CN115433532B - Low-hardness high-toughness double-component epoxy resin pouring sealant and preparation method thereof - Google Patents

Low-hardness high-toughness double-component epoxy resin pouring sealant and preparation method thereof Download PDF

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CN115433532B
CN115433532B CN202211106118.3A CN202211106118A CN115433532B CN 115433532 B CN115433532 B CN 115433532B CN 202211106118 A CN202211106118 A CN 202211106118A CN 115433532 B CN115433532 B CN 115433532B
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epoxy resin
pouring sealant
toughness
low
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CN115433532A (en
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刘海
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Shenzhen Anbos Science And Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/4007—Curing agents not provided for by the groups C08G59/42 - C08G59/66
    • 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
    • C08G59/42—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
    • C08G59/4292—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof together with monocarboxylic acids
    • 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
    • C08G59/68—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 catalysts used
    • C08G59/686—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 catalysts used containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08—Macromolecular additives
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04—Polyurethanes
    • C09J175/08—Polyurethanes from polyethers
    • 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
    • C08G2170/00—Compositions for adhesives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08G2190/00—Compositions for sealing or packing joints
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—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
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets
    • C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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  • Inorganic Chemistry (AREA)
  • Epoxy Resins (AREA)
  • Sealing Material Composition (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The application relates to the technical field of pouring sealants, in particular to a low-hardness high-toughness double-component epoxy resin pouring sealant and a preparation method thereof; the application discloses a low-hardness high-toughness double-component epoxy resin pouring sealant, which comprises a composition A and a composition B; the composition A comprises the following raw materials: polyurethane modified epoxy resin, bisphenol A epoxy resin, a first plasticizer, a reactive diluent, a silane coupling agent, a wetting and leveling agent, a flame retardant, a thixotropic agent and a colorant; the composition B comprises the following raw materials: phthalic anhydride curing agent, carboxylic acid curing agent, modified anhydride curing agent, second plasticizer and accelerator. The pouring sealant prepared by the application has the characteristics of low hardness, high toughness and good buffering and shockproof effects after hardening.

Description

Low-hardness high-toughness double-component epoxy resin pouring sealant and preparation method thereof
Technical Field
The application relates to the technical field of pouring sealants, in particular to a low-hardness high-toughness double-component epoxy resin pouring sealant and a preparation method thereof.
Background
The pouring sealant is used for bonding, sealing, pouring and coating protection of electronic components. The pouring sealant is liquid before solidification, has fluidity, and the viscosity of the glue solution is different according to the material, performance and production process of the product. The pouring sealant can realize the use value after being completely cured, and can play roles of water proofing, moisture proofing, dust proofing, insulation, heat conduction, confidentiality, corrosion resistance, temperature resistance and vibration resistance after being cured. The electronic pouring sealant is very various, and is mainly 3 types of most common materials, namely epoxy resin pouring sealant, organic silicon resin pouring sealant and polyurethane pouring sealant.
Epoxy resins are widely used as packaging materials for electronic devices and integrated circuits because of their low shrinkage, excellent heat resistance, electrical insulating properties, sealability, and low dielectric properties. With the rapid development of high-performance and high-density packaging technology of packaging devices in the electronic field, more and higher requirements are put on packaging materials.
For example, packaging of vehicle capacitors requires low hardness, high toughness of the potting adhesive, cushioning and vibration resistance, high voltage resistance and flame retardant properties. The existing epoxy resin pouring sealant system on the market has a large number of rigid groups due to the molecular structure, and the index of high hardness and low toughness or low hardness and low toughness is difficult to reach simultaneously after curing, so that the pouring requirements of the electronic devices are not met.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the application aims to provide the low-hardness high-toughness double-component epoxy resin pouring sealant and the preparation method thereof, and the pouring sealant has the characteristics of low hardness, high toughness and good buffering and shockproof effects after being hardened.
