CN113773777A - Novel bi-component phase-change energy-storage flame-retardant pouring sealant - Google Patents

Novel bi-component phase-change energy-storage flame-retardant pouring sealant Download PDF

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CN113773777A
CN113773777A CN202011434911.7A CN202011434911A CN113773777A CN 113773777 A CN113773777 A CN 113773777A CN 202011434911 A CN202011434911 A CN 202011434911A CN 113773777 A CN113773777 A CN 113773777A
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component
flame retardant
phase
parts
curing agent
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胡磊
刘宏伟
陈蕾
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Hangzhou Innock New Materials Co ltd
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Hangzhou Innock New Materials Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J163/00Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • C08K2003/322Ammonium phosphate
    • C08K2003/323Ammonium polyphosphate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/38Boron-containing compounds
    • C08K2003/387Borates
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • C08L2203/206Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Sealing Material Composition (AREA)

Abstract

The invention belongs to the technical field of flame-retardant pouring sealants, and particularly relates to a novel two-component phase-change energy-storage flame-retardant pouring sealant which comprises a component A and a component B, wherein the component A comprises the following raw materials: the epoxy resin phase-change microcapsule comprises epoxy resin, an epoxy diluent, a phase-change microcapsule and an auxiliary agent, wherein the component B comprises the following raw materials: the AB component is simply mixed according to a proper proportion to be used when the curing agent, the flame retardant, the phase-change microcapsule and the auxiliary agent are used, and the pouring sealant can be stably stored for a long time and is convenient to use. The bi-component phase change energy storage flame retardant pouring sealant provided by the invention utilizes the advantages of long service life and high electrical property of epoxy resin, and the addition of the flame retardant enables the product to have excellent flame retardant property, so that the product does not have any combustion risk even in extreme conditions such as lightning strike or fire, the reliability, flame retardant property and service life of the product are increased, and the increasingly high-performance requirements of modern electronic products can be met.

Description

Novel bi-component phase-change energy-storage flame-retardant pouring sealant
Technical Field
The invention relates to a novel bi-component phase-change energy-storage flame-retardant pouring sealant. Belongs to the technical field of bi-component phase change energy storage flame-retardant pouring sealant.
Background
The existing phase-change pouring sealant generally adopts silicone oil as a base material, uses the silicone oil as all or part of liquid components, and then is added with phase-change fillers and other functional fillers to form the phase-change pouring sealant. For example, chinese patent publication No. CN108130040A discloses a "modified two-component potting adhesive", which is formed by adding a heat conductive filler and microcapsules having a phase transition temperature to modified two-component silicone oil. The method for reusing the silicone oil pouring sealant after curing has some defects, and as some electronic products have higher electrical property requirements when in use, such as high breakdown voltage or high volume resistivity, and the electrical property of the cured silicone oil cannot meet the requirements, the silicone oil is used as a base material, so that the electrical property is low, but the electrical property of the pouring sealant is a great obstacle for restricting the improvement of the performance of modern electronic products. Due to the increasing performance requirements of modern electronic products, for example, chargers for various electronic products develop to high power, and the high power of the charger requires that the potting adhesive has high breakdown voltage and high volume resistance to ensure that the charger does not generate electrical breakdown to cause short circuit or electric leakage to cause danger when in use. Therefore, the electrical property is an important performance index for the pouring sealant.
In addition, after the silicone oil-based pouring sealant is used for a long time (for example, more than 5 years), the aging resistance is poor, and the performance is easily reduced greatly, for example, various dust can be adhered to the silicone oil due to precipitation of the silicone oil, so that the electrical performance is greatly reduced, and the use safety and the performance of the product are finally influenced.
Disclosure of Invention
The invention provides a phase change energy storage pouring sealant adopting epoxy resin as a base material, which is a novel two-component phase change energy storage flame retardant pouring sealant formed by taking the epoxy resin as the base material and utilizing the advantages of high electrical property and long service life of the epoxy resin and adding microcapsules with phase change temperature and other functional fillers. In order to solve the technical problems, the technical scheme of the invention is as follows:
the utility model provides a novel fire-retardant casting glue of two-component phase change energy storage, novel fire-retardant casting glue of two-component phase change energy storage includes A component and B component, A component comprises following raw materials: the epoxy resin phase-change microcapsule comprises epoxy resin, an epoxy diluent, a phase-change microcapsule and an auxiliary agent, wherein the component B comprises the following raw materials: curing agent, flame retardant, phase-change microcapsule and auxiliary agent.
