CN115572562A - Bi-component epoxy resin and preparation method and application thereof - Google Patents
Bi-component epoxy resin and preparation method and application thereof Download PDFInfo
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- CN115572562A CN115572562A CN202211395075.5A CN202211395075A CN115572562A CN 115572562 A CN115572562 A CN 115572562A CN 202211395075 A CN202211395075 A CN 202211395075A CN 115572562 A CN115572562 A CN 115572562A
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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
- 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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- 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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Abstract
The invention provides a preparation method of bi-component epoxy resin, which comprises the following steps: reacting bisphenol F epoxy resin and polyetheramine to produce a first component; reacting tetraglycidyl amine type epoxy resin and polybutadiene rubber to generate a second component; mixing polyamide, triethylene tetramine and aluminum hydroxide to prepare a third component; mixing the first component and the second component to produce a two-component epoxy resin precursor, mixing the two-component epoxy resin precursor and a bisphenol a epoxy resin to produce a first product, mixing the first product, a silane coupling agent, and aluminum hydroxide to produce a main agent material; the third component and the main agent material are mixed to prepare the bi-component epoxy resin, so that the problem of poor high temperature resistance of the bi-component epoxy resin under the conditions of high strength and high peeling is solved. The invention also provides a bi-component epoxy resin and application thereof.
Description
Technical Field
The invention relates to the technical field of bi-component epoxy resin, in particular to bi-component epoxy resin and a preparation method and application thereof.
Background
The bi-component epoxy resin is composed of a resin component and a curing agent component, and is a structural adhesive with wide application because the mixing proportion of the bi-component epoxy resin is adjustable, the mixing is convenient, and the performance of the cured product is balanced.
The tetraglycidyl amine type epoxy resin used in the two-component epoxy resin has high Tg point after curing and good temperature resistance, and is very suitable for occasions with high temperature resistance requirements, but in practical application, the peeling strength of a cured product is poor due to the molecular structure characteristics, so that the application range of the tetraglycidyl amine type epoxy resin is limited.
Due to the self-relationship of the two-component epoxy resin, the high-temperature resistance of the cured product is defective, and even if the product of the two-component epoxy resin normal-temperature curing system is subjected to heating post-curing treatment, the temperature resistance of the product is still poor, so that the high-temperature resistance requirement under the conditions of high strength and high peeling is difficult to meet.
Therefore, there is a need to develop a two-component epoxy resin, a method for preparing the same, and applications thereof, which avoid the above problems in the prior art.
Disclosure of Invention
The invention aims to provide a bi-component epoxy resin and a preparation method and application thereof, and solves the problem that the bi-component epoxy resin has poor high-temperature resistance under the conditions of high strength and high peeling.
In order to achieve the purpose, the preparation method of the two-component epoxy resin comprises the following steps:
reacting a bisphenol F epoxy resin and a polyetheramine to produce a first component;
reacting tetraglycidyl amine type epoxy resin and polybutadiene rubber to generate a second component;
mixing polyamide, triethylene tetramine and aluminum hydroxide to prepare a third component;
mixing the first component and the second component to produce a two-component epoxy resin precursor, mixing the two-component epoxy resin precursor and a bisphenol a epoxy resin to produce a first product, mixing the first product, a silane coupling agent, and aluminum hydroxide to produce a main agent material;
mixing the third component and the main agent material to prepare the two-component epoxy resin.
The preparation method of the bi-component epoxy resin has the beneficial effects that: the method comprises the steps of reacting bisphenol F epoxy resin and polyether amine to generate a first component, reacting tetraglycidyl amine epoxy resin and polybutadiene rubber to generate a second component, wherein due to the fact that the tetraglycidyl amine epoxy resin is high in viscosity and the bisphenol F epoxy resin is low in viscosity, the bisphenol F epoxy resin and the polyether amine are firstly used to react to generate the first component, and therefore the polyether amine is not prone to implosion at high temperature; mixing the first component and the second component to prepare a two-component epoxy resin precursor, wherein the shortcoming of low cohesive strength of the polyetheramine is overcome due to high cohesive strength of the tetraglycidyl amine type epoxy resin; the dual-component epoxy resin is prepared by mixing the dual-component epoxy resin precursor and bisphenol A epoxy resin to prepare a first product, mixing the first product, a silane coupling agent and aluminum hydroxide to prepare a main agent material, and mixing the third component and the main agent material to prepare the dual-component epoxy resin.