The aim of the application is achieved by the following technical scheme:
a low-hardness high-toughness two-component epoxy resin pouring sealant comprises a composition A and a composition B;
the A composition comprises the following raw materials in percentage by weight:
further, the polyurethane modified epoxy resin is polyether polyurethane modified bisphenol A epoxy resin;
further, the reactive diluent is 4-butanediol diglycidyl ether;
further, the silane coupling agent is gamma-glycidyl ether oxypropyl trimethoxy silane;
further, the wetting leveling agent is BYK-333;
further, the thixotropic agent is fumed silica;
further, the colorant is oil-soluble nigrosine;
further, the flame retardant is one or two of aluminum hydroxide and decabromodiphenyl ethane; in the application, the aluminum hydroxide is surface modified nano aluminum hydroxide powder, which has the advantages of narrow particle size distribution, high purity, low impurity content and good stability, and the aluminum hydroxide powder used in the application is easy to disperse in a matrix, has low thickening amplitude, good filling property and excellent processing performance due to the low surface polarity of the powder.
The aluminum hydroxide has the functions of increasing flame retardance, increasing heat conductivity and reducing expansion coefficient, if the added aluminum hydroxide is less (less than 10%), the effects of flame retardance, heat conductivity and expansion coefficient reduction are not achieved, and if the added aluminum hydroxide is higher (more than 60%), the powder is easy to cause poor dispersibility, the viscosity of the system is high, the fluidity is poor, the filling and sealing are not facilitated, and meanwhile, the toughness is low and the elongation at break is insufficient.
Further, the first plasticizer is epoxy fatty acid methyl ester or epoxy soybean oil; wherein, the epoxy fatty acid methyl ester or the epoxy soybean oil is characterized in that the functional group is an epoxy structure, is consistent with the characteristic functional group of the epoxy resin of the composition A, and belongs to the same type of components; the epoxy fatty acid methyl ester (epoxy soybean oil) and the polyurethane modified epoxy resin have good compatibility, do not react with each other to form a unified whole, can well play roles in dilution, viscosity reduction and plasticization, can react into a system, and have no risk of precipitation;
the composition B comprises the following raw materials in percentage by weight:
further, the phthalic anhydride curing agent is methyl tetrahydrophthalic anhydride;
further, the carboxylic acid curing agent is an isomeric fatty acid;
further, the modified anhydride curing agent is one or more of tung oil anhydride, dodecenyl succinic anhydride, maleic anhydride and nadic anhydride;
further, the second plasticizer is castor oil.
Further, the accelerator is one or more of 2-ethyl-4-methylimidazole, 2-phenylimidazole and 2-phenyl-4-ethylimidazole.
In the application, the second plasticizer is castor oil, and the functional group is hydroxyl structure, and can be subjected to crosslinking reaction with the epoxy resin, so that the second plasticizer has the functions of plasticizing and crosslinking reinforcement.
Specifically, in the present application, the actions of the respective raw materials are as follows:
action of the ingredients in the A composition
Raw materials Action
Polyurethane modified epoxy resin The adhesive effect has better flexibility
Bisphenol a epoxy 128 The adhesive effect has better rigidity
First plasticizer Dilution, reduced viscosity, and increased flexibility
Reactive diluents Dilution effect, viscosity reduction
Silane coupling agent Improving the adhesive force and increasing the binding force of inorganic particles and resin
Wetting leveling agent Increase wettability, leveling property and particle dispersibility of pouring sealant
Flame retardant Flame retarding and filling effects
Thixotropic agent Anti-settling and rheology control
Coloring agent Coloring of
Action of the ingredients in the B composition
Assembly of A and B compositions
The main raw materials of the composition A are resin components and flame retardant components, and the composition A has good adhesion, low viscosity, good fluidity, low hardness and high toughness compared with the common epoxy resin after solidification. The filler aluminum hydroxide and decabromodiphenyl ethane have good flame retardance (V0 grade). The other auxiliary agents have the functions of toughening and reducing viscosity, and increasing adhesive force and dispersibility. If the A composition reacts with a conventional acid anhydride curing agent, a material with high or low hardness and toughness can be formed, or a material with poor heat resistance can be formed by reacting with a conventional polyether curing agent.
