CN115449323B - High-performance magnetic steel bonding epoxy adhesive and preparation method thereof - Google Patents
High-performance magnetic steel bonding epoxy adhesive and preparation method thereof Download PDFInfo
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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
- 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
- C08G59/46—Amides together with other curing agents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/56—Amines together with other curing agents
- C08G59/60—Amines together with other curing agents with amides
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- 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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- 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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—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
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Abstract
The invention discloses a high-performance magnetic steel bonding epoxy adhesive which comprises a resin component and a curing agent component in parts by weight: 0.9:1 to 1.1:1, a step of; the toughening curing agent and the aromatic amine curing agent are added to be matched in a proper range for use, and the light nano calcium carbonate is used for thickening and improving layering precipitation; the epoxy adhesive has good operability and can be applied to vertical surfaces by matching with proper resin components, so that the effects of high Tg and high bonding strength can be obtained; the cured adhesive has strong bonding strength, good vibration resistance and impact resistance, and has enough retention degree and good storage stability within the working range of-40 ℃ to 180 ℃.
Description
Technical Field
The invention relates to the field of adhesives, in particular to a high-performance magnetic steel bonding epoxy adhesive and a preparation method thereof.
Background
With the rapid development of modern science and technology, higher requirements are put on the working stability and safety of various electronic and electric equipment, the requirements on the motor performance are also higher and higher, and a plurality of motors need to operate at high temperature, so that the heat resistance of the adhesive for the motors is also more and more important. The thermal stability of the magnetic steel adhesive has direct influence on the safety and stability of the motor under high-temperature and high-speed operation, the integrity and the adhesiveness of the colloid are maintained at a higher temperature, and meanwhile, the magnetic steel adhesive has good toughness, so that the whole safe operation of the motor can be ensured, and the motor cannot be degummed during high-speed rotation.
For the adhesion of magnetic steel, various types of adhesives have been used in the industry for years, and can be broadly classified into acrylic adhesives, polyurethane adhesives, anaerobic adhesives, epoxy adhesives, and the like.
The acrylic adhesive has the advantages of short bonding time, poor bonding strength, poor durability, long-time magnetic steel falling off, and the like inorganic adhesive, and belongs to a brittle adhesive. When the adhesive is used, auxiliary fixing means such as screws, brackets and the like are usually arranged on the magnetic steel so as to improve the use stability of the motor. The polyurethane adhesive has higher requirements on application environment, poorer operability and poorer capability of resisting environmental corrosivity such as salt mist, water, high temperature and the like. Anaerobic adhesives have the characteristics of quick curing, high bonding strength and the like, but also have the problem of poor performance in the aspects of temperature resistance, high-speed running impact resistance and ring measurement resistance. The single-component anaerobic structural adhesive of the Letai 326 is an anaerobic magnetic tile adhesive with higher awareness in the market, the problems also exist, the low-temperature strength at the temperature of minus 40 ℃ is obviously reduced, the price is very high, and the high-viscosity operation performance is not ideal.
The epoxy resin adhesive has the advantages of high bonding strength to steel, good environmental corrosion resistance, high hardness and Tg, low water absorption and the like, and is always one of the first choice of magnetic steel bonding adhesive research. The early epoxy glue for magnetic steel adhesion uses carboxyl butyl cyanide rubber (CTBN) to toughen the epoxy double-component glue, but contains a solvent, so that the epoxy glue is not environment-friendly. The current epoxy magnetic steel adhesive has developed towards no solvation, and has higher requirements on adhesive strength, impact strength and performance retention rate under high and low temperature conditions, so that adhesive manufacturers are urgently required to develop products with stronger performance.
