CN115074068A - Double-component epoxy adhesive and preparation method thereof - Google Patents
Double-component epoxy adhesive and preparation method thereof Download PDFInfo
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- CN115074068A CN115074068A CN202210873212.5A CN202210873212A CN115074068A CN 115074068 A CN115074068 A CN 115074068A CN 202210873212 A CN202210873212 A CN 202210873212A CN 115074068 A CN115074068 A CN 115074068A
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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
- 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
- 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
-
- 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
- C09J11/08—Macromolecular additives
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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
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Abstract
The invention discloses a two-component epoxy adhesive and a preparation method thereof, wherein the two-component epoxy adhesive comprises a component A and a component B; the component A comprises the following raw materials in parts by mass: 30-60 parts of epoxy resin, 15-40 parts of a toughening agent, 20-45 parts of a filler, 5-10 parts of a reactive diluent, 0-1 part of a coupling agent, 0-1 part of a defoaming agent and 0-1 part of a dispersing agent; the component B comprises the following raw materials in parts by mass: 40-90 parts of curing agent, 5-15 parts of toughening agent, 10-30 parts of filler and 0-5 parts of accelerator. The adhesive has high toughness, has good adhesive strength to aluminum alloy, glass fiber reinforced plastic and polyurethane heat-insulating materials, can be heated and cured at normal temperature or medium and low temperature not more than 80 ℃ when being used for adhering the vehicle skin and the polyurethane heat-insulating materials, does not need to reach the temperature at which the polyurethane heat-insulating materials are easy to deform under pressure, and can well meet the adhesive requirement of the vehicle skin and the polyurethane heat-insulating materials.
Description
Technical Field
The invention relates to the field of double-component epoxy glue, in particular to double-component epoxy glue for bonding a vehicle skin and a thermal insulation material and a preparation method thereof.
Background
For the requirements of heat preservation and sound insulation of vehicles such as military refrigerated vehicles, civil refrigerated vehicles, military shower vehicles, military shelter, thermal insulation vehicles, passenger cars, buses and the like, glass fiber reinforced plastics or special aluminum alloy plates are generally adopted as inner and outer vehicle skins, a thermal insulation core material between the inner and outer vehicle skins is a polyurethane thermal insulation material, the inner and outer vehicle skins are connected with the thermal insulation core material in a bonding way, the product has no seam, is corrosion resistant, smog resistant, mould resistant, impact resistant, flat and beautiful outside, but the polyurethane heat-insulating material as the heat-insulating core material is easy to deform under pressure when the temperature is higher than 80 ℃, therefore, the epoxy adhesive suitable for bonding the vehicle skin and the polyurethane thermal insulation material needs to be developed, so that the epoxy adhesive can be heated and cured at normal temperature or medium and low temperature not higher than 80 ℃ when the vehicle skin and the polyurethane thermal insulation material are bonded, and the temperature at which the polyurethane thermal insulation material is easy to deform under pressure does not need to be reached.
At present, the 90-degree peel strength of the epoxy adhesive on the market when bonding the aluminum alloy and the polyurethane heat-insulating material is higher, but the 90-degree peel strength when bonding the glass fiber reinforced plastic and the polyurethane heat-insulating material is poorer, so that the bonding requirement of the vehicle skin and the polyurethane heat-insulating material cannot be met.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a two-component epoxy adhesive and a preparation method thereof, and aims to solve the technical problems in the prior art. The epoxy adhesive has high toughness, has good bonding strength for aluminum alloy, glass fiber reinforced plastic and polyurethane heat-insulating materials, can effectively solve the problem of poor 90-degree peel strength of the existing epoxy adhesive when bonding the glass fiber reinforced plastic and the polyurethane heat-insulating materials, can be heated and cured at normal temperature or medium and low temperature not higher than 80 ℃ when bonding the vehicle skin and the polyurethane heat-insulating materials, does not need to reach the temperature at which the polyurethane heat-insulating materials are easy to deform under pressure, and can well meet the bonding requirement of the vehicle skin and the polyurethane heat-insulating materials.
