CN113929875A - Curing agent for epoxy interface agent suitable for being used in humid environment, epoxy interface agent and application of curing agent - Google Patents

Curing agent for epoxy interface agent suitable for being used in humid environment, epoxy interface agent and application of curing agent Download PDF

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Publication number
CN113929875A
CN113929875A CN202111376177.8A CN202111376177A CN113929875A CN 113929875 A CN113929875 A CN 113929875A CN 202111376177 A CN202111376177 A CN 202111376177A CN 113929875 A CN113929875 A CN 113929875A
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epoxy
agent
parts
amine
component
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包来燕
喻明洋
任银霞
朱永斌
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Shanghai Gomidt New Material Technology Co ltd
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Shanghai Gomidt New Material Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates 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
    • C08G59/18Macromolecules 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
    • C08G59/40Macromolecules 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
    • C08G59/62Alcohols or phenols
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates 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
    • C08G59/18Macromolecules 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
    • C08G59/40Macromolecules 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
    • C08G59/44Amides
    • C08G59/46Amides together with other curing agents
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates 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
    • C08G59/18Macromolecules 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
    • C08G59/40Macromolecules 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
    • C08G59/50Amines
    • C08G59/56Amines together with other curing agents
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates 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
    • C08G59/18Macromolecules 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
    • C08G59/68Macromolecules 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 catalysts used
    • C08G59/686Macromolecules 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 catalysts used containing nitrogen
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D163/00Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Epoxy Resins (AREA)

Abstract

The invention belongs to the technical field of interface agents, and provides a curing agent for an epoxy interface agent, the epoxy interface agent and application thereof, wherein the curing agent is suitable for being used in a humid environment. The curing agent for the epoxy interface agent suitable for being used in a humid environment comprises the following components in parts by weight: 44-68 parts of phenolic amine, 28-35 parts of polyamide, 2-16 parts of polyether amine and 2-5 parts of epoxy accelerator. The curing agent for the epoxy interface agent, which is suitable for being used in a humid environment, compounds the phenolic aldehyde amine, the polyamide and the polyether amine, and the phenolic aldehyde amine, the polyamide and the polyether amine do not react with water and carbon dioxide in the air under the humid environment to cause failure, so that the curing agent for the epoxy interface agent can successfully play a role in curing in the humid environment, and the bonding strength of the epoxy interface agent is ensured; in addition, as the phenolic aldehyde amine has a rigid structure, the polyamide and the polyether amine have flexible structures, and the epoxy interface agent with higher elongation at break and tensile strength can be obtained by adopting a proper proportion.

Description

Curing agent for epoxy interface agent suitable for being used in humid environment, epoxy interface agent and application of curing agent
Technical Field
The invention relates to the technical field of interface agents, in particular to a curing agent for an epoxy interface agent, the epoxy interface agent and application thereof, wherein the curing agent is suitable for being used in a humid environment.
Background
The epoxy interface agent is obtained by reacting a material A and a material B of two components, wherein: epoxy resin (bisphenol A resin and bisphenol F resin), reactive diluent, coupling agent and some auxiliary agents form a material A of the epoxy interface agent; the amine curing agent forms the material B of the epoxy interface agent. Epoxy interfacial agents are generally suitable for use in dry environments because: the amine curing agent in the material B is usually aliphatic amine which has good solubility in water, so that ammonium salt can be easily reacted with water and carbon dioxide in a humid environment to obtain ammonium salt, active hydrogen on the amino group is ineffective, the ammonium salt can not react with an epoxy group in the material A, a normally cured epoxy interface agent is difficult to obtain, and the bonding strength of the epoxy interface agent is reduced. In order to obtain an epoxy interfacial agent that can be normally cured in a humid environment, modified amine-based curing agents such as phenol-aldehyde amines and polyamides are generally used. The phenolic aldehyde amine can be directly cured under water, so that the epoxy interface agent has better water resistance, the reaction speed is high or low, and the rigid structure of the phenolic aldehyde can cause the elongation at break of a cured product to be lower. Polyamides do not cure underwater but are fully workable in humid environments, the products are less water resistant than the phenalkamines and the reaction rate is usually slower but more flexible than the phenalkamines.
