CN110373140A - A kind of epoxy adhesive and preparation method thereof - Google Patents
A kind of epoxy adhesive and preparation method thereof Download PDFInfo
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- CN110373140A CN110373140A CN201910737606.6A CN201910737606A CN110373140A CN 110373140 A CN110373140 A CN 110373140A CN 201910737606 A CN201910737606 A CN 201910737606A CN 110373140 A CN110373140 A CN 110373140A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The present invention provides a kind of epoxy adhesive, the problem of can solve the mechanical properties such as toughness, intensity that epoxy adhesive can not be significantly improved using existing filler.It is configured in proportion by epoxy resin, curing agent and filler, and the filler graphene nanometer sheet, the graphene nanometer sheet is dispersed in the epoxy resin and the curing agent.Meanwhile the present invention also provides the preparation methods of such epoxy adhesive.
Description
Technical field
The present invention relates to the technical field of modification of epoxy adhesive in structure glue field more particularly to structure glue, specially
A kind of epoxy adhesive and preparation method thereof.
Background technique
Cementing structure will not be destroyed because its is light-weight by the continuity of bonded part, the advantages such as bond stress is evenly distributed and
It is widely used in various fields, such as civil engineering, aerospace and medicine etc..The actual strength of cementing structure is mainly by by glue
The performance of fitting and bonding layer determines that bonding layer is usually the most weak part of entire cementing structure, is easiest to occur to damage broken
Bad, therefore, the correlated performance for exploring cementing position adhesive has very important significance.
Epoxy adhesive has excellent mechanical property and adhesive property, is the macromolecule thermosetting being widely used in recent years
Property material.It is the curing system being configured to by a certain percentage using epoxy resin (as matrix) and curing agent.Epoxy resin
Molecular structure be by strand contain active epoxy group characterized by, epoxy group can be located at strand end, in
Between or circlewise structure.It due to containing active epoxy group in molecular structure, send out them can with a plurality of types of curing agent
It gives birth to cross-linking reaction and forms the insoluble high polymer with three-dimensional reticular structure.Epoxy resin (i.e. epoxy adhesive) after solidification
With good physics, chemical property, it has excellent adhesive strength, dielectric properties to the surface of metal and nonmetallic materials
Well, deformation retract rate is small, and stability is good, and hardness is high, and flexibility is preferable, to alkali and most of solvent-stable, but since its is crisp
Property big, the disadvantages of fatigue durability is poor, and Anticrack ability is poor, it is difficult to meet engineering technology requirement, it is therefore necessary to it
It is modified.
Domestic and foreign scholars mostly use the fillers such as heat-resistant powder filler, thermoplastic resin to improve the property of epoxy adhesive at present
Energy.However, there are also many problems, heat-resistant powder filler modified epoxy are such as used, although obtaining the toughness of material
To other mechanical properties such as the intensity for being greatly improved, but sacrificing material.Epoxy can be improved using thermoplastic resin
The toughness of resin also compensates for the epoxy resin toughened defect of heat-resistant powder filler, but thermoplastic resin dissolubility is poor, increases
The viscosity of epoxy-resin systems, to processing technology can be made to complicate.
Summary of the invention
It is asked for the technology for using existing filler that can not significantly improve the mechanical properties such as the toughness of epoxy adhesive, intensity
Topic, the present invention provides a kind of epoxy adhesive, the mechanical properties such as toughness, intensity are significantly better than Conventional epoxy adhesive,
The present invention also provides the preparation methods of the epoxy adhesive simultaneously, and preparation process is simple.
Its technical solution is such that
A kind of epoxy adhesive is configured, it is characterised in that: described to fill out in proportion by epoxy resin, curing agent and filler
Expect that graphene nanometer sheet, the graphene nanometer sheet are dispersed in the epoxy resin and the curing agent.
It is further characterized by:
The quality of the graphene nanometer sheet accounts for the 0.25% ~ 0.75% of the gross mass of the epoxy resin and the curing agent.
The number of plies of the graphene nanometer sheet sandwich is 1 ~ 19 layer.
The preparation method of above-mentioned epoxy adhesive, it is characterised in that: by the graphene nanometer sheet again with the asphalt mixtures modified by epoxy resin
The full and uniform mixing of rouge obtains graphene nanometer sheet modified epoxy, then the graphene nano is added in the curing agent
In piece modified epoxy and make the full and uniform mixing of the two, finally obtained graphene nanometer sheet is epoxy binder modified.