The purpose of the invention is realized by the following technical scheme:
a double-component epoxy glue comprises a component A and a component B; the component A comprises the following raw materials in parts by mass: 30-60 parts of epoxy resin, 15-40 parts of a toughening agent, 20-45 parts of a filler, 5-10 parts of an active diluent, 0-1 part of a coupling agent, 0-1 part of a defoaming agent and 0-1 part of a dispersing agent; the component B comprises the following raw materials in parts by mass: 40-90 parts of curing agent, 5-15 parts of toughening agent, 10-30 parts of filler and 0-5 parts of accelerator; the epoxy resin is at least two of bisphenol A epoxy resin, bisphenol F epoxy resin, polyurethane modified epoxy resin and elastomer modified epoxy resin.
Preferably, the toughening agent in the component A adopts at least one of blocked polyurethane and nitrile rubber modified epoxy resin; the toughening agent in the component B adopts amino-terminated butadiene-acrylonitrile rubber.
Preferably, the curing agent is a polyamide modified with an aliphatic amine and a phenol.
Preferably, the reactive diluent adopts at least one of carbon dodecyl to tetradecyl glycidyl ether, polypropylene glycol diglycidyl ether, 1, 4-butanediol diglycidyl ether, neopentyl glycol diglycidyl ether and plant polyene phenol epoxy resin modifier.
Preferably, the filler in the component A and the filler in the component B adopt one or two of silica micropowder, calcium carbonate, aluminum hydroxide, polyphosphate, talcum powder and bentonite.
Preferably, the coupling agent adopts at least one of gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, 3-aminopropyl triethoxy silane and gamma-mercaptopropyl trimethoxy silane.
Preferably, the defoaming agent is one of BYK A535, Defom 6800 and ACP001 of Dow Corning chemical.
Preferably, the accelerator is at least one of tertiary amine, imidazole and nonyl phenol.
The preparation method of the double-component epoxy glue comprises the following steps:
s1, preparation of the component A: according to the formula of the component A in the two-component epoxy adhesive, the epoxy resin, the toughening agent, the reactive diluent, the coupling agent, the defoaming agent and the dispersing agent which are required for preparing the component A are added into a reaction kettle and mixed for 30-50 min at 25-60 ℃, then the filler required for preparing the component A is added into the reaction kettle and mixed for 50-70 min at 25-60 ℃, and vacuum is started during mixing, so that the component A is prepared;
s2, preparation of a component B: according to the formula of the component B in the two-component epoxy adhesive, the curing agent, the toughening agent and the accelerator required for preparing the component B are added into a reaction kettle and mixed for 30-50 min at 25-60 ℃, then the filler required for preparing the component B is added into the reaction kettle and mixed for 50-70 min at 25-60 ℃, and vacuum is started during mixing, so that the component B is prepared.
Compared with the prior art, the special epoxy resin is matched with the special toughening agent in the component A and the special toughening agent in the component B according to a specific proportion, and is matched with the special curing agent in the component B, so that the prepared two-component epoxy adhesive has high toughness, has good bonding strength to aluminum alloy, glass fiber reinforced plastic and polyurethane heat-insulating materials, can effectively solve the problem that the 90-degree peel strength of the existing epoxy adhesive is poor when the existing epoxy adhesive is used for bonding glass fiber reinforced plastic and polyurethane heat-insulating materials, can be heated and cured at normal temperature or medium and low temperature not higher than 80 ℃ when the existing epoxy adhesive is used for bonding vehicle skins and polyurethane heat-insulating materials, does not need to reach the temperature at which the polyurethane heat-insulating materials are easy to deform under pressure, and can well meet the bonding requirement of the vehicle skins and the polyurethane heat-insulating materials.