Disclosure of Invention
In view of the above, the present invention aims to provide a curing agent for an epoxy interfacial agent suitable for use in a humid environment, an epoxy interfacial agent and applications thereof. The curing agent for the epoxy interface agent can be used in a humid environment.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a curing agent for an epoxy interface agent, which is suitable for being used in a humid environment and comprises the following components in parts by weight:
44-68 parts of phenolic amine, 28-35 parts of polyamide, 2-16 parts of polyether amine and 2-5 parts of epoxy accelerator.
Preferably, the phenolic aldehyde amine comprises a first phenolic aldehyde amine and a second phenolic aldehyde amine, and the active hydrogen equivalent of the first phenolic aldehyde amine and the second phenolic aldehyde amine is 97; the curing speed of the first phenolic aldehyde amine is higher than that of the second phenolic aldehyde amine; the mass ratio of the first phenolic aldehyde amine to the second phenolic aldehyde amine is 20: 80-35: 65.
preferably, the polyamide has an active hydrogen equivalent weight of 110.
Preferably, the polyetheramine comprises a first polyetheramine or a second polyetheramine; the first polyetheramine has a difunctional average molecular weight of 2000; the second polyetheramine has a trifunctional average molecular weight of 5000.
Preferably, the epoxy accelerator comprises a tertiary amine; the tertiary amine comprises triethanolamine, methyldiethanolamine and aminophenols; the aminophenols include 2,4, 6-tris (dimethylaminomethyl) phenol.
The invention also provides an epoxy interface agent suitable for being used in a humid environment, which comprises a component A and a component B which are independently packaged, wherein the component A comprises the following components in parts by weight:
73-88 parts of epoxy resin, 10-23 parts of glycidyl ether and 2-4 parts of silane coupling agent;
the epoxy resin is an epoxy resin mixture comprising bisphenol A resin and bisphenol F resin;
the glycidyl ethers include C12-14 alkyl glycidyl ethers;
the component B is the curing agent for the epoxy interfacial agent which is suitable for being used in a humid environment and is described in the technical scheme;
the mass ratio of the component A to the component B is 100: 35-100: 55.
preferably, the mass ratio of the bisphenol a resin to the bisphenol F resin in the epoxy resin mixture is 10: 90-65: 35.
preferably, the glycidyl ethers further comprise 1, 6-hexanediol diglycidyl ether; when the glycidyl ether is a mixed glycidyl ether of C12-14 alkyl glycidyl ether and 1, 6-hexanediol diglycidyl ether, the mass fraction of the C12-14 alkyl glycidyl ether in the mixed glycidyl ether is 30-70%.
Preferably, the silane coupling agent includes one or more of gamma- (2, 3-glycidoxy) propyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, vinyltriethoxysilane, and vinyltrimethoxysilane.
The invention also provides the application of the epoxy interface agent suitable for being used in a humid environment in concrete, metal and wood.
The invention provides a curing agent for an epoxy interface agent, which is suitable for being used in a humid environment and comprises the following components in parts by weight: 44-68 parts of phenolic amine, 28-35 parts of polyamide, 2-16 parts of polyether amine and 2-5 parts of epoxy accelerator. The curing agent for the epoxy interface agent, which is suitable for being used in a humid environment, compounds the phenolic aldehyde amine, the polyamide and the polyether amine, and the phenolic aldehyde amine, the polyamide and the polyether amine do not react with water and carbon dioxide in the air under the humid environment to cause failure, so that the curing agent for the epoxy interface agent can successfully play a role in curing in the humid environment, and the bonding strength of the epoxy interface agent is ensured; meanwhile, the epoxy interface agent has proper surface drying time and pot life by reasonably controlling the weight parts of the phenolic amine, the polyamide and the polyether amine. In addition, as the phenolic aldehyde amine has a rigid structure, the polyamide and the polyether amine have flexible structures, and the epoxy interface agent with higher elongation at break and tensile strength can be obtained by adopting a proper proportion.