It is further characterized by:
By the graphene nanometer sheet with the epoxy resin is full and uniform mix before, it is first that the graphene nanometer sheet is abundant
Removing and dispersion.
The method that the graphene nanometer sheet is sufficiently removed and dispersed are as follows: the graphene nanometer sheet is dissolved in HPLC third
In ketone, and progress ultrasonic wave shake in water-bath will be put into after the container closure for filling the graphene nanometer sheet and the HPLC acetone
It swings, ultrasonic oscillation time 6h ~ 7h, bath temperature is 20 DEG C ~ 30 DEG C.
Graphene nanometer sheet described in every 2mg is dissolved in HPLC acetone described in 0.8ml ~ 1.2ml.
Make the graphene nanometer sheet and the well-mixed method of the epoxy resin are as follows: the epoxy resin is added and is passed through
It crosses in the graphene nanometer sheet of ultrasonic oscillation and the mixture of the HPLC acetone, with magnetic stirrer to the above mixing
Object is stirred, and first stirring mixes mixture tentatively at normal temperature, then is heated up to 100 DEG C and continues to stir, and evaporates mixture
In the HPLC acetone, the mixture after the HPLC acetone is evaporated is exactly the graphene nanometer sheet modified epoxy tree
Rouge.
Entire evaporation Whole Process Control is within 3h.
Make the curing agent and the well-mixed method of graphene nanometer sheet modified epoxy are as follows: by the solidification
Agent is added in the graphene nanometer sheet modified epoxy, is put into planetary stirring machine, the master of the planetary stirring machine
Axis revolving speed is 1800rpm, mixing time 90s, and stirring while vacuumizes, and completes the graphene nanometer sheet modified epoxy gluing
The preparation of agent.
The beneficial effects of the present invention are:
Epoxy adhesive of the invention, filler is graphene nanometer sheet, since graphene itself has excellent mechanical property,
After being scattered in epoxy resin and curing agent, it can help to bear certain load, play the role of transmission force and support construction,
Increase substantially the mechanical properties such as toughness, the intensity of epoxy adhesive；In addition, the graphene nanometer sheet of dispersion can reduce epoxy
Free volume in molecular resin chain, so that the thermal stability of epoxy adhesive is improved, the subsidiary official in graphene nanometer sheet surface
(i.e. hydroxy or carboxy) can be rolled into a ball can also form stable chemical bonding with the epoxy group on epoxy resin, improve filler and epoxy
Binding force between resin.
The preparation method of epoxy adhesive of the invention, it is full and uniform by carrying out graphene nanometer sheet with epoxy resin
Mixing, it is ensured that graphene nanometer sheet is uniformly distributed in epoxy resin, and forms stable chemical bonding with epoxy resin, is subtracted
Free volume in small epoxy molecule chain；It is last again that curing agent and graphene nanometer sheet modified epoxy is full and uniform
Mixing, the graphene nanometer sheet for being made final is epoxy binder modified, so that evenly dispersed graphene nanometer sheet can be effective
Improve the mechanical properties such as the intensity, toughness of epoxy adhesive.
Detailed description of the invention
Fig. 1 is the main view of single overlap joint cementing structure；
Fig. 2 is the top view of Fig. 1；
Fig. 3 is the stretching force-displacement curve of the single overlap joint cementing structure failure by shear prepared using epoxy adhesive of the invention；
Fig. 4 is maximum stretching force needed for the single overlap joint cementing structure failure by shear prepared using epoxy adhesive of the invention
Error rod figure；
Fig. 5 is the tensile shear stress-displacement curve of the single overlap joint cementing structure prepared using epoxy adhesive of the invention.
Specific embodiment
A kind of epoxy adhesive of the invention, is configured in proportion by epoxy resin, curing agent and filler, wherein
For the proportionate relationship of epoxy resin and curing agent according to the conventional ratio relationship of existing epoxy adhesive, filler is graphene nano
Piece, the number of plies of graphene nanometer sheet sandwich are 1 ~ 19 layer, and the quality of graphene nanometer sheet accounts for epoxy resin and curing agent
Gross mass 0.25% ~ 0.75%, graphene nanometer sheet is dispersed in epoxy resin and curing agent.