Preferably, the step of reacting to form the first component using a bisphenol F epoxy resin and a polyetheramine comprises: and mixing the bisphenol F epoxy resin and the polyether amine, heating, stirring and reacting to obtain the first component, sealing and storing the first component, and placing the first component to normal temperature for later use. The beneficial effects are that: because the tetraglycidyl amine type epoxy resin has high viscosity and the bisphenol F epoxy resin has low viscosity, the bisphenol F epoxy resin and the polyether amine are mixed firstly, so that the polyether amine is not easy to implode under the high-temperature reaction.
Preferably, the weight part ratio of the bisphenol F epoxy resin to the polyether amine is (1-5): 1.
Preferably, the first component comprises the following components in parts by weight: 100-150 parts of bisphenol F epoxy resin and 30-100 parts of polyether amine.
Preferably, the step of reacting the tetraglycidyl amine type epoxy resin and the polybutadiene type rubber to form the second component comprises: grinding the polybutadiene rubber, mixing the ground polybutadiene rubber with the tetraglycidyl amine type epoxy resin, heating, stirring and reacting to obtain the second component, sealing and storing the second component, and placing the second component at normal temperature for later use. The beneficial effects are that: the polybutadiene rubber is ground to be mixed with the tetraglycidyl amine type epoxy resin, and due to the high temperature resistance of the tetraglycidyl amine type epoxy resin and the capability of toughening the polybutadiene rubber and having small influence on Tg, the polybutadiene rubber can be cured at normal temperature, and the cured bicomponent epoxy resin has good high temperature resistance and stripping performance.
Preferably, the weight part ratio of the tetraglycidyl amine type epoxy resin to the polybutadiene rubber is (2-5): 1.
Preferably, the second component comprises the following components in parts by weight: 100-150 parts of tetraglycidyl amine epoxy resin and 30-50 parts of polybutadiene rubber.
Preferably, the temperature for the temperature-rising stirring reaction is 50-100 ℃, and the time for the temperature-rising stirring reaction is 0.5-5h.
Preferably, the weight part ratio of the first component to the second component is 1 (1-8).
Preferably, the two-component epoxy resin precursor comprises the following components in parts by weight: the first component is 20-80 parts by weight, and the second component is 100-150 parts by weight.
Preferably, the weight part ratio of the two-component epoxy resin precursor to the bisphenol A epoxy resin is (1.6-10): 1.
Preferably, the first product comprises the following components in parts by weight: 100-150 parts of the two-component epoxy resin precursor and 15-60 parts of the bisphenol A epoxy resin.
Preferably, the main agent material comprises the following components in parts by weight: 115-210 parts of the first product, 1-5 parts of the silane coupling agent and 25-65 parts of aluminum hydroxide.
Preferably, the silane coupling agent is KH-560.
Preferably, the weight part ratio of the third component to the main agent material is (0.35-1): 1.
Preferably, the two-component epoxy resin comprises the following components in parts by weight: 35-100 parts of the third component and 100 parts of the main agent material.
Preferably, the third component comprises the following components in parts by weight: 30-50 parts of polyamide, 1-5 parts of triethylene tetramine and 45-70 parts of aluminum hydroxide.
Preferably, the mesh number of the aluminum hydroxide is 600-2000 meshes.
The invention also aims to provide a two-component epoxy resin prepared by the preparation method of the two-component epoxy resin, which comprises the following specific steps: reacting bisphenol F epoxy resin and polyetheramine to produce a first component; reacting tetraglycidyl amine type epoxy resin and polybutadiene rubber to generate a second component; mixing polyamide, triethylene tetramine and aluminum hydroxide to prepare a third component; mixing the first component and the second component to produce a two-component epoxy resin precursor, mixing the two-component epoxy resin precursor and a bisphenol A epoxy resin to produce a first product, mixing the first product, a silane coupling agent, and aluminum hydroxide to produce a main agent material; mixing the third component and the main agent material to prepare the two-component epoxy resin.
The bicomponent epoxy resin has the beneficial effects that: the bi-component epoxy resin can be cured at normal temperature, and the cured bi-component epoxy resin has good high temperature resistance and stripping performance, so that the problems of poor stripping strength and poor shearing strength at high temperature of the bi-component epoxy resin are solved.