The invention also provides an epoxy interface agent suitable for being used in a humid environment, which comprises a component A and a component B which are independently packaged, wherein the component A comprises the following components in parts by weight: 73-88 parts of epoxy resin, 10-23 parts of glycidyl ether and 2-4 parts of silane coupling agent; the epoxy resin is an epoxy resin mixture comprising bisphenol A resin and bisphenol F resin; the glycidyl ethers include C12-14 alkyl glycidyl ethers; the component B is the curing agent for the epoxy interfacial agent which is suitable for being used in a humid environment and is described in the technical scheme; the mass ratio of the component A to the component B is 100: 35-100: 55. the epoxy interface agent has excellent water resistance and is suitable for being used in a humid environment. Meanwhile, the epoxy interface agent can be coated on the base surfaces of concrete, metal, wood and the like to be used as an interface agent, has excellent bonding performance and better flexibility, and has the tensile strength of more than 25MPa and the elongation at break of more than 10 percent after being cured in air at room temperature for 28 days. In addition, the epoxy interface agent is convenient to use, can be used only by mixing the component A and the component B at room temperature, and is simple to operate in a using method; and has good operability time, namely the surface drying time at 23 ℃ is 3-4 hours, and the working life is about 1 hour.
Detailed Description
The invention provides a curing agent for an epoxy interface agent, which is suitable for being used in a humid environment and comprises the following components in parts by weight:
44-68 parts of phenolic amine, 28-35 parts of polyamide, 2-16 parts of polyether amine and 2-5 parts of epoxy accelerator.
In the present invention, the starting materials used in the present invention are preferably commercially available products unless otherwise specified.
The curing agent for the epoxy interface agent suitable for being used in a humid environment comprises 44-68 parts by weight of phenolic aldehyde amine, preferably 45-65 parts by weight, more preferably 50-60 parts by weight, and even more preferably 55 parts by weight. In the present invention, the phenolic amine preferably includes a first phenolic amine and a second phenolic amine; the curing speed of the first phenolic aldehyde amine is preferably greater than the curing speed of the second phenolic aldehyde amine; the mass ratio of the first phenolic aldehyde amine to the second phenolic aldehyde amine is preferably 20: 80-35: 65. in the present invention, the first phenolic amine preferably comprises one or more of a changzhou mountain SX5622 curing agent, a changzhou mountain SX5253 curing agent, and a changzhou mountain PAA4816D curing agent; the second hydroxyamine preferably comprises one or more of a Changzhou mountain PAA4812G curative, a Changzhou mountain LT4928F curative, and a Changzhou mountain PAA 4922F. In the present invention, the active hydrogen equivalent of the phenolic amine is independently preferably 97. In the invention, the main differences of the first phenolic aldehyde amine and the second phenolic aldehyde amine are reaction speed, cured product tensile strength and cured product elongation at break; the first phenolic aldehyde amine has a high curing speed, and the obtained cured product has high tensile strength and low elongation at break; the second phenol-aldehyde amine has a slower curing speed, and the obtained product has lower tensile strength and higher elongation at break than the first phenol-aldehyde amine. The invention controls the mass ratio of the first phenolic aldehyde amine with higher curing speed to the second phenolic aldehyde amine with lower curing speed to be 20: 80-35: 65, the epoxy interface agent can be endowed with a faster curing rate; the phenolic aldehyde amine has a rigid structure, so that the tensile strength of the epoxy interface agent is improved.
The curing agent for the epoxy interface agent suitable for being used in a humid environment comprises, by weight, 28-35 parts of polyamide, preferably 29-34 parts, more preferably 30-33 parts, and even more preferably 31-32 parts, based on the weight parts of the phenolic aldehyde amine. In the present invention, the active hydrogen equivalent of the polyamide is preferably 110. In the invention, the polyamide is preferably adida 498 polyamide, in the invention, the polyamide can be cured in a humid environment, and the cured product has good water resistance; compared with a phenolic aldehyde amine curing agent, the polyamide has a slower curing rate, and can endow the epoxy interface agent with higher elongation at break and longer pot life; the polyamide is matched with the phenolic aldehyde amine, so that a relatively proper curing speed can be obtained.