Since common graphene nanometer sheet is stacked by tens layers graphene, graphene is two-dimensional layered structure,
The thickness of single-layer graphene is only 0.34nm, and the number of plies by controlling graphene nanometer sheet sandwich is 1 ~ 19 layer, can be with
Make the thinner of graphene nanometer sheet, to be not easily formed stress concentration after it is scattered in epoxy resin and curing agent
Point.
By taking the WD3003 construction structure glue of Shanghai Kangda Chemical New Material Co., Ltd. as an example, in the construction structure glue
The mass ratio of epoxy resin and curing agent is 3:1, then when being modified using graphene nanometer sheet to it, epoxy resin and solidification
The mass ratio of agent still presses 3:1 configuration, and the quality of graphene nanometer sheet is according to the gross mass for accounting for epoxy resin and curing agent
0.50% ~ 0.75% is configured.
A kind of preparation method of epoxy adhesive of the invention, comprising the following steps:
S1, elder generation determine the mass ratio between epoxy resin and curing agent according to the type of epoxy adhesive, weigh by this mass ratio
The epoxy resin and curing agent of certain mass, the gross mass of epoxy resin and curing agent is accounted for further according to the quality of graphene nanometer sheet
0.25% ~ 0.75%, weigh graphene nanometer sheet；
S2, graphene nanometer sheet is sufficiently removed and is dispersed, the thickness of graphene nanometer sheet is thinned to 1 ~ 19 layer, specific side
Method are as follows: graphene nanometer sheet is directly poured into the container for filling HPLC acetone, the two is made to mix, container closure (can be used into guarantor
Fresh membrane cover lives vessel port and puts on rubber band and fixes) to prevent HPLC acetone from volatilizing, then container is put into water-bath and is surpassed
Sound wave shock, ultrasonic oscillation time 6h ~ 7h, bath temperature are 20 DEG C ~ 30 DEG C；It, can be by graphene by ultrasonic oscillation
Nanometer sheet is sufficiently removed, and the piece number of plies of graphene nanometer sheet is reduced to several layers of to ten several layers of, and graphene nanometer sheet can be made uniform
It spreads out, avoids reuniting；It should be noted that every 2mg graphene nanometer sheet will be dissolved in 0.8ml ~ 1.2ml HPLC acetone, if
HPLC acetone is very little, and in ultrasonic oscillation, graphene nanometer sheet disperses not open, and dispersion effect is bad；If HPLC acetone is too many,
Then the subsequent evaporation time is long, and the structure of epoxy molecule can be destroyed under long term high temperature evaporitic environment；
S3, epoxy resin is added by using magnetic force in the graphene nanometer sheet of ultrasonic oscillation and the mixture of HPLC acetone
Blender is stirred the above mixture, when be added in the mixture of graphene nanometer sheet and HPLC acetone due to epoxy resin
It will appear lamination, therefore should first stir at normal temperature 5 minutes mixes mixture tentatively, then be heated up to 100 DEG C of continuation
Stirring, evaporates the HPLC acetone in mixture, and entire Whole Process Control of evaporating is mixed after HPLC acetone is evaporated within 3h
Closing object is exactly graphene nanometer sheet modified epoxy；The HPLC that evaporation time control is added before can guarantee within 3 hours
Acetone sufficiently volatilizees completely, and will not damage to epoxy molecule；
S4, will curing agent be added graphene nanometer sheet modified epoxy in, be put into planetary stirring machine (Shenzhen Zhong Yi company
ZYMC-200V non-intervention type material homogenizer) in be stirred, the speed of mainshaft of planetary stirring machine is 1800rpm, when stirring
Between 90s, so may insure that mixing effect is good, due to and be not in because to cause epoxy resin largely to generate heat solid in advance for excessive whipping
The phenomenon that change, meanwhile, vacuumizing function is opened in whipping process, is completed graphene to eliminate bubble, after stirring and is received
The epoxy binder modified preparation of rice piece.
In general, the performance evaluation of epoxy adhesive is that the related mechanical property of cementing structure is overlapped by test list, below
With a kind of single overlap joint cementing structure of epoxy adhesive preparation of the invention, its mechanical property is tested.
