CN110452648A - A kind of epoxy adhesive and its application - Google Patents
A kind of epoxy adhesive and its application Download PDFInfo
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- CN110452648A CN110452648A CN201910737608.5A CN201910737608A CN110452648A CN 110452648 A CN110452648 A CN 110452648A CN 201910737608 A CN201910737608 A CN 201910737608A CN 110452648 A CN110452648 A CN 110452648A
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- epoxy adhesive
- nanometer sheet
- graphene nanometer
- epoxy
- curing agent
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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
-
- 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 adhesives, though can solve the water absorption rate that can reduce epoxy adhesive using existing filler, are unable to improve the mechanical property of epoxy adhesive, lead to the epoxy adhesive low problem of reliability in wet condition.It is configured in proportion by epoxy resin, curing agent and filler, and filler is graphene nanometer sheet, and the quality of graphene nanometer sheet accounts for the 0.25% of the gross mass of epoxy resin and curing agent, and graphene nanometer sheet is dispersed in epoxy resin and curing agent.Meanwhile the present invention also provides the applications of such epoxy adhesive.
Description
Technical field
The present invention relates to the modification technology necks of epoxy adhesive in construction structure glue field more particularly to construction structure glue
Domain, specially a kind of epoxy adhesive and its application.
Background technique
Being glued connection, light weight, stress distribution are uniform, will not destroy by advantages such as the continuitys of bonded part in soil because having
Wood engineering field is widely used.
Epoxy adhesive is common material binder in building trade, it is using epoxy resin (as matrix) and solidification
The curing system that agent is configured to by a certain percentage.The molecular structure of epoxy resin is to contain active epoxy group in strand
It is characterized, epoxy group can be located at the end of strand, centre or circlewise structure.Due to containing vivaciously in molecular structure
Epoxy group crosslink them can with a plurality of types of curing agent and react and be formed insoluble with three-dimensional reticular structure
High polymer.Epoxy resin (i.e. epoxy adhesive) after solidification has good physics, chemical property, it is to metal and nonmetallic
The surface of material has excellent adhesive strength, and dielectric properties are good, and deformation retract rate is small, and stability is good, and hardness is high, flexibility
Preferably, to alkali and most of solvent-stable, thus it is widely used in building field, uses epoxy adhesive outer patch fibre reinforced
Composite material (CFRP) has become reinforcing and one of the important means of mending concrete and steel construction.
But currently, the disadvantage that epoxy adhesive is low there is also reliability in wet condition, limits epoxy adhesive and exists
Application in building trade greatly reduces the durability of cementing structure.Because building is generally all exposed to outdoor, be easy by
To the influence of wet environment, hydrone is existed by changing epoxy adhesive and being glued the mechanical characteristic at interface to reduce cementing structure
Durability under wet environment.The study found that the suction of diffusion coefficient and epoxy adhesive of the hydrone in epoxy adhesive
Water rate affects the changing rule of cementing structure mechanical property under high humidity environment, wherein diffusion coefficient is bigger, cementing structure
Mechanical properties decrease it is faster；Water absorption rate is higher, and mechanical properties decrease amplitude is bigger.
Therefore, by reducing hydrone in the diffusion coefficient of epoxy adhesive and the water absorption rate of epoxy adhesive to changing
The mechanical property of kind epoxy adhesive in wet condition is a research direction of current epoxy adhesive.Expand to reduce
It dissipates coefficient and water absorption rate, domestic and foreign scholars used a variety of fillers to be modified epoxy adhesive, such as hydrophobic inorganic filler
(processing-type silica, quartz sand), hydrophobicity organic filler (heat foamable particle) etc..By that will have filling out for certain width-thickness ratio
Expect it is evenly dispersed in the epoxy, so that filler is constructed in epoxy resin and form complicated hydrophobic network, to moisturize
The son tortuous of diffusion and transmission path, and then the diffusion coefficient of reduction hydrone in the epoxy, reduces Wear Characteristics of Epoxy Adhesive
The water absorption rate of agent.But though above-mentioned filler can reduce the water absorption rate of epoxy adhesive, to the mechanical property of epoxy adhesive
Improvement is not obvious.This is because the thickness of above-mentioned filler is usually millimeter rank, filler it is generous smaller, with asphalt mixtures modified by epoxy resin
Rouge contact area is small, therefore binding force is poor therebetween, can not form stable network；Furthermore since width-thickness ratio is small, need to add
The network with zigzag path could be formed by entering more amount (usually 10% ~ 20%), play the effect for reducing water absorption rate, still
So a large amount of filler is added, will result in stress concentration, and stress concentrates the mechanical property that can destroy epoxy adhesive, thus
It is final the result is that the mechanical property improvement of epoxy adhesive is unobvious, or even it is also poorer than unloaded mechanical property.