The surface of the phase-change microcapsule needs to be treated by a coupling agent, and the treatment process comprises the following steps: dissolving a coupling agent which is soluble in water or soluble in water after pH adjustment in water, stirring for 10-30 minutes, adding the coupling agent into a phase-change microcapsule emulsion with the solid content of 30-50%, stirring for 1-2 hours, and after stirring, carrying out spray drying on the microcapsule to obtain the phase-change microcapsule.
In another embodiment, the surface of the phase-change microcapsule is treated by a coupling agent, and the treatment process comprises the following steps: emulsifying coupling agent, emulsifier and water which are insoluble in water or insoluble in water after PH adjustment for 10-30 minutes, adding the emulsified coupling agent, emulsifier and water into phase-change microcapsule emulsion with solid content of 30-50%, stirring for 1-2 hours, and spray drying the microcapsule after stirring is finished to obtain the microcapsule.
The novel double-component phase-change energy-storage flame-retardant pouring sealant comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 14-45 parts of epoxy resin, 1-8 parts of epoxy diluent, 14-45 parts of phase change microcapsule and 0.01-10 parts of auxiliary agent, wherein the component B comprises the following raw materials in parts by weight: 5-30 parts of curing agent, 8-35 parts of flame retardant, 2-22 parts of phase-change microcapsule and 1-16 parts of auxiliary agent.
The auxiliary agent comprises the following raw materials in parts by weight: 0-1 part of curing accelerator, 0-2 parts of dispersant, 0-3 parts of flatting agent, 0-5 parts of defoaming agent and 0-7 parts of heat-conducting filler.
The epoxy resin is one or a combination of bisphenol A epoxy resin, bisphenol F epoxy resin, bisphenol S epoxy resin and linear phenolic epoxy resin; the epoxy diluent is multifunctional and monofunctional glycidyl ether, and the epoxy diluent is one or a combination of C12-C16 alcohol glycidyl ether and butyl glycidyl ether.
The curing agent is a curing agent which can react with epoxy resin and generate crosslinking, and is one or a combination of more of an aliphatic amine curing agent, a boron amine curing agent, an aliphatic amide curing agent, a polyamide curing agent, a phenolic aldehyde curing agent, an aromatic tertiary amine curing agent, an imidazole curing agent, a polyether amine curing agent, a mixed amine curing agent and an anhydride curing agent. More preferably, it is a modified adduct of an amine-based curing agent and an aromatic amine which have undergone a mannich reaction.
The coupling agent is a silane coupling agent, a phthalate coupling agent and an aluminate coupling agent: the silane coupling agent can be alkyl n-methoxysilane (n is an integer of 1-3), alkyl n-ethoxysilane (n is an integer of 1-3), and epoxy n-methoxysilane (n is an integer of 1-3), preferably octyl trimethoxysilane, hexadecyl trimethoxysilane, and 2- (3, 4-epoxycyclohexyl) ethyl trimethoxysilane. The phthalate coupling agent can be monoalkoxyl titanate, phosphoric acid monoalkoxyl titanate and pyrophosphoric acid monoalkoxyl titanate, and is preferably phosphoric acid monoalkoxyl titanate; the aluminate coupling agent can be triisopropoxyaluminum, triacetylaluminum, ethyl acetoacetate diisopropyl aluminum, isopropoxy distearoyloxy aluminate, preferably isopropoxy distearoyloxy aluminate.