Epoxy adhesive selects the WD3003 construction structure glue of Shanghai Kangda Chemical New Material Co., Ltd., with graphite
The quality of alkene nanometer sheet accounts for 0,0.25%, 0.50%, the 0.75% of the gross mass of epoxy resin and curing agent, using system of the invention
Preparation Method prepares epoxy adhesive respectively, wherein when graphene nanometer sheet content is 0, need to only press epoxy resin and curing agent
It is put into above-mentioned planetary stirring machine according to the mass ratio of 3:1 and is stirred.For ease of description, graphene is now not added with to receive
The epoxy adhesive of rice piece is denoted as 0GNP, and the epoxy adhesive of 0.25% graphene nanometer sheet of addition is denoted as 0.25% GNP, adds
The epoxy adhesive of 0.50% graphene nanometer sheet is denoted as 0.50% GNP, adds the epoxy adhesive of 0.75% graphene nanometer sheet
It is denoted as 0.75% GNP, then prepares single overlap joint cementing structure respectively using above-mentioned four kinds of epoxy adhesives.
Single overlap joint cementing structure is as depicted in figs. 1 and 2, and single cementing structure preparation method that overlaps is conventional method.1 material of sample
Material is No. 45 steel, and specimen width W is 25.4mm, and length L, width B and the thickness H of bonding layer 2 are respectively 12.70mm, 25.40mm
And 0.2mm.In order to guarantee that experimental result is accurate, every kind of epoxy adhesive prepares 4 samples.
After completing preparation, under quasi-static (0.5mm/min) operating condition of room temperature, glue is overlapped to single by electronic universal tester
Binding structure is stretched, the stretching force-displacement curve of obtained typical failure by shear, as shown in Figure 3；Each curve in Fig. 3
The result of maximum stretching force and maximum displacement summarizes as shown in table 1；The error bar of maximum stretching force is as shown in Figure 4；Utilize drawing
Stretch overlaps the tensile shear stress-displacement curve of cementing structure divided by bonding layer area, available list, as shown in Figure 5；Root
According to the integral area under curve each in Fig. 5, it can estimate that the ductility values of material, ductility values summarize as shown in table 2 roughly.
As can be drawn from Table 1, with the increase of graphene content, the maximum stretching force of epoxy adhesive failure by shear and
Maximum displacement all first increases to be reduced afterwards, and the maximum stretching force and maximum displacement of 0.5% GNP reaches maximum value, respectively
Raising about 93.9% and 73.3% than 0GNP；The maximum stretching force and maximum displacement of 0.75% GNP takes second place；0.25% GNP
Though the maximum stretching force and maximum displacement with 0.75% GNP are not so good as 0.5% GNP, it is also superior to 0GNP.
As can be drawn from Table 2, with the increase of graphene content, the toughness of epoxy adhesive is first to increase to reduce afterwards,
The toughness of 0.5% GNP reaches maximum value, the raising than 0GNP about 233%；The toughness of 0.75% GNP is taken second place；0.25% GNP and
Though the toughness of 0.75% GNP is not so good as 0.5% GNP, it is also superior to 0GNP.
By Fig. 4 it can be found that the heterogeneity of 0.5% GNP is higher, illustrate that graphene nanometer sheet divides in epoxy resin-base
It is best to dissipate property, better anisotropic elastic solid is presented, single cementing structure that overlaps is made to be had fracture to become by huge imposed load
When gesture, 0.5% graphene plays the role of best transmitting and dispersion force in glue-line, greatly improves the intensity of structure
And toughness.
The peak load and maximum displacement of the different epoxy adhesives of table 1
The toughness of the different epoxy adhesives of table 2
According to the peak load in table 1, the tensile shear strength of epoxy adhesive, τ=Pmax/ can be calculated according to following formula
(B×L).In formula:
τ-tensile shear strength, MPa；
Pmax-sample failure by shear peak load (maximum stretching force i.e. in table 1), N；
B-bonding layer width, mm；
L-bonding layer length, mm.
The tensile shear strength being calculated is as shown in table 3.From table 3 it is observed that with the increase of graphene content,
The tensile shear strength of epoxy adhesive first increases to be reduced afterwards, and the tensile shear strength of 0.5% GNP reaches maximum value, compares 0GNP
Raising about 94%；The tensile shear strength of 0.75% GNP takes second place；Though the tensile shear strength of 0.25% GNP and 0.75% GNP
Not as good as 0.5% GNP, but also it is superior to 0GNP.