Disclosure of Invention
The invention aims to provide a magnetic steel bonding epoxy adhesive with high Tg and high bonding strength and a preparation method thereof.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the high-performance magnetic steel bonding epoxy adhesive comprises a resin component and a curing agent component, wherein the resin component and the curing agent component are mixed according to parts by weight: 0.9:1 to 1.1:1, a step of; wherein the resin component comprises the following components:
epoxy resin I which is one or a mixture of a plurality of bisphenol A type, bisphenol F type, cyclic hydrocarbon type, phenolic aldehyde type and other epoxy resins, wherein each molecular structure of each epoxy resin contains 2 epoxy groups on average; the dosage range is 1% -60% of the resin component; the optimal range is 10% -60%.
Epoxy resin II which is one or a mixture of a plurality of multifunctional epoxy resins and contains 3 or more epoxy groups in average in each molecular structure of each epoxy; the dosage range is 1% -60% of the resin component; the most preferred range is 10% to 60%, preferably meta-aminophenol trifunctional epoxy resin (AFG-90) because of its relatively low viscosity for ease of dispersion.
The epoxy resin III is toughened and modified, and the epoxy equivalent in each molecular structure is in the range of 150-800; the dosage range is 1% -40% of the resin component; the optimal range is 5% -35%, and polyurethane modified epoxy resin is preferred, because the interpenetrating network structure contained in the polyurethane modified epoxy resin can provide better shock resistance.
Filler I, the dosage range of which is 1-50% of the resin component; the optimal range is 10% -40%.
The dosage range of the coupling agent I is 2% -4% of the resin component;
the dosage range of the defoamer is 2% -4% of the resin component;
the curing agent comprises the following components in percentage by mass:
the curing agent I is a toughening modified amine curing agent, has an active hydrogen equivalent of 150-250, and the dosage range of the curing agent I is 5-50% of the curing agent component;
the curing agent II is a modified high-temperature-resistant aromatic amine curing agent and has an active hydrogen equivalent of 30-150; the dosage range is 5 to 50 percent of the curing agent component
Filler II, the dosage range of which is 1% -50% of the curing agent component;
the dosage range of the coupling agent II is 2% -4% of the curing agent component.
Preferably, the epoxy resin III is one or a mixture of more than one of rubber modified epoxy resin, polyurethane modified epoxy resin and particle modified epoxy resin.
Further, the curing agent I is prepared by the following method:
a. firstly, carrying out vacuum reaction on Dimer Acid (DA) and Epichlorohydrin (ECH) in a certain proportion at 60 ℃ for 1.5h in the presence of a catalyst to obtain a chlorohydrin ester intermediate;
b. slowly dropwise adding a NaOH solution into a chlorohydrin ester intermediate at a cyclization reaction temperature, maintaining a reaction for 4 hours after the dropwise adding is finished to obtain a dimer acid epoxy DADGE crude product, extracting with toluene, standing, removing salt alkali liquor, washing with water to neutralize to pH=7, and then carrying out reduced pressure distillation on an oil phase to remove excessive Epichlorohydrin (ECH) and toluene to obtain a dimer acid modified epoxy (DADGE) product; c. under the protection of nitrogen, slowly dripping a certain proportion of dimer acid modified epoxy (DADGE) into the IPDA, and carrying out heat preservation reaction for a certain time until the amine value is stable, and ending the amination reaction to obtain the dimer acid toughening modification curing agent.
The dimer acid has good adhesion and softer molecular structure, so the synthesized curing agent I has good adhesion and low temperature resistance.
The curing agent II is prepared by the following method:
d. adding a certain amount of diaminodiphenyl methane (DDM), diphenyl methane Bismaleimide (BDM) and dichloroethane into a container, heating to 65 ℃ under the protection of nitrogen, stirring for dissolution, and carrying out heat preservation reaction for 3 hours;
e. detecting a reaction end point by using a thin layer chromatography (the volume ratio of the developing agent to the acetone/petroleum ether is 1:1), and obtaining the reaction end point after the BDM point disappears;
f. after the reaction, the mixture is distilled under reduced pressure, and the product is washed by absolute ethyl alcohol and subjected to Soxhlet extraction for 24 hours, and then dried in vacuum at 70 ℃ for 12 hours to obtain the product.