The flame retardant can be a combination of one or more of metal hydroxide, solid flame retardant and liquid flame retardant containing P element or N element, preferably a combination of one or more of aluminum hydroxide, magnesium hydroxide, 3.5-hydrated zinc borate, montmorillonite, ammonium polyphosphate, melamine polyphosphate, microcapsule-coated red phosphorus, melamine cyanurate, dimethyl methyl phosphate, tricresyl phosphate, BDP, RDP, pentaerythritol, CFA, aluminum alkyl phosphinate, DOPO and derivatives thereof, cyclophosphazene and organosilicon flame retardant, more preferably a combination of multiple flame retardants capable of showing a "synergistic effect" in the two-component phase change energy storage flame retardant potting adhesive, and can be exemplified by 3: 1:1, aluminum hydroxide, 3.5 zinc borate hydrate, melamine polyphosphate, pentaerythritol 5: 1: 4:1, 1 of montmorillonite, melamine, aluminum alkyl phosphinate, tricresyl phosphate: 3: 6: 10, in a solvent.
The heat conducting filler is one or a combination of more of metal oxide, metal hydroxide, carbon fiber, carbon nanotube and graphene, and the D50 particle size of the particles is 0-100um, preferably 0-60 um. The curing accelerator is one or more of bisphenol A, ethylene glycol, DMP-30 and salts thereof, imidazole and salts thereof, boron trifluoride and salts thereof, and thiourea, preferably bisphenol A, DMP-30.
The invention has the following advantages and beneficial effects:
the novel two-component phase change energy storage flame-retardant pouring sealant utilizes the advantages of long service life and high electrical property of epoxy resin to replace the pouring sealant made of silicone oil, effectively overcomes the defects of insufficient electrical property and short service life of the traditional silicone oil system, and ensures that the product has excellent flame retardant property so that the product does not have any combustion risk even in extreme conditions such as lightning stroke or fire, further improves the reliability of the product, has higher electrical property, flame retardant property and service life, and meets the increasing high-performance requirements of modern electronic products.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a data table of an embodiment of a novel two-component phase-change energy-storage flame-retardant pouring sealant of the present invention;
FIG. 2 is a table showing curing agents of the two-component phase-change energy-storage flame-retardant pouring sealant according to various embodiments of the present invention;
FIG. 3 is a comparison graph of breakdown voltage under various embodiments of the novel two-component phase-change energy-storage flame-retardant pouring sealant and breakdown voltage after aging.
Detailed Description
The following further describes the embodiments of the present invention. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The utility model provides a novel fire-retardant casting glue of two-component phase change energy storage, novel fire-retardant casting glue of two-component phase change energy storage includes A component and B component, A component comprises following raw materials: the epoxy resin phase-change microcapsule comprises epoxy resin, an epoxy diluent, a phase-change microcapsule and an auxiliary agent, wherein the component B comprises the following raw materials: curing agent, flame retardant, phase-change microcapsule and auxiliary agent. The bi-component phase change energy storage flame-retardant pouring sealant comprises a component A and a component B, wherein the components are mixed into the component A and the component B according to a proper proportion to obtain the phase change energy storage flame-retardant pouring sealant, the component AB is simply mixed according to a proper proportion to be used when the sealant is used, and the pouring sealant can be stably stored for a long time and is convenient to use.
The surface of the phase-change microcapsule needs to be treated by a coupling agent, and the treatment process comprises the following steps: dissolving a coupling agent which is soluble in water or soluble in water after pH adjustment in water, stirring for 10-30 minutes, adding the coupling agent into a phase-change microcapsule emulsion with the solid content of 30-50%, stirring for 1-2 hours, and after stirring, carrying out spray drying on the microcapsule to obtain the phase-change microcapsule.
In another embodiment, the surface of the phase-change microcapsule is treated by a coupling agent, and the treatment process comprises the following steps: emulsifying coupling agent, emulsifier and water which are insoluble in water or insoluble in water after PH adjustment for 10-30 minutes, adding the emulsified coupling agent, emulsifier and water into phase-change microcapsule emulsion with solid content of 30-50%, stirring for 1-2 hours, and spray drying the microcapsule after stirring is finished to obtain the microcapsule.
The novel double-component phase-change energy-storage flame-retardant pouring sealant comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 14-45 parts of epoxy resin, 1-8 parts of epoxy diluent, 14-45 parts of phase change microcapsule and 0.01-10 parts of auxiliary agent, wherein the component B comprises the following raw materials in parts by weight: 5-30 parts of curing agent, 8-35 parts of flame retardant, 2-22 parts of phase-change microcapsule and 1-16 parts of auxiliary agent.