Why with graphene content increase, maximum stretching force, maximum displacement, toughness, tensile shear strength are first
Reduced after increase, analysis the reason is that, graphene nanometer sheet intensity with higher itself and hardness, a certain amount of graphene nano
Piece is scattered in epoxy resin, can be helped to bear certain load, be played the role of transmission force and support construction, thus substantially
Degree improves the mechanical property of epoxy adhesive.But when graphene continues to add and reaches a certain amount of, in the epoxy can
It is uneven to be easy dispersion, is easy to appear reunion and forms stress concentration point, so that mechanical property be made to be declined.
The tensile shear strength of the different epoxy adhesives of table 3
To sum up, it can be seen that epoxy adhesive of the invention is cut when graphene additive amount is in 0.25% ~ 0.75% range
It cuts through the mechanical properties such as bad maximum stretching force, maximum displacement, toughness, tensile shear strength and is superior to common Wear Characteristics of Epoxy Adhesive
Agent.
Described in detail below with several specific embodiments the preparation method of epoxy adhesive of the invention.
Embodiment 1
Using WD3003 construction structure glue as raw material, epoxy resin 30g, curing agent 10g, graphene nanometer sheet 0.1g are weighed
(0.25%)；0.1g graphene nanometer sheet is directly poured into the container for filling 40ml HPLC acetone, covers container with preservative film
Mouthful and put on rubber band and fix, then container is put into water-bath and carries out ultrasonic oscillation, ultrasonic oscillation time 6h, water-bath temperature
Degree is 20 DEG C；30g epoxy resin is added to the mixture of the graphene nanometer sheet and HPLC acetone by ultrasonic oscillation again
In, the above mixture is stirred with magnetic stirrer, is first stirred 5 minutes at normal temperature, then be heated up to 100 DEG C and continue to stir
It mixes, evaporates the HPLC acetone in mixture, entire Whole Process Control of evaporating is in 3h, and the mixture after HPLC acetone is evaporated is just
It is graphene nanometer sheet modified epoxy；Finally 10g curing agent is added in graphene nanometer sheet modified epoxy, is put into
It is stirred in planetary stirring machine, the speed of mainshaft of planetary stirring machine is 1800rpm, mixing time 90s, in whipping process
Middle unlatching vacuumizing function completes the epoxy binder modified preparation of graphene nanometer sheet to eliminate bubble after stirring.
Embodiment 2
Using WD3003 construction structure glue as raw material, epoxy resin 30g, curing agent 10g, graphene nanometer sheet 0.2g are weighed
(0.50%)；0.2g graphene nanometer sheet is directly poured into the container for filling 100ml HPLC acetone, covers container with preservative film
Mouthful and put on rubber band and fix, then container is put into water-bath and carries out ultrasonic oscillation, ultrasonic oscillation time 7h, water-bath temperature
Degree is 30 DEG C；30g epoxy resin is added to the mixture of the graphene nanometer sheet and HPLC acetone by ultrasonic oscillation again
In, the above mixture is stirred with magnetic stirrer, is first stirred 5 minutes at normal temperature, then be heated up to 100 DEG C and continue to stir
It mixes, evaporates the HPLC acetone in mixture, entire Whole Process Control of evaporating is in 3h, and the mixture after HPLC acetone is evaporated is just
It is graphene nanometer sheet modified epoxy；Finally 10g curing agent is added in graphene nanometer sheet modified epoxy, is put into
It is stirred in planetary stirring machine, the speed of mainshaft of planetary stirring machine is 1800rpm, mixing time 90s, in whipping process
Middle unlatching vacuumizing function completes the epoxy binder modified preparation of graphene nanometer sheet to eliminate bubble after stirring.