Summary of the invention
Though being unable to improve the power of epoxy adhesive for the water absorption rate for using existing filler that can reduce epoxy adhesive
Performance is learned, leads to the epoxy adhesive low technical problem of reliability in wet condition, the present invention provides a kind of Wear Characteristics of Epoxy Adhesive
Agent can improve the mechanical property of epoxy adhesive while reducing epoxy adhesive water absorption rate, improve epoxy adhesive and exist
Reliability under wet environment, while the present invention also provides the applications of the epoxy adhesive.
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
Material is graphene nanometer sheet, and the quality of the graphene nanometer sheet accounts for the gross mass of the epoxy resin and the curing agent
0.25%, the graphene nanometer sheet is dispersed in the epoxy resin and the curing agent.
It is further characterized by:
The graphene nanometer sheet is the graphene nanometer sheet by sufficiently removing.
The method that the graphene nanometer sheet is sufficiently removed are as follows: the graphene nanometer sheet is dissolved in HPLC acetone,
And ultrasonic oscillation is carried out by being put into water-bath after the container closure for filling the graphene nanometer sheet and the HPLC acetone, surpass
Sound wave shock time 6h ~ 7h, bath temperature are 20 DEG C ~ 30 DEG C.
Graphene nanometer sheet described in every 2mg is dissolved in HPLC acetone described in 0.8ml ~ 1.2ml.
The application of above-mentioned epoxy adhesive, it is characterised in that: the epoxy adhesive is used under wet environment
In cementing structure, the wet environment is environment of the relative humidity of air 70% or more.
The beneficial effects of the present invention are:
Epoxy adhesive of the invention, filler are graphene nanometer sheet, since the thickness of graphene nanometer sheet is in Nano grade,
And graphene is two-dimensional layered structure, therefore graphene nanometer sheet has the width-thickness ratio of super large, as filler, graphene nano
The contact area super large of piece and epoxy resin, and functional group's (i.e. hydroxy or carboxy) energy and ring that graphene nanometer sheet surface is subsidiary
Epoxy group on oxygen resin forms stable chemical bonding, so that the binding force between graphene nanometer sheet and epoxy resin is non-
Chang Qiang；Furthermore graphene nanometer sheet is super-hydrophobic material, can construct to form hydrophobic network in the epoxy, and by
In its width-thickness ratio super large, therefore minimal amount of graphene nanometer sheet need to only be added and can construct to be formed there is complicated zigzag path
Hydrophobic network, the present invention in graphene nanometer sheet quality only account for epoxy resin and curing agent gross mass 0.25%, due to adding
Dosage is few, not will form stress concentration, epoxy adhesive of the invention application test in wet condition the result shows that,
Water absorption rate is substantially less than conventional epoxy adhesive, and mechanical property is significantly better than conventional epoxy adhesive；In addition, graphene is received
Rice piece excellent in mechanical performance itself, is able to bear certain load, can further improve tensile strength, the elasticity of epoxy adhesive
Modulus and fracture toughness.
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 quality of graphene nanometer sheet account for the 0.25% of the gross mass of epoxy resin and curing agent, and graphene nanometer sheet is dispersed in
In epoxy resin and curing agent.It, should by taking the WD3003 construction structure glue of Shanghai Kangda Chemical New Material Co., Ltd. as an example
The mass ratio of epoxy resin and curing agent is 3:1 in construction structure glue, then when being modified using graphene nanometer sheet to it, ring
The mass ratio of oxygen resin and curing agent still presses 3:1 configuration, and the quality of graphene nanometer sheet is then according to accounting for epoxy resin and solidification
The 0.25% of the gross mass of agent is configured.
In general, the graphene film number of plies in graphene nanometer sheet is tens layers, in order to further increase graphene nanometer sheet
Width-thickness ratio, graphene nanometer sheet can sufficiently be removed in advance, reduce graphene nanometer sheet in the piece number of plies, be thinned stone
The thickness of black alkene nanometer sheet.The method that graphene nanometer sheet is sufficiently removed are as follows: graphene nanometer sheet is directly poured into and is filled
In the container of HPLC acetone, so that the two is mixed, container closure (can be covered vessel port with preservative film and put on rubber band and fixed)
To prevent HPLC acetone from volatilizing, then container is put into water-bath and carries out ultrasonic oscillation, ultrasonic oscillation time 6h ~ 7h is excellent
6.5h is selected, bath temperature is 20 DEG C ~ 30 DEG C；By ultrasonic oscillation, graphene nanometer sheet can sufficiently be removed, make graphite
The piece number of plies in alkene nanometer sheet is reduced to several layers of to ten several layers of, and can make graphene nanometer sheet is evenly dispersed to come, and avoids reuniting；
It should be noted that every 2mg graphene nanometer sheet will be dissolved in 0.8ml ~ 1.2ml HPLC acetone, preferably 1ml, because of HPLC acetone
Very little, in ultrasonic oscillation, graphene nanometer sheet disperses not open, and dispersion effect is bad；HPLC acetone is too many, then subsequent evaporation
Time required for HPLC acetone is long, and the structure of epoxy molecule can be destroyed under long term high temperature evaporitic environment.