The composition B belongs to a hardening agent, and the composition A is crosslinked and solidified to form a material with certain strength, toughness and hardness. Phthalic anhydride curing agents provide substantial strength, heterogeneous fatty acids, tung oil anhydride, castor oil provide toughness and reduced hardness, and 2-ethyl-4-methylimidazole enhances the chemical reaction rate.
The A composition and the B composition react to form a three-dimensional crosslinked network structure, and the hardness, the toughness and the heat resistance of the crosslinked network structure are jointly influenced by the materials of the A composition and the B composition, so that the A composition and the B composition have certain plasticizing and toughening effects.
Further, in the pouring sealant, the mass ratio of the a composition to the B composition is =4: 1.
a preparation method of a low-hardness high-toughness double-component epoxy resin pouring sealant comprises the following steps:
preparation of the composition of step 1) A
Preparing materials according to the mass percentage of the composition A;
stirring polyurethane modified epoxy resin and bisphenol A epoxy resin at 50-60 ℃ and 800-1000r/min, and mixing uniformly; cooling to room temperature, adding an active diluent, a first plasticizer, a silane coupling agent and a wetting leveling agent, uniformly mixing and stirring, adding a flame retardant, a thixotropic agent and a colorant, and fully mixing to obtain a composition A;
preparation of the composition of step 2) B
Preparing materials according to the mass percentage of the composition B;
adding phthalic anhydride curing agent, carboxylic acid curing agent and modified anhydride curing agent, stirring and mixing uniformly at room temperature of 800-1000 r/min; adding a plasticizer and an accelerator, and fully mixing to obtain a composition B;
step 3) preparation of pouring sealant
And (3) fully mixing the composition A and the composition B to obtain the pouring sealant.
The application has the beneficial effects that:
1. the pouring sealant prepared by the application has low hardness (Shore A: 30) after hardening, high toughness (elongation at break of 70%), good buffering and shockproof effects, obvious self-extinguishing property, flame retardant grade V0 and no precipitate under high temperature conditions; the curing conditions are consistent with those of the conventional pouring sealant, and specifically, the heat curing is 100 ℃ for 1h+140 ℃ for 10h or the curing mode and the curing conditions are selected according to the actual conditions in the field.
2. In the preparation process, no o-benzene plasticizer is used, and the vegetable oil plasticizer is more environment-friendly; the composition A is introduced with environment-friendly plasticizer epoxy fatty acid methyl ester, so that the hardness can be reduced and the toughness can be improved while the environment is protected; the heterogeneous fatty acid, tung oil anhydride and castor oil are introduced into the composition B to be used as a curing agent with plasticizing and toughening functions; therefore, the polyether polyurethane modified epoxy resin has lower hardness, higher toughness and better strength after being cured.
3. The pouring sealant prepared by the application is applied to encapsulation of vehicle-mounted electronic components, has small coil extrusion force, good flexibility, good flame retardance and good temperature resistance, and has good shockproof and buffering effects.
Drawings
The application will be further described with reference to the drawings and examples.
FIG. 1 is a diagram showing the ratio of raw materials and the detection result of pouring sealant according to the embodiment 1 of the present application;
FIG. 2 is a graph showing the raw material ratios and the detection results of the pouring sealant obtained in comparative example 1 of the present application;
FIG. 3 is a graph showing the raw material ratio and the detection result of the pouring sealant obtained in comparative example 2;
FIG. 4 is a graph showing the raw material ratio and the detection result of the pouring sealant obtained in comparative example 3 of the present application;
FIG. 5 is a graph showing the raw material ratio and the detection result of the pouring sealant obtained in comparative example 4;
FIG. 6 is a graph showing the ratio of the raw materials and the detection result of the pouring sealant obtained in comparative example 5;
FIG. 7 is a graph showing the ratio of the raw materials and the detection result of the pouring sealant obtained in comparative example 6 of the present application;
FIG. 8 is a graph showing the ratio of raw materials and the detection result of pouring sealant according to comparative example 7;
FIG. 9 is a graph showing the ratio of the raw materials and the detection result of the pouring sealant according to comparative example 8;
FIG. 10 is a graph showing the results of the measurement of the ratio of the raw materials and the pouring sealant obtained in comparative example 9 of the present application.