Embodiment 3
Using WD3003 construction structure glue as raw material, epoxy resin 30g, curing agent 10g, graphene nanometer sheet 0.3g are weighed
(0.75%)；0.3g graphene nanometer sheet is directly poured into the container for filling 180ml HPLC acetone, covers container with preservative film
Mouthful and put on rubber band and fix, then container is put into water-bath and carries out ultrasonic oscillation, ultrasonic oscillation time 6.5h, water-bath
Temperature is 25 DEG C；30g epoxy resin is added to the mixture of the graphene nanometer sheet and HPLC acetone by ultrasonic oscillation again
In, the above mixture is stirred with magnetic stirrer, is first stirred 5 minutes at normal temperature, then be heated up to 100 DEG C and continue to stir
It mixes, evaporates the HPLC acetone in mixture, entire Whole Process Control of evaporating is in 3h, and the mixture after HPLC acetone is evaporated is just
It is graphene nanometer sheet modified epoxy；Finally 10g curing agent is added in graphene nanometer sheet modified epoxy, is put into
It is stirred in planetary stirring machine, the speed of mainshaft of planetary stirring machine is 1800rpm, mixing time 90s, in whipping process
Middle unlatching vacuumizing function completes the epoxy binder modified preparation of graphene nanometer sheet to eliminate bubble after stirring.
Claims (10)
1. a kind of epoxy adhesive is configured, it is characterised in that: described in proportion by epoxy resin, curing agent and filler
Filler graphene nanometer sheet, the graphene nanometer sheet are dispersed in the epoxy resin and the curing agent.
2. a kind of epoxy adhesive according to claim 1, it is characterised in that: the quality of the graphene nanometer sheet accounts for institute
State the 0.25% ~ 0.75% of the gross mass of epoxy resin and the curing agent.
3. a kind of epoxy adhesive according to claim 2, it is characterised in that: the graphene nanometer sheet sandwich
The number of plies be 1 ~ 19 layer.
4. a kind of preparation method of epoxy adhesive of any of claims 1-3, it is characterised in that: by the graphite
Alkene nanometer sheet again with the epoxy resin is full and uniform mixes, obtain graphene nanometer sheet modified epoxy, then will be described solid
Agent is added in the graphene nanometer sheet modified epoxy and makes the full and uniform mixing of the two, and graphene nano is finally made
Piece is epoxy binder modified.
5. a kind of preparation method of epoxy adhesive according to claim 4, it is characterised in that: by the graphene nano
Piece with the epoxy resin is full and uniform mix before, first the graphene nanometer sheet is sufficiently removed and is dispersed.
6. a kind of preparation method of epoxy adhesive according to claim 5, it is characterised in that: by the graphene nano
The method that piece is sufficiently removed and dispersed are as follows: the graphene nanometer sheet is dissolved in HPLC acetone, and the graphene will be filled
It is put into water-bath after the container closure of nanometer sheet and the HPLC acetone and carries out ultrasonic oscillation, ultrasonic oscillation time 6h ~ 7h,
Bath temperature is 20 DEG C ~ 30 DEG C.
7. a kind of preparation method of epoxy adhesive according to claim 6, it is characterised in that: graphene described in every 2mg
Nanometer sheet is dissolved in HPLC acetone described in 0.8ml ~ 1.2ml.
8. a kind of preparation method of epoxy adhesive according to claim 6, it is characterised in that: make the graphene nano
Piece and the well-mixed method of the epoxy resin are as follows: the epoxy resin is added to the graphene for passing through ultrasonic oscillation
In the mixture of nanometer sheet and the HPLC acetone, the above mixture is stirred with magnetic stirrer, is first stirred at normal temperature
Mixing mixes mixture tentatively, then is heated up to 100 DEG C and continues to stir, and the HPLC acetone in mixture is evaporated, to described
Mixture after HPLC acetone is evaporated is exactly the graphene nanometer sheet modified epoxy.
9. a kind of preparation method of epoxy adhesive according to claim 8, it is characterised in that: entire evaporation overall process control
System is within 3h.
10. a kind of preparation method of epoxy adhesive according to claim 4 or 8, it is characterised in that: make the curing agent
With the well-mixed method of graphene nanometer sheet modified epoxy are as follows: the graphene nano is added in the curing agent
It in piece modified epoxy, is put into planetary stirring machine, the speed of mainshaft of the planetary stirring machine is 1800rpm, stirring
Time 90s, stirring while, vacuumize, and complete the epoxy binder modified preparation of the graphene nanometer sheet.
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| CN115302895A (en) * | 2022-07-11 | 2022-11-08 | 张家港飞腾复合新材料股份有限公司 | Light composite board with stable application and production process thereof |
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