The auxiliary agent comprises the following raw materials in parts by weight: 0-1 part of curing accelerator, 0-2 parts of dispersant, 0-3 parts of flatting agent, 0-5 parts of defoaming agent and 0-7 parts of heat-conducting filler.
The epoxy resin is one or a combination of bisphenol A epoxy resin, bisphenol F epoxy resin, bisphenol S epoxy resin and phenol novolac epoxy resin, preferably bisphenol A epoxy resin and bisphenol F epoxy resin or a mixture thereof; the epoxy diluent is multifunctional and monofunctional glycidyl ether, and the epoxy diluent is one or a combination of C12-C16 alcohol glycidyl ether and butyl glycidyl ether.
The curing agent is a curing agent which can react with epoxy resin and generate crosslinking, and is one or a combination of more of an aliphatic amine curing agent, a boron amine curing agent, an aliphatic amide curing agent, a polyamide curing agent, a phenolic aldehyde curing agent, an aromatic tertiary amine curing agent, an imidazole curing agent, a polyether amine curing agent, a mixed amine curing agent and an anhydride curing agent. More preferably, it is a modified adduct of an amine-based curing agent and an aromatic amine which have undergone a mannich reaction.
The coupling agent is a silane coupling agent, a phthalate coupling agent and an aluminate coupling agent: the silane coupling agent can be alkyl n-methoxysilane (n is an integer of 1-3), alkyl n-ethoxysilane (n is an integer of 1-3), and epoxy n-methoxysilane (n is an integer of 1-3), preferably octyl trimethoxysilane, hexadecyl trimethoxysilane, and 2- (3, 4-epoxycyclohexyl) ethyl trimethoxysilane. The phthalate coupling agent can be monoalkoxyl titanate, phosphoric acid monoalkoxyl titanate and pyrophosphoric acid monoalkoxyl titanate, and is preferably phosphoric acid monoalkoxyl titanate; the aluminate coupling agent can be triisopropoxyaluminum, triacetylaluminum, ethyl acetoacetate diisopropyl aluminum, isopropoxy distearoyloxy aluminate, preferably isopropoxy distearoyloxy aluminate.
The coupling agent used for the surface treatment of the microcapsule after the surface treatment is a silane coupling agent, a phthalate coupling agent and an aluminate coupling agent: the silane coupling agent can be alkyl n-methoxysilane (n is an integer of 1-3), alkyl n-ethoxysilane (n is an integer of 1-3), and epoxy n-methoxysilane (n is an integer of 1-3), preferably octyl trimethoxysilane, hexadecyl trimethoxysilane, and 2- (3, 4-epoxycyclohexyl) ethyl trimethoxysilane. The phthalate coupling agent can be monoalkoxyl titanate, phosphoric acid monoalkoxyl titanate and pyrophosphoric acid monoalkoxyl titanate, and is preferably phosphoric acid monoalkoxyl titanate; the aluminate coupling agent can be triisopropoxyaluminum, triacetylaluminum, ethyl acetoacetate diisopropyl aluminum, isopropoxy distearoyloxy aluminate, preferably isopropoxy distearoyloxy aluminate.
The flame retardant can be a combination of one or more of metal hydroxide, solid flame retardant and liquid flame retardant containing P element or N element, preferably a combination of one or more of aluminum hydroxide, magnesium hydroxide, 3.5-hydrated zinc borate, montmorillonite, ammonium polyphosphate, melamine polyphosphate, microcapsule-coated red phosphorus, melamine cyanurate, dimethyl methyl phosphate, tricresyl phosphate, BDP, RDP, pentaerythritol, CFA, aluminum alkyl phosphinate, DOPO and derivatives thereof, cyclophosphazene and organosilicon flame retardant, more preferably a combination of multiple flame retardants capable of showing a "synergistic effect" in the two-component phase change energy storage flame retardant potting adhesive, and can be exemplified by 3: 1:1, aluminum hydroxide, 3.5 zinc borate hydrate, melamine polyphosphate, pentaerythritol 5: 1: 4:1, 1 of montmorillonite, melamine, aluminum alkyl phosphinate, tricresyl phosphate: 3: 6: 10, in a solvent.