Detailed Description
The application will be further illustrated by the following examples, which are not intended to limit the scope of the application, in order to facilitate the understanding of those skilled in the art.
In the following examples and comparative examples, the starting materials were all commercially available; wherein, the specific sources of part of raw materials are as follows:
unmodified non-nano aluminum hydroxide was from Chengdu Maackia chemical Co., ltd., reagent cargo number: m015547;
modified nano aluminum hydroxide is from Shandong morning Xue New Material Co., ltd., model: CX-GL-B1.
Example 1
A low-hardness high-toughness two-component epoxy resin pouring sealant comprises a composition A and a composition B;
the A composition comprises the following raw materials in percentage by weight:
the composition B comprises the following raw materials in percentage by weight:
the preparation method of the low-hardness high-toughness double-component epoxy resin pouring sealant comprises the following steps:
preparation of the composition of step 1) A
Preparing materials according to the mass percentage of the composition A;
stirring and mixing polyurethane modified epoxy resin and bisphenol A epoxy resin 128 at 50 ℃ and 800r/min for 5min; cooling to room temperature, adding an active diluent, a first plasticizer, a silane coupling agent and a wetting leveling agent, and stirring and mixing at a rotating speed for 5min; increasing the rotating speed to 1300r/min, stirring and mixing for 30min to obtain a composition A;
preparation of the composition of step 2) B
Preparing materials according to the mass percentage of the composition B;
adding phthalic anhydride curing agent, carboxylic acid curing agent and modified anhydride curing agent, stirring and mixing for 10min at room temperature of 800 r/min; adding plasticizer and promoter, stirring at rotating speed for 20min to obtain composition B;
step 3) preparation of pouring sealant
And (3) fully mixing the composition A and the composition B to obtain the pouring sealant.
Example 2
A low-hardness high-toughness two-component epoxy resin pouring sealant comprises a composition A and a composition B;
the A composition comprises the following raw materials in percentage by weight:
the composition B comprises the following raw materials in percentage by weight:
the preparation method of the low-hardness high-toughness double-component epoxy resin pouring sealant comprises the following steps:
preparation of the composition of step 1) A
Preparing materials according to the mass percentage of the composition A;
stirring and mixing polyurethane modified epoxy resin and bisphenol A epoxy resin 128 at 50 ℃ and 1000r/min for 5min; cooling to room temperature, adding an active diluent, a first plasticizer, a silane coupling agent and a wetting leveling agent, and stirring and mixing at a rotating speed for 5min; increasing the rotating speed to 1500r/min, stirring and mixing for 30min to obtain a composition A;
preparation of the composition of step 2) B
Preparing materials according to the mass percentage of the composition B;
adding phthalic anhydride curing agent, carboxylic acid curing agent and modified anhydride curing agent, stirring and mixing for 10min at room temperature of 800 r/min; adding plasticizer and promoter, stirring at rotating speed for 20min to obtain composition B;
step 3) preparation of pouring sealant
And (3) fully mixing the composition A and the composition B to obtain the pouring sealant.