Detailed Description
The technical scheme in the embodiment of the invention is clearly and completely described below; it is to be understood that the described embodiments are merely exemplary of the invention, and are not intended to limit the invention to the particular forms disclosed. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
The terms that may be used herein are first described as follows:
the terms "comprising," "including," "containing," "having," or other similar terms of meaning should be construed as non-exclusive inclusions. For example: including a feature (e.g., material, component, ingredient, carrier, formulation, material, dimension, part, component, mechanism, device, process, procedure, method, reaction condition, processing condition, parameter, algorithm, signal, data, product, or article of manufacture), is to be construed as including not only the particular feature explicitly listed but also other features not explicitly listed as such which are known in the art.
The term "parts by mass" is intended to indicate a mass ratio relationship between a plurality of components, for example: if X component is X parts by mass and Y component is Y parts by mass, the mass ratio of the X component to the Y component is X: Y; 1 part by mass may represent any mass, for example: 1 part by mass may be expressed as 1kg or 3.1415926 kg. The sum of the parts by mass of all the components is not necessarily 100 parts, and may be more than 100 parts, less than 100 parts, or equal to 100 parts. Parts, ratios and percentages described herein are by mass unless otherwise indicated.
When concentrations, temperatures, pressures, dimensions, or other parameters are expressed as ranges of values, the ranges of values should be understood to specifically disclose all ranges formed by any pair of upper values, lower values, or preferred values within the range, regardless of whether the ranges are explicitly recited; for example, if a numerical range of "2 ~ 8" is recited, then the numerical range should be interpreted to include ranges of "2 ~ 7", "2 ~ 6", "5 ~ 7", "3 ~ 4 and 6 ~ 7", "3 ~ 5 and 7", "2 and 5 ~ 7", and the like. Unless otherwise indicated, the numerical ranges recited herein include both the endpoints thereof and all integers and fractions within the numerical range.
The two-component epoxy adhesive and the preparation method thereof provided by the invention are described in detail below. Details which are not described in detail in the embodiments of the invention belong to the prior art which is known to the person skilled in the art. Those not specifically mentioned in the examples of the present invention were carried out according to the conventional conditions in the art or conditions suggested by the manufacturer. The reagents or instruments used in the examples of the present invention are not specified by manufacturers, and are all conventional products available by commercial purchase.
The invention provides a two-component epoxy adhesive for bonding a vehicle skin and a thermal insulation material, which comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 1-2: 1; the component A comprises the following raw materials in parts by mass: 30-60 parts of epoxy resin, 15-40 parts of a toughening agent, 20-45 parts of a filler, 5-10 parts of a reactive diluent, 0-1 part of a coupling agent, 0-1 part of a defoaming agent and 0-1 part of a dispersing agent; the component B comprises the following raw materials in parts by mass: 40-90 parts of curing agent, 5-15 parts of toughening agent, 10-30 parts of filler and 0-5 parts of accelerator; wherein the epoxy resin in the component A adopts at least two of bisphenol A type epoxy resin, bisphenol F type epoxy resin, polyurethane modified epoxy resin and elastomer modified epoxy resin; the toughening agent in the component A adopts at least one of closed polyurethane and nitrile rubber modified epoxy resin; the toughening agent in the component B adopts amino-terminated nitrile rubber.
In some embodiments of the present invention, the filler in the component a is one or two of silica micropowder, calcium carbonate, aluminum hydroxide, polyphosphate, talcum powder and bentonite.
In some embodiments of the present invention, the reactive diluent in the a component is at least one of dodecenyl to tetradecyl glycidyl ether, polypropylene glycol diglycidyl ether, 1, 4-butanediol diglycidyl ether, neopentyl glycol diglycidyl ether, and plant polyene phenol epoxy resin modifier.
In some embodiments of the present invention, the coupling agent in the a component is at least one of gamma- (2, 3-glycidoxy) propyltrimethoxysilane, 3-aminopropyltriethoxysilane, and gamma-mercaptopropyltrimethoxysilane.
In some embodiments of the invention, the defoamer in component a is one of BYK a535, Defom 6800, dow corning ACP001 in pycnoch chemistry.
In some embodiments of the invention, the dispersant in the component A can adopt one of BYK-W9010, BYK-W980, DISPERBYK-111 and DISPERBYK-102 in Pico chemistry.