Since the finished product of the curing agent II has a large number of rigid benzene rings in the molecular structure, a cured product formed by using the curing agent has high Tg and excellent heat resistance.
Preferably, the filler I comprises one or a mixture of more of asbestos, alumina, kaolin, carbon black, graphite, silica micropowder, silica fume, calcium silicate, diatomite, magnesium oxide, titanium oxide, magnesium hydroxide, aluminum hydroxide, quartz powder, calcium carbonate, magnesium carbonate, barite, mica and clay, and the D50 particle size range is 5-500 microns.
Preferably, the coupling agent I is 3- (2, 3-glycidoxy) propyl trimethoxy silane.
Preferably, the filler II comprises one or a mixture of more of asbestos, alumina, kaolin, carbon black, graphite, silica micropowder, silica fume, calcium silicate, diatomite, magnesium oxide, titanium oxide, magnesium hydroxide, aluminum hydroxide, quartz powder, calcium carbonate, magnesium carbonate, barite, mica and clay, and the D50 particle size range is 5-500 microns. Preferably, the coupling agent II is gamma-aminopropyl triethoxysilane.
Preferably, the defoaming agent is one or a mixture of more of organosilicon defoaming agents and acrylic acid ester defoaming agents.
The invention also provides a method for preparing the high-performance magnetic steel bonding epoxy adhesive, which comprises the following steps:
the preparation method of the resin component comprises the following steps: the components are proportionally added into a power mixer to be heated to 60 ℃, and are discharged and packaged after being dispersed in vacuum for 1 to 2 hours under proper revolution and rotation speed;
the preparation method of the curing agent component comprises the following steps: the components are proportionally added into a power mixer to be heated to 60 ℃, vacuum dispersed for 1-2 hours under proper revolution and rotation speed, discharged and packaged:
when in use, the resin component and the curing agent component are mixed and stirred uniformly according to a certain proportion.
The invention develops a double-component epoxy resin adhesive which is used for bonding motor magnetic steel sheets; the epoxy adhesive has good operation performance and can be applied to vertical surface; the cured adhesive has strong bonding strength, good vibration resistance and impact resistance, and has enough retention degree and good storage stability within the working range of-40 ℃ to 180 ℃. The storage stability of one year is ensured.
The dimer acid polyamide curing agent and the aromatic amine curing agent are used in the invention to provide good adhesive force and higher Tg point respectively, and proper filler is used to improve the compatibility, and the product prepared by the method still has a shearing strength of 24MPa when the Tg is up to 192 ℃.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, but the scope of the present invention is not limited thereto.
The invention provides a high-performance magnetic steel bonding epoxy adhesive which comprises a resin component and a curing agent component, wherein the resin component and the curing agent component are mixed according to parts by weight: 0.9:1 to 1.1:1, a step of; wherein, the liquid crystal display device comprises a liquid crystal display device,
the resin component comprises:
a. epoxy resin I: the epoxy resin is one or a mixture of a plurality of bisphenol A type, bisphenol F type, cyclic hydrocarbon type, phenolic aldehyde type and other types of epoxy resins, and each molecular structure of each epoxy resin contains 2 epoxy groups on average. The dosage range is 1% -60% of the resin component, and the optimal range is 10% -60%.
b. Epoxy resin II: the epoxy resin is multifunctional epoxy resin, can be one or a mixture of a plurality of epoxy resins, and contains 3 or more epoxy groups in average in each molecular structure of each epoxy resin. The dosage range is 1% -60% of the resin component, and the optimal range is 10% -60%.
c. Epoxy resin III: for toughening one or a mixture of several of modified epoxy resins such as rubber modified epoxy resin, polyurethane modified epoxy resin, particle modified epoxy resin, etc., and the epoxy equivalent in each molecular structure is in the range of 150-800. The dosage range is 1-40% of the resin component, and the optimal range is 5-35%.