Based on the weight portion of the phenolic aldehyde amine, the curing agent for the epoxy interface agent suitable for being used in a humid environment comprises 2-16 parts of polyether amine, preferably 5-15 parts, more preferably 8-14 parts, and even more preferably 9-11 parts. In the present invention, the polyetheramine preferably includes a first polyetheramine or a second polyetheramine; the bifunctional average molecular weight of the first polyetheramine is preferably 2000 (abbreviated as D2000), and more preferably hensmyl polyetheramine D2000; the trifunctional average molecular weight of the second polyetheramine is preferably 5000 (abbreviated as T5000), and more preferably hensmyl polyetheramine T5000. In the invention, although the water resistance of the polyether amine is lower than that of the phenolic amine and the polyamide, the dosage of the polyether amine is less, and the high molecular weight flexible chain segment contained in the molecular structure can endow the epoxy interface agent with higher elongation at break, thereby further improving the flexibility of the epoxy interface agent.
Based on the weight portion of the phenolic aldehyde amine, the curing agent for the epoxy interface agent suitable for being used in a humid environment comprises 2-5 parts by weight of an epoxy accelerator, and preferably 3-4 parts by weight of the epoxy accelerator. In the present invention, the epoxy accelerator preferably includes a tertiary amine; the tertiary amine preferably comprises triethanolamine, methyldiethanolamine and aminophenols; the aminophenols preferably comprise 2,4, 6-tris (dimethylaminomethyl) phenol (abbreviated DMP-30). In the invention, the epoxy accelerator can obviously shorten the surface drying time of the epoxy interface agent and improve the construction efficiency; and the tensile strength of the epoxy interface agent can be further improved.
The preparation method of the curing agent for epoxy interfacial agent suitable for use in humid environment is not specifically limited in the present invention, and the curing agent can be prepared by a method well known to those skilled in the art.
The invention also provides an epoxy interface agent suitable for being used in a humid environment, which comprises a component A and a component B which are independently packaged, wherein the component A comprises the following components in parts by weight:
73-88 parts of epoxy resin, 10-23 parts of glycidyl ether and 2-4 parts of silane coupling agent;
the epoxy resin is an epoxy resin mixture comprising bisphenol A resin and bisphenol F resin;
the glycidyl ethers include C12-14 Alkyl Glycidyl Ethers (AGEs);
the component B is the curing agent for the epoxy interfacial agent which is suitable for being used in a humid environment and is described in the technical scheme;
the mass ratio of the component A to the component B is 100: 35-100: 55.
the component A in the epoxy interface agent suitable for being used in a humid environment comprises 73-88 parts by weight of epoxy resin, preferably 75-85 parts by weight, and more preferably 80 parts by weight. In the present invention, the epoxy resin is an epoxy resin mixture including a bisphenol a resin and a bisphenol F resin; the mass ratio of bisphenol a resin to bisphenol F resin in the epoxy resin mixture is preferably 10: 90-65: 35.
based on the weight portion of the epoxy resin, the component A in the epoxy interface agent suitable for being used in a humid environment comprises 10-23 parts of glycidyl ether by weight, and preferably 15-20 parts. In the present invention, the glycidyl ether includes C12-14 alkyl glycidyl ether. In the present invention, the glycidyl ether preferably further includes 1, 6-hexanediol diglycidyl ether; when the glycidyl ether is preferably a mixed glycidyl ether of C12-14 alkyl glycidyl ether and 1, 6-hexanediol diglycidyl ether, the mass fraction of the C12-14 alkyl glycidyl ether in the mixed glycidyl ether is preferably 30-70%.
Based on the weight portion of the epoxy resin, the component A in the epoxy interface agent suitable for being used in a humid environment comprises 2-4 parts of silane coupling agent by weight, and preferably 3 parts. In the present invention, the silane coupling agent preferably includes one or more of γ - (2, 3-glycidoxy) propyltrimethoxysilane (abbreviated as KH560), γ -aminopropyltriethoxysilane (KH550), γ - (methacryloyloxy) propyltrimethoxysilane (KH570), vinyltriethoxysilane (KH151) and vinyltrimethoxysilane (KH171), and more preferably, KH 560. In the present invention, the silane coupling agent is more preferably KH560, and since KH560 contains an epoxy group in its molecular structure, it has better compatibility with bisphenol a resins and bisphenol F resins.
In the invention, the component A preferably also comprises an auxiliary agent; the auxiliary agent preferably comprises a defoaming agent and a wetting agent; the mass of the defoaming agent is preferably 0.3 percent of the total mass of the component A and the component B except the auxiliary agent; the mass of the wetting agent is preferably 0.2% of the total mass of the A component and the B component except the auxiliary agent. In the present invention, the antifoaming agent preferably includes a BYK 066N antifoaming agent; the wetting agent preferably comprises a eucarb 493U wetting agent.