In some embodiments of the invention, the curing agent in the B component is a polyamide modified with an aliphatic amine and a phenol.
In some embodiments of the present invention, the filler in the component B is one or two of silica micropowder, calcium carbonate, aluminum hydroxide, polyphosphate, talcum powder and bentonite.
In some embodiments of the present invention, the accelerator in the B component is at least one of tertiary amine, imidazole, and nonylphenol.
The invention also provides a preparation method of the two-component epoxy adhesive, which is used for preparing the two-component epoxy adhesive and specifically comprises the following steps:
s1, preparation of the component A: according to the formula of the component A in the two-component epoxy adhesive, the epoxy resin, the flexibilizer, the reactive diluent, the coupling agent, the defoaming agent and the dispersing agent which are required for preparing the component A are added into a reaction kettle, stirred and mixed for 30-50 min at 25-60 ℃, then the filler required for preparing the component A is added into the reaction kettle, stirred and mixed for 50-70 min at 25-60 ℃, and the vacuum is started during stirring and mixing, so that the component A is prepared.
S2, preparation of a component B: according to the formula of the component B in the two-component epoxy adhesive, the curing agent, the toughening agent and the accelerator required for preparing the component B are added into a reaction kettle, stirred and mixed for 30-50 min at 25-60 ℃, then the filler required for preparing the component B is added into the reaction kettle, stirred and mixed for 50-70 min at 25-60 ℃, and vacuum is started during stirring and mixing, so that the component B is prepared.
S3, matching the component A with the component B according to the mass ratio of 1-2: 1, and obtaining the two-component epoxy glue.
Compared with the prior art, the two-component epoxy glue and the preparation method thereof provided by the invention have the following advantages:
(1) the special epoxy resin is adopted in the component A, so that the flexibility of the finally prepared two-component epoxy glue can be reduced, and the toughness is improved, so that the finally prepared two-component epoxy glue has the advantage that the tensile strength and the elongation at break are obviously higher than those of other epoxy glue under the condition of the same flexibility.
(2) The invention adopts the special toughening agent in the component A and the component B simultaneously, the composite toughening method can better improve the toughness and the bonding strength of the final two-component epoxy adhesive, and has better effect than that of only one component containing the toughening agent, in particular, the invention matches the special epoxy resin with the special toughening agent in the component A and the special toughening agent in the component B according to the specific proportion for use, so that the finally prepared two-component epoxy adhesive not only has very high toughness, but also has good 90-degree peel strength when bonding the glass fiber reinforced plastic and the polyurethane heat-insulating material, the hardness of a cured product is between A60 and A80, simultaneously, the preparation method of the two-component epoxy adhesive has simple process and easy operation, can be heated and cured at normal temperature or medium and low temperature not more than 80 ℃, does not need to reach the temperature at which the polyurethane heat-insulating material is easy to deform under pressure, can well meet the bonding requirement of the vehicle skin and the polyurethane thermal insulation material.
(3) According to the invention, the component B adopts polyamide modified by aliphatic amine and phenol as a curing agent, so that the flexibility of the finally prepared two-component epoxy adhesive can be improved, the bonding strength between the finally prepared two-component epoxy adhesive and a base material can be improved, the reaction activity can be improved, the curing rate can be improved, and the curing temperature and time can be reduced, so that the technical effect same as that when an accelerant is used can be achieved under the condition that the accelerant is not used, and the toughness of the finally prepared two-component epoxy adhesive product can be influenced by using the accelerant, therefore, the accelerant can be omitted by adopting the special curing agent, and the toughness and the bonding strength of the finally prepared two-component epoxy adhesive can be improved; particularly, on the basis that the special epoxy resin is matched with the special toughening agent in the component A and the special toughening agent in the component B according to a specific proportion for use, the special epoxy resin is matched with the special curing agent in the component B, so that the toughness and the bonding property of the prepared two-component epoxy glue can be further enhanced, the two-component epoxy glue has good bonding strength to aluminum alloy, glass fiber reinforced plastic and polyurethane heat-insulating materials, the problem of poor 90-degree peel strength of the existing epoxy glue when the glass fiber reinforced plastic and the polyurethane heat-insulating materials are bonded can be more effectively solved, and when the adhesive is used for bonding the vehicle skin and the polyurethane heat-insulating material, the adhesive can be heated and cured at normal temperature or medium and low temperature not higher than 80 ℃, the temperature at which the polyurethane heat-insulating material is easy to deform under pressure is not required to be reached, and the adhesive requirement of the vehicle skin and the polyurethane heat-insulating material can be well met.
