CN106633632A - Preparation method of epoxy resin/carbon nano-tube/nano nickel composite material - Google Patents
Preparation method of epoxy resin/carbon nano-tube/nano nickel composite material Download PDFInfo
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- CN106633632A CN106633632A CN201610911235.5A CN201610911235A CN106633632A CN 106633632 A CN106633632 A CN 106633632A CN 201610911235 A CN201610911235 A CN 201610911235A CN 106633632 A CN106633632 A CN 106633632A
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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
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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- C—CHEMISTRY; METALLURGY
- 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
- C08G59/44—Amides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0862—Nickel
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
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Abstract
The invention provides a preparation method of an epoxy resin/carbon nano-tube/nano nickel composite material and belongs to the field of composite materials. The invention aims to toughen epoxy resin and also improve electric-conductivity. The method includes the steps of: 1) supporting nano nickel powder on carbon nano-tubes; 2) adding the carbon nano-tubes to epoxy resin with emulsifying dispersion to prepare an epoxy resin/carbon nano-tube/nano nickel mixture; 3) respectively pre-heating and uniformly mixing the epoxy resin/carbon nano-tube/nano nickel mixture and a curing agent PA-651, pouring the mixture into a polytetrafluoroethylene mould which has been pre-heated and is coated with high-vacuum silicone grease, and curing the mixture in a drying box to produce the epoxy resin/carbon nano-tube/nano nickel composite material. The epoxy resin/carbon nano-tube/nano nickel composite material has excellent electric-conductivity and mechanical performance, so that the composite material has wide application in the fields of adhesives, electronic instruments, aerospace, paints, electronic and electrical insulation materials, etc.
Description
Technical field
The invention belongs to technical field of composite materials；Specifically related to epoxy resin/carbon nanotube/nanometer nickel composite material
Preparation method.
Background technology
Epoxy resin (Epoxy Resin) is a kind of macromolecule thermoset synthetic materials being widely used in recent years, it
With excellent adhesive property, corrosion resistance and electrical insulation capability etc., it is widely used in coating, adhesive and engineering material
Material field.Play in many industrial circles such as electric and electronic, machine-building, chemical anticorrosion, ship harbour, Aero-Space and focus on
The effect wanted, is one of basic material indispensable in various industrial circles.Epoxy resin have so many application be by
In its excellent mechanical property, electrical insulation capability, shrinkage factor is low, and adhesive property is good, chemical resistance, good processing characteristics, valency
The features such as lattice are cheap.EP matter is crisp, and it is also necessary to carry out toughening modifying to it.
The content of the invention
The invention provides a kind of method for preparing epoxy resin/carbon nanotube/nanometer nickel composite material, by hydro-thermal method
Carbon nanotube/nano nickel composite material is prepared, recycles mulser that carbon nanotube/nano nickel is uniformly dispersed in into asphalt mixtures modified by epoxy resin
In fat.Epoxy resin/carbon nanotube/nanometer nickel composite material is prepared using situ aggregation method, it is therefore intended that epoxy resin is increased
Strong its mechanical property.
The preparation method of epoxy resin of the present invention/carbon nanotube/nano nickel composite material is carried out in the steps below：
Step one, nano-nickel powder is loaded on the carbon nanotubes；
Step 2, it is subsequently adding in epoxy resin, emulsion dispersion, obtains epoxy resin/carbon nanotube/nano nickel mixing
Thing；
Step 3, epoxy resin/carbon nanotube obtained in step 2/nano nickel mixture and firming agent PA-651 are distinguished
Mix after preheating, then pour in the preheated Teflon mould for scribbling fine vacuum silicone grease, be put in baking oven and solidify, obtain
Epoxy resin/graphite alkene/nanometer nickel composite material；
Solidification wherein described in step 3 is first 2h to be reacted at a temperature of 70 DEG C, then 2.5h is reacted at a temperature of 125 DEG C, so
React 1h at a temperature of 150 DEG C afterwards.