The component B of the epoxy interface agent provided by the invention is the curing agent for the epoxy interface agent suitable for being used in a humid environment, which is described in the technical scheme. The composition of the curing agent is preferably consistent with the technical scheme, and is not described again.
In the invention, the mass ratio of the component A to the component B in the epoxy interface agent is 100: 35-100: 55.
the preparation method of the component A and the component B is not particularly limited, and the resin is prepared by adopting a preparation method of a mixture of resin by a person skilled in the art.
In the present invention, when the epoxy interfacial agent is used, it is preferable to mix and use the A-component and the B-component in situ. In the invention, the on-site mixing is preferably carried out under the condition of stirring, the rotating speed of the stirring is preferably 800-1400 rpm, and the time is preferably 2-5 min.
The invention also provides the application of the epoxy interface agent suitable for being used in a humid environment in concrete, metal and wood.
The following examples are provided to illustrate the curing agent for epoxy interfacial agent and the epoxy interfacial agent suitable for use in humid environment and the application thereof, but they should not be construed as limiting the scope of the present invention.
Example 1
1. Taking the preparation of 1kg of epoxy interface agent as an example, the component A and the component B are respectively prepared according to the following formula.
Preparing a component A: 332.89g of bisphenol A resin, 249.81g of bisphenol F resin, 87.41g of AGE, 87.48g of KH56017, 2.98g of BYK 066N defoaming agent and 1.99g of Youka 493U wetting agent, the components are weighed, stirred at 1200rpm for 10min and mixed uniformly to obtain a component A.
Preparing a component B: 55.29g of first phenolic aldehyde amine (Changzhou mountain PAA4816D curing agent with active hydrogen equivalent of 97), 119.99g of second phenolic aldehyde amine (Changzhou mountain LT4928F curing agent with active hydrogen equivalent of 97), 92.34g of polyamide (preferably Dida498 polyamide curing agent with active hydrogen equivalent of 110), D200027.65g and DMP-3012.17g are weighed, stirred at 800rpm for 10min and mixed uniformly to obtain the component B.
And mixing the prepared component A and the component B, and stirring at the rotating speed of 1400rpm for 3min to obtain the epoxy interface agent.
2. Performance testing
(1) Initial viscosity: the initial viscosity of the epoxy interfacial agent was determined using a rotational viscometer as specified in GB/T2794-1995, and the results were: 547.6 mPas.
(2) Room temperature 23 ℃ pot life: according to the test method specified in GB/T7123.1-2002, the result is as follows: and (5) 55 min.
(3) Surface dry time at room temperature 23 ℃: the surface drying time of the epoxy interface agent is tested according to GB/T16777-: 3 hours and 5 minutes.
(4) Tensile properties at room temperature for 28 days: preparing dumbbell I-shaped sample bars according to the specification of GB/T528-one 2009, and testing the tensile property after curing the sample bars for 28 days in an environment with the room temperature of 23 +/-2 ℃ and the humidity of 50 +/-10 percent, wherein the tensile strength is 31.396MPa, and the elongation at break is 15.093 percent;
(5) and bonding strength: the adhesive strength was tested according to the method specified in 7.9 of JC/T2217-2014, the dry base was 5.273MPa, the wet base was 3.818MPa, the water immersion treatment was 4.285MPa, and the heat treatment was 4.047MPa, and the coating did not peel, crack or peel during the whole process.
Example 2
1. Taking preparation of 1kg of interfacial agent as an example, the component A and the component B are respectively prepared according to the following formulas.
Preparing a component A: 100.25g of bisphenol A resin, 455.68g of bisphenol F resin, 127.86g of AGE, 56016.68 g of KH, 2.99g of BYK 066N defoamer and 1.99g of Youka 493U wetting agent are weighed, stirred at 900rpm for 10min and mixed uniformly to obtain the component A.
Preparing a component B: 41.23g of first phenolic aldehyde amine (Changzhou mountain SX5622 curing agent with active hydrogen equivalent of 97), 117.91g of second phenolic aldehyde amine (Changzhou mountain PAA4922F with active hydrogen equivalent of 97), 103.07g of polyamide (preferably Dida498 polyamide curing agent with active hydrogen equivalent of 110), T500017.67g and DMP-3014.72g, and the components are weighed, stirred for 10min at 1000rpm and mixed uniformly to obtain the component B.