Preferably, the two-part epoxy resin has a shear strength of 1.2 to 6.9MPa at 200 ℃.
The invention further aims to provide application of the two-component epoxy resin, wherein the two-component epoxy resin is used for mounting and bonding a liquid cooling system of a new energy automobile. The traditional process for installing the liquid cooling system of the new energy automobile is welding, the liquid cooling pipe is easy to damage and crack in installation, the problem that the liquid cooling pipe is easy to damage when installed by the traditional process can be solved by adopting the double-component epoxy resin for bonding, the bonding construction process is simple to operate, and the factory productivity can be greatly improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. Unless defined otherwise, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs. As used herein, the word "comprising" and similar words are intended to mean that the element or item listed before the word covers the element or item listed after the word and its equivalents, but does not exclude other elements or items.
In an embodiment of the invention, a preparation method of a two-component epoxy resin comprises the following steps:
reacting bisphenol F epoxy resin and polyetheramine to produce a first component;
reacting tetraglycidyl amine type epoxy resin and polybutadiene rubber to generate a second component;
mixing polyamide, triethylene tetramine and aluminum hydroxide to prepare a third component;
mixing the first component and the second component to produce a two-component epoxy resin precursor, mixing the two-component epoxy resin precursor and a bisphenol a epoxy resin to produce a first product, mixing the first product, a silane coupling agent, and aluminum hydroxide to produce a main agent material;
mixing the third component and the main agent material to prepare the two-component epoxy resin.
In some embodiments of the present invention, the bisphenol F epoxy resin is a low viscosity bisphenol F epoxy resin, and the polyetheramine is any one of polyetheramine D2000 and polyetheramine T403.
In some embodiments of the present invention, the tetraglycidyl amine epoxy resin is tetraglycidyl amine epoxy resin MF-4101H/AG-80.
In some embodiments of the invention, the polyamide is selected from any one of Yingchuang 350A, kening V140, shanghai Junjiang D8140.
Specifically, bisphenol F epoxy resin and polyetheramine are used for reaction to generate a first component, and tetraglycidyl amine epoxy resin and polybutadiene rubber are used for reaction to generate a second component, so that the tetraglycidyl amine epoxy resin has high viscosity, and the bisphenol F epoxy resin has low viscosity, so that the bisphenol F epoxy resin and the polyetheramine are used for reaction to generate the first component, and the polyetheramine is not easy to implode at high temperature; mixing the first component and the second component to prepare a two-component epoxy resin precursor, wherein the shortcoming of low cohesive strength of the polyetheramine is overcome due to high cohesive strength of the tetraglycidyl amine type epoxy resin; the dual-component epoxy resin is prepared by mixing the dual-component epoxy resin precursor and bisphenol A epoxy resin to prepare a first product, mixing the first product, a silane coupling agent and aluminum hydroxide to prepare a main agent material, and mixing the third component and the main agent material to prepare the dual-component epoxy resin.
In some embodiments of the invention, the step of reacting to form the first component using a bisphenol F epoxy resin and a polyetheramine comprises:
mixing the bisphenol F epoxy resin and the polyether amine, heating, stirring and reacting to obtain the first component, sealing and storing the first component, and placing the first component to normal temperature for later use. Because the tetraglycidyl amine type epoxy resin is high in viscosity and the bisphenol F epoxy resin is low in viscosity, the bisphenol F epoxy resin and the polyether amine are mixed, so that the polyether amine is not prone to implosion in a reaction at high temperature.
In some embodiments of the invention, the weight parts ratio of the bisphenol F epoxy resin to the polyetheramine is (1-5): 1. In yet other embodiments, the ratio of parts by weight of the bisphenol F epoxy resin to the polyetheramine is any one of 1. In some more specific embodiments, the first component comprises the following components in parts by weight: 100-150 parts of bisphenol F epoxy resin and 30-100 parts of polyether amine.
In some embodiments of the present invention, the step of reacting the tetraglycidyl amine type epoxy resin with the polybutadiene based rubber to form the second component comprises:
grinding the polybutadiene rubber, mixing the ground polybutadiene rubber with the tetraglycidyl amine type epoxy resin, heating, stirring and reacting to obtain the second component, sealing and storing the second component, and placing the second component at normal temperature for later use. The polybutadiene rubber is ground to be mixed with the tetraglycidyl amine type epoxy resin, and due to the high temperature resistance of the tetraglycidyl amine type epoxy resin and the capability of toughening the polybutadiene rubber and having small influence on Tg, the polybutadiene rubber can be cured at normal temperature, and the cured bicomponent epoxy resin has good high temperature resistance and stripping performance.