It, should be first abundant by the graphene nanometer sheet sufficiently removed and epoxy resin when preparing epoxy adhesive of the invention
Uniformly mixing, is made graphene nanometer sheet modified epoxy, then by curing agent and graphene nanometer sheet modified epoxy into
The full and uniform mixing of row, the graphene nanometer sheet for being finally made of the invention are epoxy binder modified.
Wherein, by the graphene nanometer sheet sufficiently removed and the full and uniform mixed method of epoxy resin are as follows: by asphalt mixtures modified by epoxy resin
Rouge is added in the mixture of the above-mentioned graphene nanometer sheet by ultrasonic oscillation and HPLC acetone, with magnetic stirrer to above
Mixture is stirred, and it is existing to will appear layering when be added in the mixture of graphene nanometer sheet and HPLC acetone due to epoxy resin
As, therefore should first stir at normal temperature 5 minutes mixes mixture tentatively, then is heated up to 100 DEG C and continues to stir, and evaporates mixed
The HPLC acetone in object is closed, for entire Whole Process Control of evaporating within 3h, the mixture after HPLC acetone is evaporated is exactly graphite
Alkene nanometer sheet modified epoxy；The HPLC acetone that evaporation time control is added before can guarantee within 3 hours sufficiently volatilizees
Completely, and epoxy molecule will not be damaged.
Curing agent is subjected to full and uniform mixed method with graphene nanometer sheet modified epoxy are as follows: by curing agent plus
Enter in graphene nanometer sheet modified epoxy, being put into planetary stirring machine, (ZYMC-200V that Shenzhen Zhong Yi company can be selected is non-
Insertion type material homogenizer) in be stirred, the speed of mainshaft of planetary stirring machine is 1800rpm, mixing time 90s, so
It is good to may insure mixing effect, and the phenomenon that be not in premature cure due to epoxy resin is caused largely to generate heat for excessive whipping,
Meanwhile vacuumizing function is opened in whipping process, the modified ring of graphene nanometer sheet is completed to eliminate bubble, after stirring
The preparation of oxygen adhesive.
Epoxy adhesive of the invention is specifically used under wet environment by the application of epoxy adhesive of the invention
Cementing structure in, wet environment refers to environment of the relative humidity of air 70% or more.Epoxy adhesive of the invention can
The mechanical property of cementing structure in wet condition is significantly improved, is illustrated below with specific test data.
Using WD3003 construction structure glue as raw material, the gross mass of epoxy resin and curing agent is accounted for graphene nanometer sheet respectively
0.25%, 0.50%, 0.75% corresponding epoxy adhesive is made, and water absorption rate to epoxy adhesive and tensile strength carry out
Test, as a comparison with unmodified WD3003 construction structure glue.
Water absorption rate test: typical high humidity environment at room temperature is selected, that is, is completely soaked in distilled water (air phase at this time
It is 100%) to humidity.Reference standard " the code test side of polymer matrix composite water imbibition
Method (ASTM D5529-2012) ", 75*75*1 mm is made in epoxy adhesive3Blob of viscose body after, dried in baking oven first
It is dry, quality is weighed with assay balance (accuracy 0.1mg) at once after taking-up.Sample is placed in the constant temperature (23 equipped with distilled water
DEG C) in sink, the quality test time of sample be determined as 0h, 6h, 12h, for 24 hours, 7d, 14d, every group of test sample is 4.Matter
When measurement, specimen surface need to be dried with absorbent filter and be weighed again.Water absorption rate calculation formula are as follows: water absorption rate=(sample water suction
Quality-sample initial mass afterwards)/sample initial mass * 100%.Experimental result is as shown in table 1:
The water absorption rate of the epoxy adhesive of the different graphene nanometer sheet contents of table 1 and the relation table of ageing time
Note: the quality that GNP content represents graphene nanometer sheet accounts for the percentage of the gross mass of epoxy resin and curing agent.
As can be seen from Table 1, as the content of graphene nanometer sheet increases, water absorption rate also increases, and works as graphene nano
When piece content increases to 0.75%, water absorption rate is suitable with unmodified epoxy adhesive；After 0.25% graphene nanometer sheet is added,
Water absorption rate reducing effect is best, and at the 14th day, compared with unmodified epoxy adhesive, 0.25% graphene nano is added
The water absorption rate of the epoxy adhesive of piece has dropped (3.34-2.95)/3.34*100%=12%.