And mixing the prepared component A and the component B, and stirring at the rotating speed of 1400rpm for 3min to obtain the epoxy interface agent.
2. Performance testing
(1) Initial viscosity: the initial viscosity of the epoxy interfacial agent was determined using a rotational viscometer as specified in GB/T2794-1995, and the results were: 345mPa · s.
(2) Room temperature 23 ℃ pot life: according to the test method specified in GB/T7123.1-2002, the result is as follows: for 60 minutes.
(3) Surface dry time at room temperature 23 ℃: the surface drying time of the epoxy interface agent is tested according to GB/T16777-: 3 hours and 49 minutes.
(4) Tensile properties at room temperature for 28 days: a dumbbell I-shaped sample bar is prepared according to the specification of GB/T528-2009, and the tensile property is tested after the sample bar is cured for 28 days in an environment with the room temperature of 23 +/-2 ℃ and the humidity of 50 +/-10 percent, wherein the tensile strength is 29.698MPa, and the breaking elongation is 13.858 percent.
(5) And bonding strength: the adhesive strength was tested according to the method specified in 7.9 of JC/T2217-2014, the dry base was 3.885MPa, the wet base was 3.486MPa, the water immersion treatment was 3.315MPa, and the heat treatment was 3.406MPa, and the coating did not peel, crack or peel during the whole process.
Example 3
1. Taking preparation of 1kg of interfacial agent as an example, the component A and the component B are respectively prepared according to the following formulas.
Preparing a component A: 69.59g of bisphenol A resin, 472.79g of bisphenol F resin, 65.32g of AGE, 20.52g of 1, 6-hexanediol diglycidyl ether, KH56016.31 g, 2.99g of BYK 066N defoamer and 1.99g of Youka 493U wetting agent, wherein the components are weighed, stirred at 1000rpm for 10min and uniformly mixed to obtain a component A.
Preparing a component B: 52.60g of first phenolic amine (Changzhou mountain SX5253 curing agent with active hydrogen equivalent of 97), 157.79g of second phenolic amine (Changzhou mountain PAA4812G curing agent with active hydrogen equivalent of 97), 91.00g of polyamide (preferably Dida498 polyamide curing agent with active hydrogen equivalent of 110), D200042.08g and DMP-307.01g are weighed, stirred for 10min at 1000rpm and mixed uniformly to obtain the component B.
And mixing the prepared component A and the component B, and stirring at the rotating speed of 1400rpm for 3min to obtain the epoxy interface agent.
2. Performance testing
(1) Initial viscosity: the initial viscosity of the epoxy interfacial agent was determined using a rotational viscometer as specified in GB/T2794-1995, and the results were: 384.8 mPas.
(2) Room temperature 23 ℃ pot life: according to the test method specified in GB/T7123.1-2002, the result is as follows: for 70 minutes.
(3) Surface dry time at room temperature 23 ℃: the surface drying time of the epoxy interface agent is tested according to GB/T16777-: 4 hours 28 minutes.
(4) Tensile properties at room temperature for 28 days: a dumbbell I-shaped sample bar is prepared according to the specification of GB/T528-2009, and the tensile property is tested after the sample bar is cured for 28 days in an environment with the room temperature of 23 +/-2 ℃ and the humidity of 50 +/-10 percent, wherein the tensile strength is 37.232MPa, and the breaking elongation is 13.891 percent.
(5) And bonding strength: the adhesive strength was tested according to the method specified in 7.9 of JC/T2217-2014, the dry base was 5.050MPa, the wet base was 4.846MPa, the water immersion treatment was 4.067MPa, and the heat treatment was 3.975MPa, and the coating did not peel, crack or peel during the whole process.
Example 4
The differences from example 1 are: no BYK 066N defoamer and no euca 493U wetting agent were added.
Performance testing
(1) Initial viscosity: the initial viscosity of the epoxy interfacial agent was determined using a rotational viscometer as specified in GB/T2794-1995, and the results were: 562.5 mPas.
(2) Room temperature 23 ℃ pot life: according to the test method specified in GB/T7123.1-2002, the result is as follows: and (5) 55 min.