d. The filler comprises one or a mixture of more of asbestos, alumina, kaolin, carbon black, graphite, silica powder, silica fume, calcium silicate, diatomite, magnesium oxide, titanium oxide, magnesium hydroxide, aluminum hydroxide, quartz powder, calcium carbonate, magnesium carbonate, barite, mica and clay, and the D50 particle size range is 5-500 microns. The dosage range is 1-50% of the resin component, and the optimal range is 10-40%.
e. Coupling agent, 3- (2, 3-epoxypropoxy) propyl trimethoxy silane (WD-60). The dosage range is 2% -4% of the resin component.
f. Defoaming agent: and (3) an organic silicon defoamer or an acrylic ester defoamer, and one or more of the organic silicon defoamer and the acrylic ester defoamer are mixed for use. The dosage range is 2% -4% of the resin component.
The resin component is produced through the process of adding the materials into a planetary stirring kettle, opening the dispersing disc and stirring at 25-30 Hz and 15-20 Hz. After stirring for 20 minutes, the kettle is cleaned once, and stirring rods, a dispersing disc or substances which are not stirred uniformly on the wall of the kettle are cleaned into the kettle. Then the dispersion and stirring are started again, the stirring rotation speed is controlled to be between 15 and 20Hz, the dispersion rotation speed is controlled to be between 15 and 20Hz, the large vacuum is gradually opened until the vacuum degree is controlled to be between-0.08 and-0.1 Mpa, and the materials are discharged after pressure maintaining and stirring for about 1.5 to 2 hours.
The curing agent comprises the following components:
a. curing agent I: the toughening modified amine curing agent has an active hydrogen equivalent of 150-250. The dosage range is 5% -50% of the curing agent component, and the optimal range is 15% -25%.
b. Curing agent II: the modified high temperature resistant aromatic amine curing agent has an active hydrogen equivalent weight of 30-150. The dosage range is 5% -50% of the curing agent component, and the optimal range is 15% -25%.
c. Filler I: comprises one or a mixture of more of asbestos, alumina, kaolin, carbon black, graphite, silicon micropowder, silica fume, calcium silicate, diatomite, magnesium oxide, titanium oxide, magnesium hydroxide, aluminum hydroxide, quartz powder, calcium carbonate, magnesium carbonate, barite, mica and clay, and the D50 particle size range is 5-500 microns. Light nano calcium carbonate is preferred. The dosage range is 1% -50% of the curing agent component, the optimal range is 10% -80%, and the optimal range is 20% -70%.
d. A coupling agent, gamma-aminopropyl triethoxysilane. The dosage range is 2% -4% of the curing agent component.
The curing agent component is prepared through metering the materials into a planetary stirring kettle, opening the dispersing disc and stirring at 25-30 Hz, and controlling the dispersing speed to 15-20 Hz. After stirring for 20 minutes, the kettle is cleaned once, and stirring rods, a dispersing disc or substances which are not stirred uniformly on the wall of the kettle are cleaned into the kettle. Then the dispersion and stirring are started again, the stirring rotation speed is controlled to be between 15 and 20Hz, the dispersion rotation speed is controlled to be between 15 and 20Hz, the large vacuum is gradually opened until the vacuum degree is controlled to be between-0.08 and-0.1 Mpa, and the materials are discharged after pressure maintaining and stirring for about 1.5 to 2 hours.
The double-component epoxy adhesive prepared by the implementation method has the following excellent properties: high adhesion strength, good cold and hot shock resistance and good vibration resistance.
The main raw materials used in the following examples are given below:
bisphenol F type epoxy resin: 862 epoxy resin, shell
Bisphenol a epoxy resin: 128 epoxy resin, south Asia
M-aminophenol trifunctional epoxy resins: AFG-90, shanghai Hua Yi
Polyurethane toughened epoxy resin: 73B, ADEKA
Epoxy coupling agent: WD-60, wuda
Amino coupling agent: WD-50, wuda
Defoaming agent: 6800, a modesty
Toughening curing agent I: homemade
High temperature resistant curing agent II: homemade
Modified polyamide curing agents: new Material technology Co.Ltd in Guangdong;
modified aromatic amine curing agent: jinan Langsheng New Material technologies Co., ltd;
the weight ratio of the resin component to the curing agent component is 1:1, pull shear data in examples and comparative examples, tested with reference to standard GB T7124-2008.