Tensile strength test: it is conformed to according to standard " preparation method (NF T76-142) of structural adhesive plate " preparation
The epoxy adhesive dumbbell shape sample asked, then by sample be placed in the constant temperature equipped with distilled water (23 DEG C) sink impregnate as defined in when
Between, according to standard " Standard test method (ASTM D638) of plastic tensile performance ", using electronic universal tester, with 2mm/
After the loading velocity of min tests unaged (impregnating 0d) respectively, impregnates 7d in wet environment and impregnate 14d, graphene nano
Piece before modified after epoxy adhesive tensile strength.Experimental result is as shown in table 2:
The tensile strength of the epoxy adhesive of the different graphene nanometer sheet contents of table 2 and the relation table of ageing time
Note: the quality that GNP content represents graphene nanometer sheet accounts for the percentage of the gross mass of epoxy resin and curing agent.
As can be seen from Table 2, as the content of graphene nanometer sheet increases, tensile strength is gradually reduced, and works as graphene
When nanometer sheet content increases to 0.75%, tensile strength is suitable with unmodified epoxy adhesive；The graphene for being added 0.25% is received
After rice piece, tensile strength improvement is best, and at the 14th day, compared with unmodified epoxy adhesive, 0.25% stone is added
The tensile strength of the epoxy adhesive of black alkene nanometer sheet improves (28.99-16.22)/16.22*100%=78.7%；In addition, not
Modified epoxy adhesive is (38.36-16.22)/38.36*100%=57.7% in the 14th day tensile strength fall, and is added
The fall for entering the tensile strength of the epoxy adhesive of 0.25% graphene nanometer sheet is (47.96-28.99)/47.96*
100%=39.5%, show under same wet environment, the fall of epoxy adhesive mechanical property of the invention obviously subtracts
It is few.
The epoxy adhesive of the invention it can be seen from the above experimental result, i.e., by 0.25% graphene nanometer sheet into
The modified epoxy adhesive obtained of row, can significantly reduce the water absorption rate of epoxy adhesive, and with the humidity aging time
Increase, the fall of modified epoxy adhesive mechanical property is substantially reduced, so as to improve cementing structure in humidity
Reliability under environment, improves the ability to bear of building, and the structure of better reinforcement and repair damage extends and reinforces cementing structure
Service life.
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 is graphene nanometer sheet, and the quality of the graphene nanometer sheet accounts for the gross mass of the epoxy resin and the curing agent
0.25%, the graphene nanometer sheet is 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 graphene nanometer sheet is by abundant
The graphene nanometer sheet of removing.
3. a kind of epoxy adhesive according to claim 2, it is characterised in that: sufficiently remove the graphene nanometer sheet
Method are as follows: the graphene nanometer sheet is dissolved in HPLC acetone, and the graphene nanometer sheet and the HPLC will be filled
It is put into after the container closure of acetone in water-bath and carries out ultrasonic oscillation.
4. a kind of epoxy adhesive according to claim 3, it is characterised in that: the time of the ultrasonic oscillation be 6h ~
7h, bath temperature are 20 DEG C ~ 30 DEG C.
5. a kind of epoxy adhesive according to claim 4, it is characterised in that: the time of the ultrasonic oscillation is
6.5h, bath temperature are 25 DEG C.
6. a kind of epoxy adhesive according to claim 3, it is characterised in that: graphene nanometer sheet described in every 2mg is dissolved in
In HPLC acetone described in 0.8ml ~ 1.2ml.
7. a kind of epoxy adhesive according to claim 6, it is characterised in that: graphene nanometer sheet described in every 2mg is dissolved in
In HPLC acetone described in 1ml.
8. a kind of application of epoxy adhesive of any of claims 1-7, it is characterised in that: by the Wear Characteristics of Epoxy Adhesive
Agent is used in the cementing structure under wet environment, and the wet environment is environment of the relative humidity of air 70% or more.
9. the application of epoxy adhesive according to claim 8, it is characterised in that: the wet environment is the opposite of air
Environment of the humidity 80% or more.
10. the application of epoxy adhesive according to claim 8, it is characterised in that: the wet environment is the phase of air
The environment for being 100% to humidity.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910737608.5A CN110452648B (en) | 2019-08-12 | 2019-08-12 | Epoxy adhesive and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910737608.5A CN110452648B (en) | 2019-08-12 | 2019-08-12 | Epoxy adhesive and application thereof |
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| CN110452648B CN110452648B (en) | 2021-09-07 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112625633A (en) * | 2020-12-11 | 2021-04-09 | 固德电材系统（苏州）股份有限公司 | Weather-resistant epoxy resin adhesive for wind power blade and preparation method and application thereof |
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