epoxy resin and add in 10ml DMF, stir 30min at 60 DEG C, obtain epoxy resin
Solution；
3, the carboxylic carbon nano-tube weighing the preparation of 0.015g step 1 joins in 20ml DMF solution, then
Add 0.75g 4,4-MDA firming agent, add after ultrasonic 30min in the epoxy resin solution of step 2 preparation, continue
Continuous ultrasonic 2.5 hours, rotation was evaporated off solvent, pours into solidify in Teflon mould and i.e. obtains carbon nano tube/epoxy resin thin film.
Condition of cure is: first solidify 2h at 80 DEG C, then raises temperature to 120 DEG C of solidification 2h, finally solidifies 4h in 160 DEG C.
From its macrograph, the macrograph of carbon nano tube/epoxy resin thin film prepared by the present embodiment is as in figure 2 it is shown, just can be seen that carbon is received
Mitron is reunited seriously in the epoxy.
Embodiment 3:
1, weigh 3g epoxy resin and add in 10ml DMF, stir 30min at 60 DEG C, obtain epoxy resin
Solution；
2, the boron nitride-carbon nanotube nanocomposite weighing 0.015g embodiment 1 preparation adds 20ml N, N-dimethyl formyl
In amine, add 0.75g4,4-MDA firming agent subsequently, after ultrasonic disperse 30min, add the ring of step 1 preparation
In epoxy resins solution, continuing ultrasonic 2.5 hours, rotation is evaporated off solvent, pours into solidify in Teflon mould and is i.e. nitrogenized
Boron-carbon nanotube/epoxy resin thin film.Condition of cure is: first solidify 2h at 80 DEG C, then raises temperature to 120 DEG C of solidification 2h,
Finally solidify 4h in 160 DEG C.
The macrograph of boron nitride prepared by the present embodiment-carbon nano tube/epoxy resin thin film as it is shown on figure 3, with Fig. 2 CNT/
Epoxy resin macrograph compares, and the dispersibility of CNT has obtained obvious improvement.
Embodiment 4:
1, weigh 0.5g boron nitride, add 100ml isopropanol, ultrasonic 48h after stirring, with the rotating speeds of 4000 revs/min from
The heart also leaves and takes upper solution；Rotation is evaporated off a part of solvent and adds water and revolve steaming again, is repeated 3 times, last remove all molten
Agent obtains the boron nitride being dried；
2, weigh 3g epoxy resin and add in 10ml DMF, stir 30min at 60 DEG C, obtain epoxy resin
Solution；
3, the boron nitride weighing the preparation of 0.015g step 1 adds in 20ml DMF, adds 0.75g4,4-subsequently
MDA firming agent, adds after ultrasonic disperse 30min in the epoxy resin solution of step 2 preparation, continues ultrasonic 2.5
Hour, rotation is evaporated off solvent, pours into solidify in Teflon mould and i.e. obtains boron nitride/epoxy resin thin film.Condition of cure is:
First solidify 2h at 80 DEG C, then raise temperature to 120 DEG C of solidification 2h, finally solidify 4h in 160 DEG C.
Boron nitride/the epoxy resin thin film preparing the present embodiment carries out Determination of conductive coefficients, as shown in Figure 4, under room temperature, and heat conduction
Coefficient is 0.306W/mK.
Embodiment 5:
The carbon nano tube/epoxy resin film obtained in embodiment 2 is carried out DMA test, as it is shown in figure 5, its storage modulus is
2272MPa。
Embodiment 6:
The boron nitride obtained in embodiment 3-carbon nano tube/epoxy resin film is carried out thermal conductivity test, as it is shown in figure 5, under room temperature,
Heat conductivity is 0.311W/mK.It is carried out DMA test, and as shown in Figure 4, when 30 DEG C, storage modulus is 2754MPa.