(4) The invention has good adhesion and meets the 90-degree peel strength performance requirement of epoxy glue bonded glass fiber reinforced plastic and polyurethane thermal insulation materials.
In conclusion, the embodiment of the invention has high toughness, has good bonding strength for aluminum alloy, glass fiber reinforced plastic and polyurethane thermal insulation materials, can effectively solve the problem of poor 90-degree peel strength of the existing epoxy adhesive when bonding the glass fiber reinforced plastic and the polyurethane thermal insulation materials, can be heated and cured at normal temperature or medium and low temperature of not more than 80 ℃ when bonding the vehicle skin and the polyurethane thermal insulation materials, does not need to reach the temperature at which the polyurethane thermal insulation materials are easy to deform under pressure, and can well meet the bonding requirement of the vehicle skin and the polyurethane thermal insulation materials.
In order to more clearly show the technical scheme and the technical effects provided by the present invention, the two-component epoxy glue and the preparation method thereof provided by the embodiments of the present invention are described in detail in the following with specific embodiments.
Example 1
A double-component epoxy glue is used for bonding a vehicle skin and a thermal insulation material, and the preparation method comprises the following steps:
s1, preparation of the component A:
the formulation of component a is shown in table 1 below:
TABLE 1
| Starting materials | Name of product in prior art | Mass portion of |
| Epoxy resin | Bisphenol F type epoxy resin NPEL-170 | 20 portions of |
| Epoxy resin | Elastomer modified epoxy resin 102C-4L | 20 portions of |
| Toughening agent | Blocked polyurethane Desmocap 14CNB | 26 portions of |
| Reactive diluent | Carbododecenyl to tetradecyl glycidyl ether | 5 portions of |
| Defoaming agent | ACP001 of Dow Corning | 0.01 part |
| Coupling agent | Gamma- (2, 3-glycidoxy) propyltrimethoxysilane | 1.0 part |
| Filler material | Calcium carbonate | 27.99 parts |
According to the formula of the component A in the table 1, the epoxy resin, the toughening agent, the reactive diluent, the coupling agent and the defoaming agent which are required for preparing the component A are added into a reaction kettle, stirred and mixed for 30min at 25-60 ℃, then the filler required for preparing the component A is added into the reaction kettle, stirred and mixed at 25-60 ℃, vacuumizing is started during stirring and mixing, stirring and mixing are stopped after 50min, and vacuumizing is stopped, so that the component A is prepared.
S2, preparation of a component B:
the formula of the component B is shown in the following table 2:
TABLE 2
| Raw materials | Name of product in prior art | Mass portion of |
| Curing agent | Polyamide XH-429 | 52 portions of |
| Curing agent | Polyamide Ancamid 2784 | 15 portions of |
| Toughening agent | Amino-terminated nitrile rubber ATBN 1300*16 | 8 portions of |
| Filler material | Calcium carbonate | 25 portions of |
According to the formula of the component B in the table 2, the curing agent and the toughening agent required for preparing the component B are added into a reaction kettle, stirred and mixed for 40min at 25-60 ℃, then the filler required for preparing the component B is added into the reaction kettle, stirred and mixed at 25-60 ℃, vacuumizing is started during stirring and mixing, stirring and mixing are stopped after 50min, and vacuumizing is stopped, so that the component B is prepared.