In some embodiments of the invention, the weight part ratio of the tetraglycidyl amine type epoxy resin to the polybutadiene based rubber is (2-5): 1. In still other embodiments, the ratio of the tetraglycidyl amine type epoxy resin to the polybutadiene-based rubber is any one of 2, 1, 3, 4. In some more specific embodiments, the second component comprises the following components in parts by weight: 100-150 parts of tetraglycidyl amine type epoxy resin and 30-50 parts of polybutadiene rubber.
In some embodiments of the invention, the temperature of the temperature-raising stirring reaction is 50 ℃ to 100 ℃, and the time of the temperature-raising stirring reaction is 0.5 h to 5h.
In some embodiments of the invention, the ratio of parts by weight of the first component to the second component is 1 (1-8). In still other embodiments, the ratio of parts by weight of the first component to the second component is any one of 1. In some more specific embodiments, the two-part epoxy resin precursor comprises the following components in parts by weight: the first component is 20-80 parts by weight, and the second component is 100-150 parts by weight.
In some embodiments of the present invention, the ratio of parts by weight of the two-part epoxy resin precursor and the bisphenol A epoxy resin is (1.6-10): 1. In yet other specific embodiments, the ratio of parts by weight of the two-part epoxy resin precursor and the bisphenol a epoxy resin is any one of 1.6. In some more specific embodiments, the first product comprises the following components in parts by weight: 100-150 parts of the two-component epoxy resin precursor and 15-60 parts of the bisphenol A epoxy resin.
In some specific embodiments of the present invention, the main agent material comprises the following components in parts by weight: 115-210 parts of the first product, 1-5 parts of the silane coupling agent and 25-65 parts of aluminum hydroxide.
In some more specific embodiments of the invention, the silane coupling agent is KH-560.
In some embodiments of the present invention, the weight portion ratio of the third component to the main agent material is (0.35-1): 1. In still other embodiments, the ratio of the third component to the main material in parts by weight is any one of 0.35. In some more specific embodiments, the two-part epoxy resin comprises the following components in parts by weight: 35-100 parts of the third component and 100 parts of the main agent material.
In some embodiments of the present invention, the third component comprises the following components in parts by weight: 30-50 parts of polyamide, 1-5 parts of triethylene tetramine and 45-70 parts of aluminum hydroxide.
In some embodiments of the invention, the aluminum hydroxide has a mesh size of 600-2000 mesh.
In an embodiment of the invention, a two-component epoxy resin is provided, and the two-component epoxy resin is prepared by a preparation method of the two-component epoxy resin. The method comprises the following specific steps: reacting a bisphenol F epoxy resin and a polyetheramine to produce a first component; reacting tetraglycidyl amine type epoxy resin and polybutadiene rubber to generate a second component; mixing polyamide, triethylene tetramine and aluminum hydroxide to prepare a third component; mixing the first component and the second component to produce a two-component epoxy resin precursor, mixing the two-component epoxy resin precursor and a bisphenol A epoxy resin to produce a first product, mixing the first product, a silane coupling agent, and aluminum hydroxide to produce a main agent material; mixing the third component and the main agent material to prepare the two-component epoxy resin. The bi-component epoxy resin can be cured at normal temperature, and the cured bi-component epoxy resin has good high temperature resistance and stripping performance, so that the problems of poor stripping strength and poor shearing strength at high temperature of the bi-component epoxy resin are solved.
In some embodiments of the invention, the two-part epoxy resin has a shear strength of 1.2 to 6.9MPa at 200 ℃.
The embodiment of the invention provides application of a two-component epoxy resin, wherein the two-component epoxy resin is used for mounting and bonding a liquid cooling system of a new energy automobile. The traditional process for installing the liquid cooling system of the new energy automobile is welding, the liquid cooling pipe is easy to damage and crack in installation, the problem that the liquid cooling pipe is easy to damage when installed by the traditional process can be solved by adopting the double-component epoxy resin for bonding, the bonding construction process is simple to operate, and the factory productivity can be greatly improved.