Example 3
A low-hardness high-toughness two-component epoxy resin pouring sealant comprises a composition A and a composition B;
the A composition comprises the following raw materials in percentage by weight:
the composition B comprises the following raw materials in percentage by weight:
the preparation method of the low-hardness high-toughness double-component epoxy resin pouring sealant comprises the following steps:
preparation of the composition of step 1) A
Preparing materials according to the mass percentage of the composition A;
stirring and mixing polyurethane modified epoxy resin and bisphenol A epoxy resin 128 at 50 ℃ and 900r/min for 5min; cooling to room temperature, adding an active diluent, a first plasticizer, a silane coupling agent and a wetting leveling agent, and stirring and mixing at a rotating speed for 5min; increasing the rotating speed to 1400r/min, stirring and mixing for 30min to obtain a composition A;
preparation of the composition of step 2) B
Preparing materials according to the mass percentage of the composition B;
adding phthalic anhydride curing agent, carboxylic acid curing agent and modified anhydride curing agent, stirring and mixing for 10min at room temperature of 900 r/min; adding plasticizer and promoter, stirring at rotating speed for 20min to obtain composition B;
step 3) preparation of pouring sealant
And (3) fully mixing the composition A and the composition B to obtain the pouring sealant.
Examination of characterization data such as hardness, toughness, PC-PC shear strength, viscosity and the like of the pouring sealants prepared in the above examples 1 to 3 and comparative examples 1 to 9 below is carried out, and specific results are shown in fig. 1 to 10; wherein the comparative examples 1 to 9 are specifically set as follows:
comparative example 1: the influence of the missing polyether polyurethane modified bisphenol A epoxy resin on viscosity, hardness and toughness is examined; specific raw material composition and detection results are shown in fig. 2; the preparation method is the same as in example 1;
comparative example 2: the influence of polyester polyurethane modified bisphenol A epoxy resin on viscosity, hardness and toughness is examined; specific raw material composition and detection results are shown in fig. 3; the preparation method is the same as in example 1;
comparative example 3: the influence of the missing epoxy fatty acid methyl ester on the viscosity, the hardness and the toughness is examined; specific raw material composition and detection results are shown in fig. 4; the preparation method is the same as in example 1;
comparative example 4: the influence of unmodified non-nanoscale aluminum hydroxide on viscosity, hardness and toughness is examined; specific raw material composition and detection results are shown in fig. 5; the preparation method is the same as in example 1;
comparative example 5: the influence of the missing heterogeneous fatty acid on the viscosity, hardness and toughness of the system is examined; specific raw material composition and detection results are shown in fig. 6; the preparation method is the same as in example 1;
comparative example 6: the influence of non-heterogeneous fatty acid on viscosity, hardness and toughness is examined; specific raw material composition and detection results are shown in fig. 7; the preparation method is the same as in example 1;
comparative example 7: the influence of non-heterogeneous fatty acid on viscosity, hardness and toughness is examined; specific raw material composition and detection results are shown in fig. 8; the preparation method is the same as in example 1;
comparative example 8: the influence of missing tung oil anhydride on the viscosity, hardness and toughness of the system is examined; specific raw material composition and detection results are shown in fig. 9; the preparation method is the same as in example 1;
comparative example 9: the influence of other anhydrides on the viscosity, hardness and toughness of the system is examined, and the specific raw material composition and the detection result are shown in FIG. 10; the preparation method is the same as in example 1;
with reference to fig. 1-10, the influence of different epoxy resin, carboxylic acid curing agent, anhydride curing agent and plasticizer on the hardness, toughness, PC-PC shear strength, viscosity and other characterization data of the pouring sealant product is respectively compared. It can be known that: the results of comparative example 1 and comparative example 2 demonstrate that polyether urethane modified bisphenol a epoxy resins have lower hardness and higher toughness than conventional bisphenol a epoxy resins and polyester urethane epoxy resins.
Comparative example 3 demonstrates that the active toughening agent epoxy fatty acid methyl ester/epoxy soybean oil can effectively reduce viscosity, reduce hardness and improve toughness.
Comparative example 4 demonstrates that the modified nanoscale aluminum hydroxide can reduce the viscosity of the system and has a certain effect on the reduction of hardness and the improvement of toughness.
Comparative examples 5, 6 and 7 show that the isomeric fatty acids have a significant reduction in hardness and a significant increase in toughness. This effect is not achieved by deleting this component or changing to other linear fatty acids.
Comparative example 8 demonstrates that tung oil anhydride can reduce hardness and improve toughness.