Glass transition temperatures in examples and comparative examples were measured using differential scanning calorimeter analysis (DSC), instrument model HITACHI DSC. The motor complete machine test in the examples and the comparative examples is performed by a motor manufacturer, and specific items and test methods are as follows:
low temperature test (see GB/T2423.1-2008): a. and placing the motor complete machine into a low-temperature box at-40 ℃ for 2 hours, wherein the motor is in a non-electrified state. The insulation resistance was then tested while maintained at-40 ℃. The specific judgment threshold value is determined by a manufacturer according to the model of the motor. b. The motor complete machine in a low temperature state is electrified, and the inspection machine can be started in a normal idle mode. c. And after the motor environment is restored to be normal, the working voltage is adjusted to be rated voltage, so that the motor works under the conditions of continuous torque and continuous power, and whether the system can work normally is checked.
High temperature test (see GB/T2423.2-2008): a. the motor was placed in an oven at 85 ℃ for 2 hours with the motor in a non-energized state. And then, keeping the temperature at 85 ℃ to check whether the grease in the motor bearing overflows or not, and retesting the insulation resistance. The specific judgment threshold value is determined by a manufacturer according to the model of the motor. b. And after the motor environment is restored to be normal, the working voltage is adjusted to be rated voltage, so that the motor works under the conditions of continuous torque and continuous power, and whether the system can work normally is checked. c. The motor is put into an oven at 85 ℃ and then electrified, the working voltage is adjusted to be rated voltage, so that the motor works under the conditions of continuous torque and continuous power, the driving motor can be checked to work normally for 2 hours, and the insulation resistance is retested under the high-temperature condition after 2 hours. The specific binding threshold is determined by the manufacturer according to the motor model.
Vibration resistance test: a. the test for vibration resistance to frequency sweep was set to a level of severity with reference to the requirements of 5.6.4.1.1 in GB/T18488.1-2015, and then tested as specified in GB/T2423.10-2008. b. Random vibration tests were set to a severity level with reference to the requirements of 5.6.4.1.1 in GB/T18488.1-2015 and then tested as specified in GB/T28046.3-2011. After the two vibration tests are completed, whether the parts are damaged or not and whether the fastener is loosened or not are checked. After the motor returns to normal state, the motor working voltage is set to rated voltage, the driving motor works under the continuous torque and continuous power conditions, and the motor can be checked to work normally.
Performance comparison of examples and comparative examples
It can be seen from the data of examples and comparative examples that products with excellent balance of properties can be obtained by carrying out the technical scheme according to the invention, whereas the obtained products are defective. As is clear from the results in comparative example 3, the product formulation obtained by the method of the present invention has a significantly better effect than the product formulation obtained after the conventional similar products on the market are matched.