Example 2
A double-component epoxy glue is used for bonding a vehicle skin and a heat insulation material, and the preparation method comprises the following steps:
s1, preparation of the component A:
the formulation of component a is shown in table 3 below:
TABLE 3
| Raw materials | Name of product in prior art | Parts by mass |
| Epoxy resin | Bisphenol A type epoxy resin YD-128 | 20 portions of |
| Epoxy resin | Polyurethane modified epoxy resin EPU-73B | 15 portions of |
| Toughening agent | Blocked polyurethane BI 7774 | 26 portions of |
| Reactive diluent | Plant polyene phenol epoxy resin modifier 602 | 6 portions of |
| Defoaming agent | Defom 6800 | 0.05 part |
| Coupling agent | Gamma- (2, 3-glycidoxy) propyltrimethoxysilane | 1.0 part |
| Filler | Calcium carbonate | 31.95 parts |
According to the formula of the component A in the table 3, the epoxy resin, the toughening agent, the reactive diluent, the coupling agent and the defoaming agent which are required for preparing the component A are added into a reaction kettle, stirred and mixed at 25-60 ℃ for 30min, then the filler required for preparing the component A is added into the reaction kettle, the temperature is raised to 30 ℃, stirred and mixed, the vacuumizing is started during the stirring and mixing process, the stirring and mixing are stopped after 60min, and the vacuumizing is stopped, so that the component A is prepared.
S2, preparation of a component B:
the formula of the component B is shown in the following table 4:
TABLE 4
| Raw materials | Name of product in prior art | Mass portion of |
| Curing agent | Polyamide Versamid 140 | 40 portions of |
| Curing agent | Polyamide XH-351 | 35 portions of |
| Toughening agent | Amino-terminated nitrile rubber ATBN 1300 x 16 | 10 portions of |
| Filler | Calcium carbonate | 15 portions of |
According to the formula of the component B in the table 4, the curing agent and the toughening agent required for preparing the component B are added into a reaction kettle, stirred and mixed for 40min at 25-60 ℃, then the filler required for preparing the component B is added into the reaction kettle, stirred and mixed at 25-60 ℃, vacuumizing is started during stirring and mixing, stirring and mixing are stopped after 50min, and vacuumizing is stopped, so that the component B is prepared.
Example 3
A double-component epoxy glue is used for bonding a vehicle skin and a thermal insulation material, and the preparation method comprises the following steps:
s1, preparation of the component A:
the formulation of component a is shown in table 5 below:
TABLE 5
| Raw materials | Name of product in prior art | Mass portion of |
| Epoxy resin | Bisphenol F type epoxy resin NPEF-170 | 10 portions of |
| Epoxy resin | Elastomer modified epoxy resin 102C-4L | 35 portions of |
| Toughening agent | Nitrile rubber modified epoxy resin 861340 | 15 portions of |
| Reactive diluent | Polypropylene glycol diglycidyl ether | 6 portions of |
| Defoaming agent | BYK A535 of Pico chemistry | 0.1 part of |
| Coupling agent | Gamma- (2, 3-glycidoxy) propyltrimethoxysilane | 0.5 portion |
| Filler material | Calcium carbonate | 33.4 parts of |
According to the formula of the component A in the table 5, the epoxy resin, the toughening agent, the reactive diluent, the coupling agent and the defoaming agent which are required for preparing the component A are added into a reaction kettle, stirred and mixed at 25-60 ℃ for 30min, then the filler required for preparing the component A is added into the reaction kettle, stirred and mixed at 25-60 ℃, vacuumizing is started during stirring and mixing, stirring and mixing are stopped after 50min, and vacuumizing is stopped, so that the component A is prepared.