The heat conducting filler is one or a combination of more of metal oxide, metal hydroxide, carbon fiber, carbon nanotube and graphene, and the D50 particle size of the particles is 0-100um, preferably 0-60 um. The curing accelerator is bisphenol A, ethylene glycol, DMP-30 and salts thereof, imidazole and salts thereof, boron trifluoride and salts thereof, thiourea, preferably one or more combinations of bisphenol A, DMP-30, preferably bisphenol A, DMP-30.
Example 1:
the substances in the components A and B are weighed according to the formula shown in the figure 1 and the figure 2 and respectively added into a conventional stirring container, dispersed for 20 minutes at the rotating speed of 2000 rpm by using an ultra-high speed disperser, and the products are respectively stored in a closed container according to the components. When in use, the materials are weighed according to the mass ratio of A to B being 1 to 1, stirred evenly, poured on the material to be sealed and solidified.
Example 2:
the substances in the components A and B are weighed according to the scheme shown in figure 1 and figure 2 in example 2, and are respectively added into a conventional stirring container, dispersed for 10 minutes at the rotating speed of 2700 revolutions per minute by using an ultra-high speed disperser, and the products are respectively stored in a closed container according to the components. When in use, the materials are weighed according to the mass ratio of A to B being 2 to 1, stirred evenly, poured on the material to be sealed and solidified.
Example 3:
according to the method shown in fig. 1 and fig. 2 and the example 3, the substances in the components A and B are weighed according to the amount and are respectively added into a conventional stirring container, the substances are dispersed for 20 minutes at the rotating speed of 2200 rpm by using an ultra-high speed disperser, and the products are respectively stored in a closed container according to the components. When in use, the materials are weighed according to the mass ratio of A to B being 5 to 2, stirred evenly, poured on the material to be sealed and solidified.
Example 4:
according to the embodiment 4 shown in fig. 1 and fig. 2, the materials of the components a and B are weighed according to the amount and are respectively added into a conventional stirring container, and are dispersed for 25 minutes at 1400 rpm by using an ultra-high speed disperser, and the products are respectively stored in a closed container according to the components. When in use, the materials are weighed according to the mass ratio of A to B being 2 to 1, stirred evenly, poured on the material to be sealed and solidified.
Example 5:
according to the embodiment 5 shown in fig. 1 and fig. 2, the substances in the components a and B are weighed according to the amount and are respectively added into a conventional stirring container, the mixture is dispersed for 40 minutes at the rotating speed of 800 r/min by using an ultra-high speed dispersion machine, and the products are respectively stored in a closed container according to the components. When in use, the materials are weighed according to the mass ratio of A to B being 1 to 1, stirred evenly, poured on the material to be sealed and solidified.
Example 6:
according to the embodiment 6 shown in fig. 1 and fig. 2, the materials of the components a and B are weighed according to the amount and are respectively added into a conventional stirring container, and are dispersed for 30 minutes at the rotating speed of 500 rpm by using an ultra-high speed dispersion machine, and the products are respectively stored in a closed container according to the components. When in use, the materials are weighed according to the mass ratio of A to B being 4 to 1, stirred evenly, poured on the material to be sealed and solidified.
Example 7:
according to the embodiment 7 shown in fig. 1 and fig. 2, the materials of the components a and B are weighed according to the amount and added into a conventional stirring container respectively, and dispersed for 8 minutes at 3000 r/min by using a super high speed disperser, and the products are stored in a closed container respectively according to the components. When in use, the materials are weighed according to the mass ratio of A to B being 2 to 1, stirred evenly, poured on the material to be sealed and solidified.
Example 8:
according to the embodiment 8 shown in fig. 1 and fig. 2, the substances in the components a and B are weighed according to the amount and are respectively added into a conventional stirring container, and are dispersed for 20 minutes at the rotating speed of 1600 rpm by using an ultra-high speed dispersion machine, and the products are respectively stored in a closed container according to the components. When in use, the materials are weighed according to the mass ratio of A to B being 1 to 2, stirred evenly, poured on the material to be sealed and solidified.
Example 9:
according to the embodiment 9 shown in fig. 1 and fig. 2, the materials of the components a and B are weighed according to the amount and are respectively added into a conventional stirring container, and are dispersed for 60 minutes at the rotating speed of 50 r/min by using an ultra-high speed dispersion machine, and the products are respectively stored in a closed container according to the components. When in use, the materials are weighed according to the mass ratio of A to B being 2 to 1, stirred evenly, poured on the material to be sealed and solidified.