The method of carbon nanotube loaded nano-nickel powder is as follows in step one：Weigh the NiSO of 1.8g4·6H2The many walls of O and 0.3g
CNT is dissolved in 25mL ethylene glycol and forms solution, adds NaOH solution, and the NaOH solution is to add 1.2g NaOH
Ultrasonic dissolution is configured in 10mL water, adds the hydrazine hydrate of 11mL 80%, after reactant liquor stirs, is transferred to stainless
In steel autoclave, 2h is reacted at 120 DEG C, after the question response time to cooling, centrifugal filtration, successively with distilled water and anhydrous
Washing with alcohol, at 50 DEG C 24h is vacuum dried, and obtains nano nickel/multi-walled carbon nano-tubes complex.
The carbon nanotube/nano nickel that mass percent is 0.9% is separately added into into 60g epoxy resin (E-51) in step 2
In, emulsion dispersion is carried out using mulser, rotating speed 4500r/min emulsion dispersion 5min-7min obtain epoxy resin/carbon nanometer
Pipe/nano nickel mixture.
Described epoxy resin is E-51 epoxy resin.
By scattered epoxy resin/carbon nanotube/nano nickel mixture and firming agent PA-651 (low molecules in step 3
Polyamide) mixing after preheating 2h in 63 DEG C of baking ovens is respectively put into, with the rotating speed stirring 3-5min of 100r/min, (discharge is rolled in epoxy
Bubble in resin), epoxy resin/carbon nanotube/nano nickel prepolymer is formed, it is poured into and preheats scribbling for 2.5h through 55 DEG C
In the Teflon mould of fine vacuum silicone grease, curing oven is subsequently placed into, obtains epoxy resin/graphite alkene/nano nickel and be combined
Material.
Firming agent PA-651 consumptions are the 50wt% of epoxy resin.
This research first loads nano nickel on the carbon nanotubes, then using special process by nano nickel/CNT
In being dispersed in epoxy resin-base, epoxy resin/carbon nanotube/nano nickel composite material I engineering plastics are developed.Carbon nanometer
Pipe can strengthen, toughness reinforcing, and nano nickel can improve electric conductivity.Therefore so obtained epoxy resin/carbon nanotube/nano nickel composite wood
Material be just provided with excellent electric conductivity and excellent mechanical performance so that its adhesive, electronic instrument, Aero-Space, coating,
The application of the fields such as electric insulant is more extensive.
Epoxy resin/carbon nanotube/nanometer nickel composite material prepared by methods described, carbon nanotube/nano nickel is in epoxy
Favorable dispersibility in resin, compared with pure epoxy resin, the tensile strength when carbon nanotube/nano nickel content is 2.3wt%
47.3% is increased respectively.
1st, under the conditions of CNT serves as surfactant, obtained nano-nickel powder particle diameter in nanoscale, dimensionally stable,
Particle diameter is less；
2nd, reducing agent is hydrazine hydrate in the present invention, and hydrazine hydrate produces during the course of the reaction nitrogen and can effectively prevent nano nickel
Oxidation, while the water for producing is reacted it without any impact；
3rd, using mulser to epoxy resin/carbon nanotube/nano nickel system dispersion, the method is simple, easy to operate, dispersion
Property is preferable, it is not necessary to add any coating material and coupling agent；
4th, epoxy resin/carbon nanotube/nanometer nickel composite material, its performance and pure epoxy tree are prepared using situ aggregation method
Lipid phase ratio, when carbon nanotube/nano nickel content is 2.3wt%, tensile strength increased 47.3%.
Description of the drawings
Fig. 1 is the SEM figures of epoxy resin/carbon nanotube/nanometer nickel composite material；
Fig. 2 is pure epoxy resin, carbon nanotube/nano nickel, the XRD figure of epoxy resin/carbon nanotube/nano nickel；
Fig. 3 is the DMA figures of epoxy resin/carbon nanotube/nanometer nickel composite material.