In some embodiments of the invention, the bisphenol F epoxy resin is produced by a south Asia manufacturer, model number NPEF-170; the manufacturer of the polyether amine is Hensman with the model of D2000; the manufacturer of the tetraglycidyl amine type epoxy resin is Hubei Zhengzheng Feng, and the model is MF-4101; the manufacturer of the polybutadiene rubber is Japan centralization, and the model is M-210; the polyamide is created by a manufacturer with the model number of 350A; the manufacturer of the triethylene tetramine is Hensman, and the model is TETA; the bisphenol A epoxy resin is produced in south Asia and is NPEL-128 in model number; the manufacturer of the silane coupling agent is Shanghai shellfish, and the model is KH-560.
In some embodiments of the invention, the tetraglycidyl amine epoxy resin is manufactured by Andebao, model AG-80; the polyamide is produced by a stretching manufacturer in Kening, and the model is V140. In yet other embodiments, the polyamide is produced by a shanghai junjiang model number D8140.
In some embodiments of the invention, the step of reacting to form the first component using a bisphenol F epoxy resin and a polyetheramine comprises:
and mixing the bisphenol F epoxy resin and the polyether amine, heating, stirring and reacting to obtain the first component, sealing and storing the first component, and placing the first component to normal temperature for later use.
Specifically, the method comprises the following steps:
weighing 100 parts by weight of bisphenol F epoxy resin in a 500ml three-neck flask, putting the bisphenol F epoxy resin in a heating jacket, and stirring for 10min at the temperature of 30 ℃; slowly adding 30 parts by weight of polyetheramine T403 into a 500ml three-neck flask filled with the bisphenol F epoxy resin during stirring, reacting for 5 hours at the reaction temperature of 50 ℃, obtaining the first component 1 after the reaction is finished, sealing and storing the first component 1, and placing the first component 1 to normal temperature for later use.
Specifically, the method comprises the following steps:
weighing 150 parts by weight of bisphenol F epoxy resin in a 500ml three-neck flask, putting the bisphenol F epoxy resin in a heating jacket, and stirring for 30min at the temperature of 30 ℃; slowly adding 100 parts by weight of the polyetheramine D2000 into a 500ml three-neck flask filled with the bisphenol F epoxy resin during stirring, reacting for 30min at the reaction temperature of 100 ℃, obtaining the first component 2 after the reaction is finished, sealing and storing the first component 2, and placing the first component to normal temperature for later use.
Specifically, the method comprises the following steps:
weighing 125 parts by weight of bisphenol F epoxy resin in a 500ml three-neck flask, putting the bisphenol F epoxy resin in a heating jacket, and stirring for 15min at the temperature of 30 ℃; and slowly adding 65 parts by weight of the polyetheramine D2000 into a 500ml three-neck flask filled with the bisphenol F epoxy resin during stirring, reacting for 3 hours at the reaction temperature of 75 ℃, obtaining the first component 3 after the reaction is finished, sealing and storing the first component 3, and placing the first component to normal temperature for later use.
In some embodiments of the present invention, the step of reacting tetraglycidyl amine epoxy resin and polybutadiene rubber to form the second component comprises:
grinding the polybutadiene rubber, mixing the ground polybutadiene rubber with the tetraglycidyl amine type epoxy resin, heating, stirring and reacting to obtain the second component, sealing and storing the second component, and placing the second component at normal temperature for later use.
Specifically, the method comprises the following steps:
weighing 30 parts by weight of the polybutadiene rubber, grinding the polybutadiene rubber by a three-roll grinder, adjusting the maximum gap to 10 micrometers and the minimum gap to 5 micrometers, grinding the polybutadiene rubber for more than 2 times until the fineness is tested by a fineness plate, mixing and stirring the polybutadiene rubber with 100 parts by weight of the tetraglycidyl amine type epoxy resin MF-4101H/AG-80 at the rotating speed of 2000r/min for 4min, and reacting for 5H at the temperature of 50 ℃; and obtaining the second component 1 after the reaction is finished, sealing and storing the second component 1, and placing the second component 1 to normal temperature for later use.