Example 10:
according to the embodiment 10 shown in fig. 1 and fig. 2, the substances in the components a and B are weighed according to the amount and are respectively added into a conventional stirring container, the mixture is dispersed for 30 minutes at the rotating speed of 1300 rpm by using an ultra-high speed disperser, and the products are respectively stored in a closed container according to the components. When in use, the materials are weighed according to the mass ratio of A to B being 1 to 1, stirred evenly, poured on the material to be sealed and solidified.
The examples 1 to 10 were subjected to performance tests:
the breakdown voltage and the breakdown voltage after aging were performed on the products of examples 1 to 7, respectively, to obtain a comparative graph of fig. 3.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.

Claims (10)

1. The utility model provides a novel fire-retardant casting glue of two-component phase transition energy storage which characterized in that: the novel double-component phase-change energy-storage flame-retardant pouring sealant comprises a component A and a component B, wherein the component A comprises the following raw materials: the epoxy resin phase-change microcapsule comprises epoxy resin, an epoxy diluent, a phase-change microcapsule and an auxiliary agent, wherein the component B comprises the following raw materials: curing agent, flame retardant, phase-change microcapsule and auxiliary agent.
2. The novel two-component phase change energy storage flame retardant pouring sealant as claimed in claim 1, wherein: the surface of the phase-change microcapsule needs to be treated by a coupling agent, and the treatment process comprises the following steps: dissolving a coupling agent which is soluble in water or soluble in water after pH adjustment in water, stirring for 10-30 minutes, adding the coupling agent into a phase-change microcapsule emulsion with the solid content of 30-50%, stirring for 1-2 hours, and after stirring, carrying out spray drying on the microcapsule to obtain the phase-change microcapsule.
3. The novel two-component phase change energy storage flame retardant pouring sealant as claimed in claim 1, wherein: the surface of the phase-change microcapsule needs to be treated by a coupling agent, and the treatment process comprises the following steps: emulsifying coupling agent, emulsifier and water which are insoluble in water or insoluble in water after PH adjustment for 10-30 minutes, adding the emulsified coupling agent, emulsifier and water into phase-change microcapsule emulsion with solid content of 30-50%, stirring for 1-2 hours, and spray drying the microcapsule after stirring is finished to obtain the microcapsule.
4. The novel two-component phase change energy storage flame retardant pouring sealant according to claim 1, 2 or 3, characterized in that: the novel double-component phase-change energy-storage flame-retardant pouring sealant comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 14-45 parts of epoxy resin, 1-8 parts of epoxy diluent, 14-45 parts of phase change microcapsule and 0.01-10 parts of auxiliary agent, wherein the component B comprises the following raw materials in parts by weight: 5-30 parts of curing agent, 8-35 parts of flame retardant, 2-22 parts of phase-change microcapsule and 1-16 parts of auxiliary agent.
5. The novel two-component phase change energy storage flame retardant pouring sealant according to claim 4, characterized in that: the auxiliary agent comprises the following raw materials in parts by weight: 0-1 part of curing accelerator, 0-2 parts of dispersant, 0-3 parts of flatting agent, 0-5 parts of defoaming agent and 0-7 parts of heat-conducting filler.
6. The novel two-component phase change energy storage flame retardant pouring sealant according to claim 4, characterized in that: the epoxy resin is one or a combination of bisphenol A epoxy resin, bisphenol F epoxy resin, bisphenol S epoxy resin and linear phenolic epoxy resin; the epoxy diluent is multifunctional and monofunctional glycidyl ether, and the epoxy diluent is one or a combination of C12-C16 alcohol glycidyl ether and butyl glycidyl ether.
7. The novel two-component phase change energy storage flame retardant pouring sealant according to claim 4, characterized in that: the curing agent is a curing agent which can react with epoxy resin and generate crosslinking, and is one or a combination of more of an aliphatic amine curing agent, a boron amine curing agent, an aliphatic amide curing agent, a polyamide curing agent, a phenolic aldehyde curing agent, an aromatic tertiary amine curing agent, an imidazole curing agent, a polyether amine curing agent, a mixed amine curing agent and an anhydride curing agent. More preferably, it is a modified adduct of an amine-based curing agent and an aromatic amine which have undergone a mannich reaction.