S2, preparation of a component B:
the formulation of component B is shown in table 6 below:
TABLE 6
| Raw materials | Name of product in prior art | Parts by mass |
| Curing agent | Polyamide XH-429 | 55 portions of |
| Curing agent | Polyamide Versamid 140 | 25 portions of |
| Accelerator | Tertiary amine DMP-30 | 2 portions of |
| Toughening agent | Amino-terminated nitrile rubber ATBN 1300 x 16 | 8 portions of |
| Filler material | Calcium carbonate | 10 portions of |
According to the formula of the component B in the table 6, the curing agent, the toughening agent and the accelerator required for preparing the component B are added into a reaction kettle, stirred and mixed for 40min at 25-60 ℃, then the filler required for preparing the component B is added into the reaction kettle, stirred and mixed at 25-60 ℃, vacuumizing is started during stirring and mixing, stirring and mixing are stopped after 50min, and vacuumizing is stopped, so that the component B is prepared.
Comparative example 1
The preparation method of the two-component epoxy glue can comprise the following steps:
s1, preparation of the component A:
the formulation of component a is shown in table 7 below:
TABLE 7
According to the formula of the component A in the table 7, the epoxy resin, the toughening agent, the reactive diluent, the coupling agent and the defoaming agent which are required for preparing the component A are added into a reaction kettle and stirred at 25-60 ℃ for 30min, then the filler which is required for preparing the component A is added into the reaction kettle and stirred at 25-60 ℃, the vacuumizing is started during the stirring process, the stirring is stopped after 50min, and the vacuumizing is stopped, so that the component A is prepared.
S2, preparation of a component B:
the formulation of component B is shown in Table 8 below:
TABLE 8
According to the formula of the component B in the table 8, the curing agent and the accelerator required for preparing the component B are added into a reaction kettle, stirred and mixed for 40min at 25-60 ℃, then the filler required for preparing the component B is added into the reaction kettle, stirred and mixed at 25-60 ℃, vacuumizing is started during stirring and mixing, stirring and mixing are stopped after 50min, and vacuumizing is stopped, so that the component B is prepared.
Comparison of Performance
The following performance tests were performed on the two-component epoxy adhesives prepared in examples 1 to 3 of the present invention and the two-component epoxy adhesive prepared in comparative example 1, respectively:
(1) and (3) detecting the hardness after curing: the post-curing hardness of example 1, example 2, example 3 and comparative example 1 was measured using a durometer in accordance with GB/T531.1-2008, respectively, to obtain the results shown in Table 9 below.
(2) And (3) detecting the tensile shear strength: the tensile shear strengths of example 1, example 2, example 3 and comparative example 1 were respectively measured using a tensile machine in accordance with GB/T7124-.
(3) And (3) detecting the peel strength at 90 ℃: the peel strength at 90 ℃ of example 1, example 2, example 3 and comparative example 1 was measured by a tensile machine according to GJB 130.8-1986, respectively, to obtain the results shown in Table 9 below.
The results of the performance measurements are shown in table 9 below:
TABLE 9
As can be seen from the above examples, comparative examples and Table 9: the adhesive can be cured only at a medium and low temperature of 70 ℃ in the embodiments 1, 2 and 3 of the invention, the temperature at which the polyurethane thermal insulation material is easy to deform under pressure is not required to be reached, and compared with the comparative example 1, the shear strength and the 90-degree peel strength of the embodiments 1, 2 and 3 of the invention are obviously improved, the adhesive has good adhesive strength for aluminum alloy, glass fiber reinforced plastic and polyurethane thermal insulation materials, the problem of too low 90-degree peel strength of epoxy glue when the glass fiber reinforced plastic and the polyurethane thermal insulation material are adhered is effectively solved, and the adhesive requirement of a vehicle skin and the polyurethane thermal insulation material can be well met. As can be seen from the experimental data for tensile strength, elongation at break and 90 ° peel strength in table 1: the toughness of the embodiment 1, the embodiment 2 and the embodiment 3 of the invention is far better than that of the comparative example 1, so that the invention is more suitable for bonding the vehicle skin and the polyurethane heat-insulating material.