Claims (9)
1. the method for boron nitride-carbon nanotube nanocomposite modified synergic epoxy resin, it is characterised in that include walking as follows
Rapid:
(1) CNT is carboxylated: weigh 0.2g CNT, and the mixing adding 75ml concentrated sulphuric acid and 25ml concentrated nitric acid is molten
Liquid, magnetic agitation 10h under the water bath condition of 40 DEG C, leave and take lower floor's material after high speed centrifugation, the pH value of lower floor's material is adjusted
To 7, obtain carboxylic carbon nano-tube；
(2) boron nitride is peeled off: weigh 0.5g boron nitride, adds 100ml isopropanol, ultrasonic 48h after stirring, low speed from
The heart leaves and takes upper solution；
(3) boron nitride is modified: add silane coupler in the upper solution that step (2) obtains and alcohol water obtains mixed solution,
It is warming up to 75 DEG C and is stirred at reflux reaction 4 hours, then dialyse 48h with bag filter, after lyophilization, obtain modified boron nitride；
(4) carboxylic carbon nano-tube prepared by step (1) is distributed in isopropanol, within ultrasonic 1 hour, obtains CNT and divide
Dissipate liquid；Modified boron nitride prepared by step (3) is distributed in isopropanol, within ultrasonic 1 hour, obtains boron nitride dispersion；By carbon
Nanotube dispersion liquid and boron nitride dispersion mixing, be stirred at reflux reaction 10 hours at 70 DEG C, obtain nitrogenizing boron-carbon after drying and receive
Mitron nano-complex；
(5) weigh 3g epoxy resin and add in 10ml DMF, stir 30min at 60 DEG C, obtain asphalt mixtures modified by epoxy resin
Lipoprotein solution；
(6) during boron nitride step (4) prepared-carbon nanotube nanocomposite adds 20ml DMF,
Adding 0.75g firming agent subsequently, ultrasonic disperse adds in the epoxy resin solution of step 5 preparation the most afterwards, continues ultrasonic 2.5
Hour, rotation is evaporated off solvent, pours into solidify in Teflon mould and i.e. obtains modified epoxy.
Method the most according to claim 1, it is characterised in that:
In step (2), the rotating speed of low-speed centrifugal is 4000 revs/min.
Method the most according to claim 1, it is characterised in that:
In step (3) mixed solution, the mass volume ratio of boron nitride, silane coupler and alcohol water is 1g:3g:1000mL, its
Middle alcohol water is isopropyl alcohol and water, and both volume ratios are 3:1.It is total different that alcohol water when herein calculating proportional quantity refers in mixed solution
Third alcohol and water, and not merely refer to the alcohol water added in step 3.
Method the most according to claim 1, it is characterised in that:
The weight average molecular weight of the bag filter used during dialysis in step (3) is 14000.
Method the most according to claim 1, it is characterised in that:
In step (3), cryodesiccated baking temperature is-50 DEG C, and drying time is 48 hours.
Method the most according to claim 1, it is characterised in that:
CNT and the mass ratio of boron nitride in step (4) are 5:1.
Method the most according to claim 1, it is characterised in that:
The 0.2-1% that quality is epoxy resin quality of boron nitride-carbon nanotube nanocomposite in step (6).
Method the most according to claim 1, it is characterised in that:
Described in step (6), firming agent is 4,4-MDA.
Method the most according to claim 1, it is characterised in that:
In step (6), cure parameter is: first solidify 2h at 80 DEG C, then raises temperature to 120 DEG C of solidification 2h, finally in 160 DEG C
Solidification 4h.
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Cited By (14)
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| CN107189292A (en) * | 2017-07-20 | 2017-09-22 | 安徽盛华管业有限公司 | A kind of composite modified high heat conduction CPVC tubing of CNT/boron nitride and preparation method |
| CN108624296A (en) * | 2018-07-11 | 2018-10-09 | 桂林电子科技大学 | A kind of composite solid-solid phase-change and preparation method thereof of boron nitride enhancing heat conduction |
| CN109338762A (en) * | 2018-08-28 | 2019-02-15 | 苏州印丝特纺织数码科技有限公司 | A kind of preparation method of the digit printing ink modified based on boron nitride nanosheet |
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| CN107189292A (en) * | 2017-07-20 | 2017-09-22 | 安徽盛华管业有限公司 | A kind of composite modified high heat conduction CPVC tubing of CNT/boron nitride and preparation method |
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| CN109338762A (en) * | 2018-08-28 | 2019-02-15 | 苏州印丝特纺织数码科技有限公司 | A kind of preparation method of the digit printing ink modified based on boron nitride nanosheet |
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| CN112778703A (en) * | 2021-01-06 | 2021-05-11 | 沈阳航空航天大学 | High-toughness and heat-conducting epoxy resin composite material and preparation method thereof |
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