Specific embodiment
Specific embodiment one：The preparation side of present embodiment epoxy resin/carbon nanotube/nano nickel composite material
Method, it is characterised in that the method is carried out in the steps below：
Step one, the NiSO for weighing 1.8g4·6H2O and 0.3g multi-walled carbon nano-tubes is dissolved in 25mL ethylene glycol and forms molten
Liquid, the solution for adding 1.2g NaOH to add 10mL water ultrasonic dissolutions to be configured to, adds the hydrazine hydrate of 11mL 80%, reactant liquor
After stirring, in being transferred to rustless steel autoclave, 2h is reacted at 120 DEG C, after the question response time to cooling, be centrifuged
Filter, successively with distilled water and absolute ethanol washing, at 50 DEG C 24h is vacuum dried, and is obtained nano nickel/multi-walled carbon nano-tubes and is combined
Thing；
Step 2, it is that 0.9% carbon nanotube/nano nickel is separately added into 60g epoxy resin (E-51) by mass percent
In, emulsion dispersion is carried out using mulser, rotating speed 4500r/min emulsion dispersion 5min-7min obtain epoxy resin/carbon nanometer
Pipe/nano nickel mixture；
Step 3, by scattered epoxy resin/carbon nanotube/nano nickel mixture and firming agent Versamid
(PA-651) (firming agent PA-651 consumptions are the 50wt% of epoxy resin.) mixing after preheating 2h in 63 DEG C of baking ovens is respectively put into,
With rotating speed stirring 3-5min (bubble in the epoxy is wrapped up in discharge) of 100r/min, formation epoxy resin/carbon nanotube/receive
Rice nickel prepolymer, is poured in 55 DEG C of Teflon moulds for scribbling fine vacuum silicone grease for preheating 2.5h.It is subsequently placed into
Curing oven, obtains epoxy resin/graphite alkene/nanometer nickel composite material, and condition of cure is：70 DEG C/2h, 125 DEG C/2.5h, 150
℃/1h。
Electronic Speculum is retouched by Fig. 1 it is observed that the new surface that formed of its sectional drawing is in addition to the streamline clear of river, crackle and disconnected
Face is all very neat well-balanced, and agglomeration does not occur, it was demonstrated that the acidification of CNT solves composite presence
The phenomenon easily reunited, it also avoid the low problem of caused composite materials property because of bad dispersibility in the epoxy.
Tested by Fig. 2 XRD, curve a is the XRD curves of pure epoxy resin in figure, gone out in the position that 2 θ are 15 °～25 °
Existing peak value is less, the larger peak of peak width, and this is the characteristic peak of epoxy resin；Curve b is the XRD curves of carbon nanotube/nano nickel,
Also there is the characteristic peak of Graphene in addition to the characteristic peak for having nickel；Curve c is the XRD curves of epoxy resin/carbon nanotube/nano nickel,
The absworption peak wide compared with pure epoxy resin characteristic peak is occurred in that in figure, is because that epoxy resin and the characteristic peak of Graphene there occurs
Overlap, in addition the characteristic peak without copper oxide is occurred in that, illustrates to be successfully prepared out epoxy resin/carbon nanotube/nanometer
Nickel composite material.
Fig. 3 is the loss of the different epoxy resin/carbon nanotube of carbon nanotube/nano nickel content/nanometer nickel composite material
Factor curve, as can be seen from the figure because confinement effect is with the peak of the addition fissipation factor of carbon nanotube/nano nickel content
Position is gradually moved to high temperature direction, and the peak value of pure epoxy resin is 104 DEG C, and adopt emulsion dispersion method prepare CNT/
Nanometer nickel content for 0.9wt% epoxy resin/carbon nanotube/nano nickel solidfied material peak position at 117 DEG C, vitrification
Transition temperature improves 13 DEG C.This be due to carbon nanotube/nano nickel have stronger surface energy and chemical reactivity, can
There is chemical bonding effect with epoxy resin, form chemical crosslinking point, the motor capacity of segment declines so that the activity of strand
Resistance increases, so as to improve their glass transition temperature.Illustrate the addition of carbon nanotube/nano nickel so that matrix epoxy
The thermostability of resin is significantly improved.
Claims (6)
1. the preparation method of epoxy resin/carbon nanotube/nanometer nickel composite material, it is characterised in that the method is in the steps below
Carry out：
Step one, nano-nickel powder is loaded on the carbon nanotubes；
Step 2, it is subsequently adding in epoxy resin, emulsion dispersion, obtains epoxy resin/carbon nanotube/nano nickel mixture；
Step 3, epoxy resin/carbon nanotube obtained in step 2/nano nickel mixture and firming agent PA-651 are preheated respectively
After mix, then pour in the preheated Teflon mould for scribbling fine vacuum silicone grease, be put in baking oven and solidify, obtain epoxy
Resin/graphite alkene/nanometer nickel composite material；
Solidification wherein described in step 3 is first 2h to be reacted at a temperature of 70 DEG C, then 2.5h, Ran Hou are reacted at a temperature of 125 DEG C
1h is reacted at a temperature of 150 DEG C.