In conclusion, the embodiment of the invention has high toughness, has good bonding strength for aluminum alloy, glass fiber reinforced plastic and polyurethane thermal insulation materials, can effectively solve the problem of poor 90-degree peel strength of the existing epoxy adhesive when bonding the glass fiber reinforced plastic and the polyurethane thermal insulation materials, can be heated and cured at normal temperature or medium and low temperature of not more than 80 ℃ when bonding the vehicle skin and the polyurethane thermal insulation materials, does not need to reach the temperature at which the polyurethane thermal insulation materials are easy to deform under pressure, and can well meet the bonding requirement of the vehicle skin and the polyurethane thermal insulation materials.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims. The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art that is already known to a person skilled in the art.
Claims (9)
1. A double-component epoxy adhesive is characterized by comprising a component A and a component B;
the component A comprises the following raw materials in parts by mass: 30-60 parts of epoxy resin, 15-40 parts of a toughening agent, 20-45 parts of a filler, 5-10 parts of a reactive diluent, 0-1 part of a coupling agent, 0-1 part of a defoaming agent and 0-1 part of a dispersing agent;
the component B comprises the following raw materials in parts by mass: 40-90 parts of curing agent, 5-15 parts of toughening agent, 10-30 parts of filler and 0-5 parts of accelerator;
wherein the epoxy resin is at least two of bisphenol A epoxy resin, bisphenol F epoxy resin, polyurethane modified epoxy resin and elastomer modified epoxy resin.
2. The two-component epoxy glue according to claim 1, wherein the toughening agent in the component A is at least one of blocked polyurethane and nitrile rubber modified epoxy resin; the toughening agent in the component B adopts amino-terminated nitrile rubber.
3. The two-component epoxy glue according to claim 1 or 2, characterized in that the curing agent is a polyamide modified with aliphatic amines and phenols.
4. The two-component epoxy adhesive according to claim 1 or 2, wherein the reactive diluent is at least one of a carbon dodecyl to tetradecyl glycidyl ether, a polypropylene glycol diglycidyl ether, a 1, 4-butanediol diglycidyl ether, a neopentyl glycol diglycidyl ether, and a plant polyphenolic epoxy resin modifier.
5. The two-component epoxy glue according to claim 1 or 2, characterized in that the filler in the component A and the filler in the component B are one or two of silica micropowder, calcium carbonate, aluminum hydroxide, polyphosphate, talcum powder and bentonite.
6. The two-component epoxy adhesive according to claim 1 or 2, wherein the coupling agent is at least one of gamma- (2, 3-glycidoxy) propyl trimethoxysilane, 3-aminopropyltriethoxysilane and gamma-mercaptopropyl trimethoxysilane.
7. The two-component epoxy glue of claim 1 or 2, wherein the defoamer is one of BYK a535, Defom 6800, dacon ACP001 from BYK chemical.
8. The two-component epoxy glue according to claim 1 or 2, characterized in that the accelerator is at least one of tertiary amines, imidazoles, nonylphenols.
9. A method of preparing a two-component epoxy glue according to any of the preceding claims 1 to 8, characterized in that it comprises the following steps:
s1, preparation of the component A: according to the formula of the component A in the two-component epoxy adhesive of any one of the claims 1 to 8, adding the epoxy resin, the toughening agent, the reactive diluent, the coupling agent, the defoaming agent and the dispersing agent which are required for preparing the component A into a reaction kettle, mixing for 30-50 min at 25-60 ℃, then adding the filler which is required for preparing the component A into the reaction kettle, mixing for 50-70 min at 25-60 ℃, and opening vacuum during mixing to prepare the component A;
s2, preparation of a component B: according to the formula of the component B in the two-component epoxy glue as claimed in any one of the claims 1 to 8, the curing agent, the toughening agent and the accelerator required for preparing the component B are added into a reaction kettle and mixed for 30-50 min at 25-60 ℃, then the filler required for preparing the component B is added into the reaction kettle and mixed for 50-70 min at 25-60 ℃, and vacuum is opened during mixing, so as to prepare the component B.
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| CN117343683A (en) * | 2023-11-03 | 2024-01-05 | 山东凯恩新材料科技有限公司 | Double-component flexible epoxy adhesive and preparation method thereof |
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