Specifically, the method comprises the following steps:
weighing 50 parts by weight of the polybutadiene rubber, grinding by a three-roll grinder, adjusting the maximum gap to 10 micrometers and the minimum gap to 5 micrometers, grinding for more than 2 times until the fineness is tested by a fineness plate, mixing and stirring with 150 parts by weight of the tetraglycidyl amine type epoxy resin MF-4101H/AG-80 at the rotating speed of 2000r/min, reacting for 30min at the temperature of 100 ℃ after stirring for 4min, obtaining the second component 2 after the reaction is finished, sealing and storing the second component 2, and placing the second component 2 at the normal temperature for later use.
Specifically, the method comprises the following steps:
weighing 40 parts by weight of the polybutadiene rubber, grinding the polybutadiene rubber by a three-roll grinder, adjusting the maximum gap to 10 micrometers and the minimum gap to 5 micrometers, grinding the polybutadiene rubber for more than 2 times until the fineness is tested by a fineness plate, mixing and stirring the polybutadiene rubber and 125 parts by weight of the tetraglycidyl amine type epoxy resin MF-4101H/AG-80 at the rotating speed of 2000r/min for 4min, and reacting for 3H at the temperature of 75 ℃; and obtaining the second component 3 after the reaction is finished, sealing and storing the second component 3, and placing the second component at normal temperature for later use.
In some embodiments of the invention, the polyamide, triethylene tetramine, and aluminum hydroxide are mixed to produce the third component.
Specifically, the method comprises the following steps:
weighing 30 parts by weight of polyamide and 2 parts by weight of triethylene tetramine, putting the polyamide and the triethylene tetramine into a 500ml sample mixing cup, putting the polyamide and the triethylene tetramine into a sample mixing machine, mixing and stirring at the rotating speed of 2000r/min, and stirring for 4min to prepare a mixture 1; adding 45 parts by weight of 2000-mesh aluminum hydroxide into the mixture 1, mixing and stirring at the rotating speed of 1500r/min, and stirring for 5min to obtain a crude product of the third component 1; and mixing and stirring the crude product of the third component 1 at the rotating speed of 2000r/min and the vacuum degree of 90kPa for 5min to obtain the third component 1 for later use.
Specifically, the method comprises the following steps:
weighing 40 parts by weight of polyamide and 4 parts by weight of triethylene tetramine, putting the polyamide and the triethylene tetramine into a 500ml sample mixing cup, putting the polyamide and the triethylene tetramine into a sample mixing machine, mixing and stirring at the rotating speed of 2000r/min, and stirring for 4min to prepare a mixture 2; adding 60 parts by weight of 2000-mesh aluminum hydroxide into the mixture 2, mixing and stirring at the rotating speed of 1500r/min, and stirring for 5min to obtain a crude product of the third component 2; and mixing and stirring the crude product of the third component 2 at the rotating speed of 2000r/min and the vacuum degree of 90kPa for 5min to obtain the third component 2 for later use.
Specifically, the method comprises the following steps:
weighing 50 parts by weight of polyamide and 5 parts by weight of triethylene tetramine, putting the polyamide and the triethylene tetramine into a 500ml sample mixing cup, putting the polyamide and the triethylene tetramine into a sample mixing machine, mixing and stirring at the rotating speed of 2000r/min, and stirring for 4min to prepare a mixture 3; adding 70 parts by weight of 2000-mesh aluminum hydroxide into the mixture 3, mixing and stirring at the rotating speed of 1500r/min, and stirring for 5min to obtain a crude product of the third component 3; and mixing and stirring the crude product of the third component 3 at the rotating speed of 2000r/min and under the vacuum degree of 90kPa for 5min to obtain the third component 3 for later use.
In some embodiments of the invention, the first component and the second component are mixed to produce a two-part epoxy resin precursor, the two-part epoxy resin precursor and the bisphenol a epoxy resin are mixed to produce a first product, and the first product, the silane coupling agent, and the aluminum hydroxide are mixed to produce a base compound material.