Comparative example 9 illustrates that dodecenyl succinic anhydride/maleic anhydride/nadic anhydride and tung oil anhydride have similar effects in terms of hardness/toughness improvement; the effect of tung oil anhydride is most obvious.
The above embodiments are preferred embodiments of the present application, and besides, the present application may be implemented in other ways, and any obvious substitution is within the scope of the present application without departing from the concept of the present application.

Claims (5)

1.A low-hardness high-toughness two-component epoxy resin pouring sealant comprises a composition A and a composition B; it is characterized in that the method comprises the steps of,
the A composition comprises the following raw materials in percentage by weight:
the flame retardant comprises aluminum hydroxide;
the first plasticizer is epoxy fatty acid methyl ester or epoxy soybean oil;
the polyurethane modified epoxy resin is polyether polyurethane modified bisphenol A epoxy resin;
the composition B comprises the following raw materials in percentage by weight:
the modified anhydride curing agent is tung oil anhydride;
the second plasticizer is castor oil;
the carboxylic acid curing agent is an isomeric fatty acid.
2. The low-hardness high-toughness two-component epoxy resin pouring sealant according to claim 1, wherein the reactive diluent is 4-butanediol diglycidyl ether.
3. The low-hardness high-toughness two-component epoxy resin pouring sealant according to claim 1, wherein the silane coupling agent is gamma-glycidoxypropyl trimethoxysilane.
4. The low-hardness high-toughness two-component epoxy resin pouring sealant according to claim 1, wherein the phthalic anhydride curing agent is methyl tetrahydrophthalic anhydride.
5. A method for preparing the low-hardness high-toughness two-component epoxy resin pouring sealant according to any one of claims 1 to 4, which is characterized by comprising the following steps:
preparation of the composition of step 1) A
Preparing materials according to the mass percentage of the composition A;
stirring polyurethane modified epoxy resin and bisphenol A epoxy resin at 50-60 ℃ and 800-1000r/min, and mixing uniformly; cooling to room temperature, adding an active diluent, a first plasticizer, a silane coupling agent and a wetting leveling agent, uniformly mixing and stirring, adding a flame retardant, a thixotropic agent and a colorant, and fully mixing to obtain a composition A;
preparation of the composition of step 2) B
Preparing materials according to the mass percentage of the composition B;
adding phthalic anhydride curing agent, carboxylic acid curing agent and modified anhydride curing agent, stirring and mixing uniformly at room temperature of 800-1000 r/min; adding a plasticizer and an accelerator, and fully mixing to obtain a composition B;
step 3) preparation of pouring sealant
And (3) fully mixing the composition A and the composition B to obtain the pouring sealant.
CN202211106118.3A 2022-09-09 2022-09-09 Low-hardness high-toughness double-component epoxy resin pouring sealant and preparation method thereof Active CN115433532B (en)

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CN104388029A (en) * 2014-12-03 2015-03-04 湖南皓志科技股份有限公司 Normal-temperature-curing epoxy resin flexible pouring sealant
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CN107163888A (en) * 2017-07-07 2017-09-15 东莞市德聚胶接技术有限公司 Epoxy resin embedding adhesive and preparation method thereof
CN107236503A (en) * 2017-06-13 2017-10-10 湖北新海鸿化工有限公司 A kind of LED casting glues and preparation method thereof
CN107418498A (en) * 2017-09-11 2017-12-01 杭州之江有机硅化工有限公司 A kind of elastic epoxy fire-proof potting compound and preparation method thereof
CN112812719A (en) * 2020-12-30 2021-05-18 江苏天康电子合成材料有限公司 High-sealing high-temperature-resistant high-toughness high-flame-retardance electronic pouring sealant

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104388029A (en) * 2014-12-03 2015-03-04 湖南皓志科技股份有限公司 Normal-temperature-curing epoxy resin flexible pouring sealant
CN106281174A (en) * 2016-09-22 2017-01-04 株洲时代新材料科技股份有限公司 A kind of high tenacity, impact resistance, high flexibility epoxy pouring sealant and preparation method thereof
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