The high-performance magnetic steel bonding epoxy adhesive has excellent product performance and good competitiveness in comparison of similar products in the market. The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (9)
1. The high-performance magnetic steel bonding epoxy adhesive is characterized by comprising a resin component and a curing agent component in parts by weight: 0.9: 1-1.1: 1, a step of; wherein the resin component comprises the following components:
epoxy resin I which is one or a mixture of a plurality of bisphenol A type, bisphenol F type, cyclic hydrocarbon type and phenolic aldehyde type epoxy resins, wherein each molecular structure of each epoxy resin contains 2 epoxy groups on average; the dosage range is 1% -60% of the resin component;
epoxy resin II which is one or a mixture of a plurality of multifunctional epoxy resins and contains 3 or more epoxy groups in average in each molecular structure of each epoxy; the dosage range is 1% -60% of the resin component;
the epoxy resin III is toughened and modified, and the epoxy equivalent weight of each molecular structure is in the range of 150-800; the dosage range is 1% -40% of the resin component;
the amount of the filler I ranges from 1% to 50% of the resin component;
the dosage range of the coupling agent I is 2% -4% of the resin component;
the using amount of the defoaming agent ranges from 2% to 4% of the resin component;
the curing agent comprises the following components in percentage by mass:
the curing agent I is a toughening modified amine curing agent, has an active hydrogen equivalent of 150-250, and the dosage of the curing agent I is 5-50% of the components of the curing agent;
the curing agent II is a modified high-temperature-resistant aromatic amine curing agent and has an active hydrogen equivalent of 30-150; the dosage range is 5% -50% of the curing agent component;
the using amount of the filler II is 1% -50% of the curing agent component;
the dosage range of the coupling agent II is 2% -4% of the curing agent component;
the curing agent I is prepared by the following method:
a. firstly, carrying out vacuum reaction on dimer acid and epoxy chloropropane in a certain proportion in the presence of a catalyst for a period of time to obtain a chlorohydrin ester intermediate;
b. slowly dropwise adding a NaOH solution into the chlorohydrin ester intermediate at the cyclization reaction temperature, maintaining the reaction for a period of time after the dropwise adding is finished to obtain a dimer acid epoxy DADGE crude product, extracting with toluene, standing, removing salt alkali liquor, washing with water to neutralize to pH=7, and then carrying out reduced pressure distillation on an oil phase to remove excessive epichlorohydrin and toluene to obtain a dimer acid modified epoxy product;
c. slowly dripping a certain proportion of dimer acid modified epoxy into IPDA under the protection of nitrogen, and carrying out heat preservation reaction for a certain time until the amine value is stable, and obtaining the dimer acid toughening modification curing agent after the amination reaction is finished;
the curing agent II is prepared by the following method:
d. adding a certain amount of diaminodiphenyl methane, diphenyl methane bismaleimide and dichloroethane into a container, heating, stirring, dissolving and reacting for a period of time under the protection of nitrogen;
e. detecting a reaction end point by using a thin layer chromatography method, and obtaining the reaction end point after the BDM point disappears;
f. after the reaction, the mixture is distilled under reduced pressure, and the product is washed by absolute ethyl alcohol and subjected to Soxhlet extraction for a period of time, and then vacuum drying is carried out, thus obtaining the product.
2. The high performance magnetic steel bonding epoxy glue of claim 1, wherein: the epoxy resin III is one or a mixture of more of rubber modified epoxy resin, polyurethane modified epoxy resin and particle modified epoxy resin.
3. The high performance magnetic steel bonding epoxy glue of claim 1, wherein: the filler I comprises one or a mixture of more of asbestos, alumina, kaolin, carbon black, graphite, silica micropowder, silica fume, calcium silicate, diatomite, magnesium oxide, titanium oxide, magnesium hydroxide, aluminum hydroxide, quartz powder, calcium carbonate, magnesium carbonate, barite, mica and clay, and the D50 particle size range is 5-500 microns.
4. The high performance magnetic steel bonding epoxy glue of claim 1, wherein: the coupling agent I is 3- (2, 3-glycidoxy) propyl trimethoxy silane.
5. The high performance magnetic steel bonding epoxy glue of claim 1, wherein: the filler II comprises one or a mixture of more of asbestos, alumina, kaolin, carbon black, graphite, silica micropowder, silica fume, calcium silicate, diatomite, magnesium oxide, titanium oxide, magnesium hydroxide, aluminum hydroxide, quartz powder, calcium carbonate, magnesium carbonate, barite, mica and clay, and the D50 particle size range is 5-500 microns.
6. The high performance magnetic steel bonding epoxy glue of claim 1, wherein: the coupling agent II is gamma-aminopropyl triethoxysilane.
7. The high performance magnetic steel bonding epoxy glue of claim 1, wherein: the defoaming agent is one or a mixture of more of organic silicon defoaming agents and acrylic ester defoaming agents.