Specifically, the method comprises the following steps:
weighing 100 parts by weight of the second component 1 and 20 parts by weight of the first component 1, placing the second component 1 and the first component 1 into a 500ml sample mixing cup, placing the two components into a sample mixing machine, mixing and stirring the two components at a rotating speed of 2000r/min for 5min to obtain a two-component epoxy resin precursor 1, weighing 100 parts by weight of the two-component epoxy resin precursor 1 and 15 parts by weight of the bisphenol A epoxy resin, placing the two components into the 500ml sample mixing cup, placing the two components into the sample mixing machine, mixing and stirring the two components at a rotating speed of 1500r/min for 5min to obtain a first product 1, placing the first product 1, 2 parts by weight of KH-560 and 25 parts by weight of 2000-mesh aluminum hydroxide into the sample mixing machine, mixing and stirring the two components at a rotating speed of 1000r/min to obtain a crude product of the main agent material 1 after stirring for 5min; and mixing and stirring the crude product of the main agent material 1 at the rotating speed of 2000r/min and under the vacuum degree of 90kPa for 5min to obtain the main agent material 1 for later use.
Specifically, the method comprises the following steps:
weighing 150 parts by weight of the second component 2 and 80 parts by weight of the first component 2, placing the second component 2 and 80 parts by weight of the first component 2 in a 500ml sample mixing cup, placing the two components in a sample mixing machine, mixing and stirring at a rotating speed of 2000r/min, stirring for 5min to obtain the two-component epoxy resin precursor 2, weighing 150 parts by weight of the two-component epoxy resin precursor 2 and 60 parts by weight of the bisphenol A epoxy resin, placing the two components in a 500ml sample mixing cup, placing the two components in a sample mixing machine, mixing and stirring at a rotating speed of 1500r/min, stirring for 5min to obtain a first product 2, placing the first product 2, 5 parts by weight of KH-560 and 65 parts by weight of 2000-mesh aluminum hydroxide in a sample mixing machine, mixing and stirring at a rotating speed of 1000r/min, and stirring for 5min to obtain a crude product of the main agent material 2; and mixing and stirring the crude product of the main agent material 2 at the rotating speed of 2000r/min and the vacuum degree of 90kPa for 5min to obtain the main agent material 2 for later use.
Specifically, the method comprises the following steps:
weighing 125 parts by weight of the second component 3 and 50 parts by weight of the first component 3, placing the second component 3 and 50 parts by weight of the first component 3 into a 500ml sample mixing cup, placing the two components into a sample mixing machine, mixing and stirring the two components at the rotating speed of 2000r/min, stirring the two components for 5min to obtain a two-component epoxy resin precursor 3, weighing 125 parts by weight of the two-component epoxy resin precursor 3 and 40 parts by weight of the bisphenol A epoxy resin, placing the two components into the 500ml sample mixing cup, placing the two components into the sample mixing machine, mixing and stirring the two components at the rotating speed of 1500r/min, stirring the two components for 5min to obtain a first product 3, placing the first product 3, 3 parts by weight of KH-560 and 45 parts by weight of 2000-mesh aluminum hydroxide into the sample mixing machine, mixing and stirring the mixture at the rotating speed of 1000r/min to obtain a crude product of the main agent material 3 after stirring for 5min; and mixing and stirring the crude product of the main agent material at the rotating speed of 2000r/min and under the vacuum degree of 90kPa for 5min to obtain a main agent material 3 for later use.
In some embodiments of the present invention, the third component and the host material are reacted to produce the two-part epoxy resin.
Examples 1 to 5
Examples 1-5 of the present invention each provide a two-part epoxy resin having the specific composition shown in table 2, in parts by weight.
TABLE 2
The preparation method of the bi-component epoxy resin comprises the following steps:
reacting the third component and the host material to produce the two-part epoxy resin.
Comparative example
Putting 40 parts by weight of bisphenol A epoxy resin, 3 parts by weight of KH-560 and 45 parts by weight of 2000-mesh aluminum hydroxide into a 500ml sample mixing cup, putting into a sample mixing machine, mixing and stirring at the rotating speed of 1000r/min, and stirring for 5min to obtain a crude product of a main agent material; and (3) mixing and stirring the crude product of the main agent material at the rotating speed of 2000r/min and under the vacuum degree of 90kPa for 5min to obtain the main agent material for later use.
Weighing 40 parts by weight of polyamide and 4 parts by weight of triethylene tetramine, placing the polyamide and the triethylene tetramine in a 500ml sample mixing cup, placing the polyamide and the triethylene tetramine in a sample mixing machine, mixing and stirring at the rotating speed of 2000r/min, adding 60 parts by weight of 2000-mesh aluminum hydroxide in the sample mixing cup after stirring for 4min, mixing and stirring at the rotating speed of 1500r/min, and stirring for 5min to obtain a crude product of the third component; and mixing and stirring the crude product of the third component at the rotating speed of 2000r/min and under the vacuum degree of 90kPa for 5min to obtain a third component for later use.