(3) Surface dry time at room temperature 23 ℃: the surface drying time of the epoxy interface agent is tested according to GB/T16777-: 2 hours 55 minutes.
(4) Tensile properties at room temperature for 28 days: a dumbbell I-shaped sample bar is prepared according to the specification of GB/T528-2009, and the tensile property is tested after the sample bar is cured for 28 days in an environment with the room temperature of 23 +/-2 ℃ and the humidity of 50 +/-10 percent, wherein the tensile strength is 29.588MPa, and the breaking elongation is 10.482 percent.
(5) And bonding strength: the adhesive strength was tested according to the method specified in 7.9 of JC/T2217-2014, the dry base was 5.169MPa, the wet base was 3.422MPa, the water immersion treatment was 3.987MPa, the heat treatment was 3.752MPa, and the coating did not peel, crack or peel during the whole process.
Comparative example 1
The difference from example 1 is that the second hydroxyaldehyde amine is replaced with the first hydroxyaldehyde amine.
1. Taking the preparation of 1kg of epoxy interface agent as an example, the component A and the component B are respectively prepared according to the following formula.
Preparing a component A: 332.89g of bisphenol A resin, 249.81g of bisphenol F resin, 87.41g of AGE, 87.48g of KH56017, 2.98g of BYK 066N defoaming agent and 1.99g of Youka 493U wetting agent, the components are weighed, stirred at 1200rpm for 10min and mixed uniformly to obtain a component A.
Preparing a component B: 175.28g of first phenolic aldehyde amine (Changzhou mountain PAA4816D curing agent with active hydrogen equivalent of 97), 92.34g of polyamide (Jiadada 498 curing agent with active hydrogen equivalent of 110), D200027.65g and DMP-3012.17g are weighed, stirred for 10min at 800rpm and mixed uniformly to obtain the component B.
And mixing the prepared component A and the component B, and stirring at the rotating speed of 1400rpm for 3min to obtain the epoxy interface agent.
Performance testing
(1) Initial viscosity: the initial viscosity of the epoxy interfacial agent was determined using a rotational viscometer as specified in GB/T2794-1995, and the results were: 863.2 mPas.
(2) Room temperature 23 ℃ pot life: according to the test method specified in GB/T7123.1-2002, the result is as follows: and (5) 25 min.
(3) Surface dry time at room temperature 23 ℃: the surface drying time of the epoxy interface agent is tested according to GB/T16777-: 1 hour and 45 minutes.
(4) Tensile properties at room temperature for 28 days: a dumbbell I-shaped sample bar is prepared according to the specification of GB/T528-2009, and the tensile property is tested after the sample bar is cured for 28 days in an environment with the room temperature of 23 +/-2 ℃ and the humidity of 50 +/-10 percent, wherein the tensile strength is 44.527MPa, and the breaking elongation is 4.676 percent.
(5) And bonding strength: the adhesive strength was tested according to the method specified in 7.9 of JC/T2217-2014, the dry base was 5.854MPa, the wet base was 4.364MPa, the water immersion treatment was 4.453MPa, and the heat treatment was 3.961MPa, and the coating did not peel, crack or peel during the whole process.
Comparative example 2
The difference from example 1 is that the first phenolic aldehyde amine is replaced by a second phenolic aldehyde amine.
1. Taking the preparation of 1kg of epoxy interface agent as an example, the component A and the component B are respectively prepared according to the following formula.
Preparing a component A: 332.89g of bisphenol A resin, 249.81g of bisphenol F resin, 87.41g of AGE, 87.48g of KH56017, 2.98g of BYK 066N defoaming agent and 1.99g of Youka 493U wetting agent, the components are weighed, stirred at 1200rpm for 10min and mixed uniformly to obtain a component A.
Preparing a component B: 175.28g of second hydroxyamine (Changzhou mountain LT4928F curing agent with active hydrogen equivalent of 97), 92.34g of polyamide (Jiadada 49 polyamide 8 curing agent with active hydrogen equivalent of 110), D200027.65g and DMP-3012.17g, wherein the components are weighed, stirred at 800rpm for 10min and mixed uniformly to obtain the component B.
And mixing the prepared component A and the component B, and stirring at the rotating speed of 1400rpm for 3min to obtain the epoxy interface agent.