8. The high performance magnetic steel bonding epoxy glue of claim 1, wherein: the resin component comprises:
the dosage range of the epoxy resin I is 10% -60% of the resin component;
the dosage range of the epoxy resin II is 10% -60% of the resin component;
the dosage range of the epoxy resin III is 5% -35% of the resin component;
the amount of the filler I ranges from 10% to 40% of the resin component;
the dosage range of the coupling agent I is 2% -4% of the resin component;
the using amount of the defoaming agent ranges from 2% to 4% of the resin component;
the curing agent comprises the following components:
the dosage range of the curing agent I is 15% -25% of the curing agent component;
the dosage range of the curing agent II is 15% -25% of the curing agent component
The using amount of the filler II is 1% -50% of the curing agent component;
the dosage range of the coupling agent II is 2% -4% of the curing agent component.
9. A method for preparing the high-performance magnetic steel bonding epoxy adhesive according to any one of claims 1-8, which is characterized in that:
the preparation method of the resin component comprises the following steps: the components are proportionally added into a power mixer to be heated to 60 ℃, and the materials are discharged and packaged after being dispersed in vacuum for 1-2 hours under proper revolution and rotation speed;
the preparation method of the curing agent component comprises the following steps: the components are proportionally added into a power mixer to be heated to 60 ℃, vacuum dispersed for 1-2 hours under proper revolution and rotation speed, discharged and packaged:
when in use, the resin component and the curing agent component are mixed and stirred uniformly according to a certain proportion.
Priority Applications (1)
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| JP2004156024A (en) * | 2002-10-15 | 2004-06-03 | Dainippon Ink & Chem Inc | Epoxy resin composition, production method for epoxy resin, new epoxy resin and new phenol resin |
| CN1748045A (en) * | 2003-02-03 | 2006-03-15 | 新日本制铁株式会社 | Flat rolled magnetic steel sheet or strip having its surface coated for bonding |
| JP2007254710A (en) * | 2005-11-29 | 2007-10-04 | Ajinomoto Co Inc | Resin composition for interlayer insulation layer of multi-layer printed circuit board |
| CN106753132A (en) * | 2016-12-29 | 2017-05-31 | 南通高盟新材料有限公司 | A kind of halogen-free flame-resistant high-temperature-resistant tough epoxy adhesive and preparation method thereof |
| JP2019194322A (en) * | 2018-04-27 | 2019-11-07 | ナガセケムテックス株式会社 | adhesive |
| CN113549417A (en) * | 2021-07-19 | 2021-10-26 | 广东恒大新材料科技有限公司 | Fast-curing high-strength epoxy adhesive |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8440746B2 (en) * | 2010-12-02 | 2013-05-14 | Ppg Industries Ohio, Inc | One component epoxy structural adhesive composition prepared from renewable resources |
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| JP2004156024A (en) * | 2002-10-15 | 2004-06-03 | Dainippon Ink & Chem Inc | Epoxy resin composition, production method for epoxy resin, new epoxy resin and new phenol resin |
| CN1748045A (en) * | 2003-02-03 | 2006-03-15 | 新日本制铁株式会社 | Flat rolled magnetic steel sheet or strip having its surface coated for bonding |
| JP2007254710A (en) * | 2005-11-29 | 2007-10-04 | Ajinomoto Co Inc | Resin composition for interlayer insulation layer of multi-layer printed circuit board |
| CN106753132A (en) * | 2016-12-29 | 2017-05-31 | 南通高盟新材料有限公司 | A kind of halogen-free flame-resistant high-temperature-resistant tough epoxy adhesive and preparation method thereof |
| JP2019194322A (en) * | 2018-04-27 | 2019-11-07 | ナガセケムテックス株式会社 | adhesive |
| CN113549417A (en) * | 2021-07-19 | 2021-10-26 | 广东恒大新材料科技有限公司 | Fast-curing high-strength epoxy adhesive |
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| CN115449323A (en) | 2022-12-09 |
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