8. The novel two-component phase change energy storage flame retardant pouring sealant according to claim 4, characterized in that: the coupling agent is a silane coupling agent, a phthalate coupling agent and an aluminate coupling agent: the silane coupling agent can be alkyl n-methoxysilane (n is an integer of 1-3), alkyl n-ethoxysilane (n is an integer of 1-3), and epoxy n-methoxysilane (n is an integer of 1-3), preferably octyl trimethoxysilane, hexadecyl trimethoxysilane, and 2- (3, 4-epoxycyclohexyl) ethyl trimethoxysilane. The phthalate coupling agent can be monoalkoxyl titanate, phosphoric acid monoalkoxyl titanate and pyrophosphoric acid monoalkoxyl titanate, and is preferably phosphoric acid monoalkoxyl titanate; the aluminate coupling agent can be triisopropoxyaluminum, triacetylaluminum, ethyl acetoacetate diisopropyl aluminum, isopropoxy distearoyloxy aluminate, preferably isopropoxy distearoyloxy aluminate.
9. The novel two-component phase change energy storage flame retardant pouring sealant according to claim 4, characterized in that: the flame retardant can be a combination of one or more of metal hydroxide, solid flame retardant and liquid flame retardant containing P element or N element, preferably a combination of one or more of aluminum hydroxide, magnesium hydroxide, 3.5-hydrated zinc borate, montmorillonite, ammonium polyphosphate, melamine polyphosphate, microcapsule-coated red phosphorus, melamine cyanurate, dimethyl methyl phosphate, tricresyl phosphate, BDP, RDP, pentaerythritol, CFA, aluminum alkyl phosphinate, DOPO and derivatives thereof, cyclophosphazene and organosilicon flame retardant, more preferably a combination of multiple flame retardants capable of showing a "synergistic effect" in the two-component phase change energy storage flame retardant potting adhesive, and can be exemplified by 3: 1:1, aluminum hydroxide, 3.5 zinc borate hydrate, melamine polyphosphate, pentaerythritol 5: 1: 4:1, 1 of montmorillonite, melamine, aluminum alkyl phosphinate, tricresyl phosphate: 3: 6: 10, in a solvent.
10. The novel two-component phase change energy storage flame retardant pouring sealant according to claim 4, characterized in that: the heat conducting filler is one or a combination of more of metal oxide, metal hydroxide, carbon fiber, carbon nanotube and graphene, and the D50 particle size of the particles is 0-100um, preferably 0-60 um. The curing accelerator is one or more of bisphenol A, ethylene glycol, DMP-30 and salts thereof, imidazole and salts thereof, boron trifluoride and salts thereof, and thiourea, preferably bisphenol A, DMP-30.
CN202011434911.7A 2020-12-10 2020-12-10 Novel bi-component phase-change energy-storage flame-retardant pouring sealant Pending CN113773777A (en)

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CN116144314A (en) * 2022-12-05 2023-05-23 湖北兴瑞硅材料有限公司 Sealant for single-component rapid deep curing photovoltaic module and preparation method thereof

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CN110724499A (en) * 2019-10-24 2020-01-24 天津城建大学 Silane coupling agent modified silicon dioxide phase change microcapsule and preparation method thereof
CN111269689A (en) * 2020-02-05 2020-06-12 深圳垒石热管理技术有限公司 Flame-retardant, insulating and reliable pouring sealant based on phase-change microcapsules and preparation method thereof

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CN101671480A (en) * 2009-10-15 2010-03-17 张家港高奇化工生物有限公司 Anion silicon milk silane sol-gel modified emulsion, preparation method and application thereof
CN103316617A (en) * 2013-06-20 2013-09-25 广东药学院 Preparation method of surface-modified self-healing type microcapsule
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CN116144314B (en) * 2022-12-05 2024-03-12 湖北兴瑞硅材料有限公司 Sealant for single-component rapid deep curing photovoltaic module and preparation method thereof

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