Performance testing
(1) Initial viscosity: the initial viscosity of the epoxy interfacial agent was determined using a rotational viscometer as specified in GB/T2794-1995, and the results were: 326.5 mPas.
(2) Room temperature 23 ℃ pot life: according to the test method specified in GB/T7123.1-2002, the result is as follows: 1 hour 50 minutes.
(3) Surface dry time at room temperature 23 ℃: the surface drying time of the epoxy interface agent is tested according to GB/T16777-: 8 hours and 50 minutes.
(4) Tensile properties at room temperature for 28 days: a dumbbell I-shaped sample bar is prepared according to the specification of GB/T528-2009, and the tensile property is tested after the sample bar is cured for 28 days in an environment with the room temperature of 23 +/-2 ℃ and the humidity of 50 +/-10 percent, wherein the tensile strength is 24.755MPa, and the breaking elongation is 17.362 percent.
(5) And bonding strength: the adhesive strength was tested according to the method specified in 7.9 of JC/T2217-2014, the dry base was 4.515MPa, the wet base was 2.836MPa, the water immersion treatment was 2.907MPa, and the heat treatment was 3.067MPa, and the coating did not peel, crack or peel during the whole process.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (10)

1. The curing agent for the epoxy interface agent suitable for being used in a humid environment is characterized by comprising the following components in parts by weight:
44-68 parts of phenolic amine, 28-35 parts of polyamide, 2-16 parts of polyether amine and 2-5 parts of epoxy accelerator.
2. The curing agent for an epoxy interface agent according to claim 1, wherein the phenolic aldehyde amine comprises a first phenolic aldehyde amine and a second phenolic aldehyde amine, and the active hydrogen equivalent of the first phenolic aldehyde amine and the second phenolic aldehyde amine is 97; the curing speed of the first phenolic aldehyde amine is higher than that of the second phenolic aldehyde amine; the mass ratio of the first phenolic aldehyde amine to the second phenolic aldehyde amine is 20: 80-35: 65.
3. the curing agent for an epoxy interface agent according to claim 1, wherein the polyamide has an active hydrogen equivalent of 110.
4. The curing agent for an epoxy interface agent according to claim 1, wherein the polyetheramine comprises a first polyetheramine or a second polyetheramine; the first polyetheramine has a difunctional average molecular weight of 2000; the second polyetheramine has a trifunctional average molecular weight of 5000.
5. The curing agent for an epoxy interface agent according to claim 1, wherein the epoxy accelerator comprises a tertiary amine; the tertiary amine comprises triethanolamine, methyldiethanolamine and aminophenols; the aminophenols include 2,4, 6-tris (dimethylaminomethyl) phenol.
6. An epoxy interface agent suitable for being used in a humid environment comprises a component A and a component B which are separately packaged, wherein the component A comprises the following components in parts by weight:
73-88 parts of epoxy resin, 10-23 parts of glycidyl ether and 2-4 parts of silane coupling agent;
the epoxy resin is an epoxy resin mixture comprising bisphenol A resin and bisphenol F resin;
the glycidyl ethers include C12-14 alkyl glycidyl ethers;
the component B is the curing agent for the epoxy interface agent suitable for being used in a humid environment, which is disclosed by any one of claims 1 to 5;
the mass ratio of the component A to the component B is 100: 35-100: 55.
7. the epoxy interfacial agent according to claim 6, wherein the mass ratio of bisphenol A resin and bisphenol F resin in said epoxy resin mixture is 10: 90-65: 35.
8. the epoxy interfacial agent of claim 6, wherein said glycidyl ethers further comprise 1, 6-hexanediol diglycidyl ether; when the glycidyl ether is a mixed glycidyl ether of C12-14 alkyl glycidyl ether and 1, 6-hexanediol diglycidyl ether, the mass fraction of the C12-14 alkyl glycidyl ether in the mixed glycidyl ether is 30-70%.
9. The epoxy interface agent of claim 6, wherein the silane coupling agent comprises one or more of gamma- (2, 3-glycidoxy) propyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, vinyltriethoxysilane, and vinyltrimethoxysilane.
10. Use of an epoxy interfacial agent suitable for use in a humid environment according to any one of claims 6 to 9 in concrete, metal and wood.
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