2. the preparation method of epoxy resin/carbon nanotube/nanometer nickel composite material according to claim 1, it is characterised in that
The method of carbon nanotube loaded nano-nickel powder is as follows in step one：Weigh the NiSO of 1.8g4·6H2O and 0.3g multi-walled carbon nano-tubes
It is dissolved in 25mL ethylene glycol and forms solution, add NaOH solution, the NaOH solution is 1.2g NaOH to be added in 10mL water to surpass
Sound dissolving is configured to, and adds the hydrazine hydrate of 11mL 80%, after reactant liquor stirs, is transferred to rustless steel reaction under high pressure
In kettle, 2h is reacted at 120 DEG C, after the question response time to cooling, centrifugal filtration, successively with distilled water and absolute ethanol washing,
24h is vacuum dried at 50 DEG C, nano nickel/multi-walled carbon nano-tubes complex is obtained.
3. the preparation method of epoxy resin/carbon nanotube/nanometer nickel composite material according to claim 2, it is characterised in that
The carbon nanotube/nano nickel that mass percent is 0.9% is separately added in 60g epoxy resin, using mulser in step 2
Emulsion dispersion is carried out, rotating speed 4500r/min emulsion dispersion 5min-7min obtain epoxy resin/carbon nanotube/nano nickel mixing
Thing.
4. the preparation method of epoxy resin/carbon nanotube/nanometer nickel composite material according to claim 3, it is characterised in that
Described epoxy resin is E-51 epoxy resin.
5. the preparation method of epoxy resin/carbon nanotube/nanometer nickel composite material according to claim 3, it is characterised in that
Scattered epoxy resin/carbon nanotube/nano nickel mixture and firming agent PA-651 are respectively put into into 63 DEG C of bakings in step 3
Preheat in case after 2h and mix, 3-5min is stirred with the rotating speed of 100r/min, form epoxy resin/carbon nanotube/nano nickel pre-polymerization
Thing, is poured in 55 DEG C of Teflon moulds for scribbling fine vacuum silicone grease for preheating 2.5h, is subsequently placed into curing oven,
Obtain epoxy resin/graphite alkene/nanometer nickel composite material.
6. the preparation method of epoxy resin/carbon nanotube/nanometer nickel composite material according to claim 3, it is characterised in that
Firming agent PA-651 consumptions are the 50wt% of epoxy resin.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109593322A (en) * | 2018-12-04 | 2019-04-09 | 黑龙江大学 | The preparation method of graphene-supported corronil reinforced epoxy composite material |
| CN112724601A (en) * | 2020-12-25 | 2021-04-30 | 北京化工大学 | Carbon fiber reinforced composite material with high interface strength and strong interface conductivity and preparation method thereof |
| CN114334220A (en) * | 2021-12-29 | 2022-04-12 | 贵研铂业股份有限公司 | Low-temperature curing type three-proofing conductive nickel paste, preparation method and application thereof |
| CN116496587A (en) * | 2023-03-13 | 2023-07-28 | 苏州辰鹏电子新材料有限公司 | Preparation method of enhanced antibacterial PVC composite material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109593322A (en) * | 2018-12-04 | 2019-04-09 | 黑龙江大学 | The preparation method of graphene-supported corronil reinforced epoxy composite material |
| CN112724601A (en) * | 2020-12-25 | 2021-04-30 | 北京化工大学 | Carbon fiber reinforced composite material with high interface strength and strong interface conductivity and preparation method thereof |
| CN112724601B (en) * | 2020-12-25 | 2022-06-21 | 北京化工大学 | Carbon fiber reinforced composite material with high interface strength and strong interface conductivity and preparation method thereof |
| CN114334220A (en) * | 2021-12-29 | 2022-04-12 | 贵研铂业股份有限公司 | Low-temperature curing type three-proofing conductive nickel paste, preparation method and application thereof |
| CN116496587A (en) * | 2023-03-13 | 2023-07-28 | 苏州辰鹏电子新材料有限公司 | Preparation method of enhanced antibacterial PVC composite material |
| CN116496587B (en) * | 2023-03-13 | 2024-03-08 | 苏州辰鹏电子新材料有限公司 | Preparation method of enhanced antibacterial PVC composite material |
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