55 parts by weight of the third component and 100 parts by weight of the main agent material were reacted to prepare a two-component epoxy resin.
Performance evaluation:
the two-component epoxy resins obtained in examples 1 to 5 and comparative example were tested for shear strength, tensile modulus, T-peel force, and thermal conductivity, and the test results are shown in table 3.
Property parameters of the two-component epoxy resin described in Table 3
As can be seen from Table 3, the shear strength of the two-part epoxy resin of the present invention is still effective at a temperature of 200 ℃ while the shear strength of the two-part epoxy resin of the comparative example is not effective at a temperature of 200 ℃; the two-component epoxy resin of the present invention is also substantially superior to the two-component epoxy resin of the comparative example in terms of tensile strength, tensile modulus, T peel force, thermal conductivity, and the like.
The two-component epoxy resin is used for mounting and bonding a liquid cooling system of a new energy automobile, and solves the problem that a liquid cooling pipe is damaged and cracked easily due to welding in the traditional process. The two-component epoxy resin has low reduction rate of shear strength at high temperature, can provide enough bonding strength when a liquid cooling pipe is heated, and cannot separate parts in a liquid cooling system.
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Where the claims recite a range of values, such ranges are intended to include all sub-ranges subsumed therein, and variations within the ranges are intended to be encompassed by the claims as appended hereto where possible.
Claims (12)
1. The preparation method of the two-component epoxy resin is characterized by comprising the following steps:
reacting bisphenol F epoxy resin and polyetheramine to produce a first component;
reacting tetraglycidyl amine type epoxy resin and polybutadiene rubber to generate a second component;
mixing polyamide, triethylene tetramine and aluminum hydroxide to prepare a third component;
mixing the first component and the second component to produce a two-component epoxy resin precursor, mixing the two-component epoxy resin precursor and a bisphenol A epoxy resin to produce a first product, mixing the first product, a silane coupling agent, and aluminum hydroxide to produce a main agent material;
mixing the third component and the host material to produce the two-part epoxy resin.
2. The method of claim 1, wherein the step of reacting a bisphenol F epoxy resin and a polyetheramine to form a first component comprises:
and mixing the bisphenol F epoxy resin and the polyether amine, heating, stirring and reacting to obtain the first component, sealing and storing the first component, and placing the first component to normal temperature for later use.
3. The method of claim 1 or 2, wherein the weight parts ratio of the bisphenol F epoxy resin to the polyetheramine is (1-5): 1.
4. The method of preparing two-component epoxy resin according to claim 1, wherein the step of reacting tetraglycidyl amine type epoxy resin and polybutadiene type rubber to form the second component comprises:
grinding the polybutadiene rubber, mixing the ground polybutadiene rubber with the tetraglycidyl amine type epoxy resin, heating, stirring and reacting to obtain the second component, sealing and storing the second component, and placing the second component at normal temperature for later use.
5. The process for producing a two-component epoxy resin according to claim 1 or 4, wherein the ratio of the tetraglycidyl amine type epoxy resin to the polybutadiene-based rubber in parts by weight is (2-5): 1.
6. The method for preparing two-component epoxy resin according to claim 2 or 4, wherein the temperature of the temperature-rising stirring reaction is 50-100 ℃ and the time of the temperature-rising stirring reaction is 0.5-5h.
7. The method for preparing two-component epoxy resin according to claim 1, wherein the ratio of the weight parts of the first component to the second component is 1 (1-8).
8. The method of claim 1, wherein the weight parts ratio of the two-part epoxy resin precursor to the bisphenol a epoxy resin is (1.6-10): 1.
9. The method for preparing two-component epoxy resin according to claim 1, wherein the ratio of the weight parts of the third component to the main agent material is (0.35-1): 1.
10. Two-component epoxy resin, characterized in that it is prepared by the process for the preparation of a two-component epoxy resin according to any one of claims 1 to 9.
11. The two-part epoxy resin according to claim 10, wherein the two-part epoxy resin has a shear strength of 1.2 to 6.9MPa at 200 ℃.
12. Use of the two-component epoxy resin according to any one of claims 10 to 11 for the mounting and adhesion of liquid cooling systems in new energy vehicles.
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