CN110724489A - Single-component normal-temperature curing encapsulating material - Google Patents

Single-component normal-temperature curing encapsulating material Download PDF

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CN110724489A
CN110724489A CN201911159033.XA CN201911159033A CN110724489A CN 110724489 A CN110724489 A CN 110724489A CN 201911159033 A CN201911159033 A CN 201911159033A CN 110724489 A CN110724489 A CN 110724489A
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parts
weight
temperature
curing
phase
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张立强
张秋兵
杨小玉
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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
    • 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
    • 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
    • C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • 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
    • C09J175/06—Polyurethanes from polyesters
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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Abstract

The single-component normal-temperature curing encapsulating material comprises a mixture of the following substances: a carrier medium and a phase change material; wherein from 20 to 60 parts of said carrier medium are present per 100 parts by weight of said mixture; wherein 40 to 80 parts of said phase change material are present per 100 parts by weight of said mixture; the carrier medium comprises: moisture-curable resins and moisture curing agents; the phase change material includes: microencapsulated phase-change powder or mixed powder of the phase-change powder and an adsorption carrier, wherein the adsorption carrier is graphite or aerogel. The single-component normal-temperature curing encapsulating material adopting the formula has excellent heat absorption and temperature control performance, can effectively control electronic equipment in the electronic encapsulating glue within a proper temperature, and cannot overheat.

Description

Single-component normal-temperature curing encapsulating material
Technical Field
The invention relates to the technical field of encapsulating materials and preparation methods thereof, in particular to a single-component normal-temperature curing encapsulating material.
Background
The electronic pouring sealant is liquid before being cured, has fluidity, and the viscosity of the glue solution is different according to the material, the performance and the production process of the product. The pouring sealant can realize the use value after being completely cured, and can play the roles of water resistance, moisture resistance, dust prevention, insulation, heat conduction, confidentiality, corrosion resistance, temperature resistance and shock resistance after being cured.
However, the performance requirements of electronic devices are higher and higher, so the heat generation problem of electronic devices is more and more serious, and the heat dissipation performance of the conventional electronic potting adhesive is far from the requirements.
Disclosure of Invention
The invention aims to provide a single-component normal-temperature curing encapsulating material to solve the heat dissipation problem of an electronic encapsulating adhesive in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
the single-component normal-temperature curing encapsulating material provided by the first aspect of the embodiment of the invention comprises a mixture of the following substances: a carrier medium and a phase change material;
wherein from 20 to 60 parts of said carrier medium are present per 100 parts by weight of said mixture;
wherein 40 to 80 parts of said phase change material are present per 100 parts by weight of said mixture;
the carrier medium comprises: moisture-curable resins and moisture curing agents;
the phase change material includes: microencapsulated phase-change powder or mixed powder of the phase-change powder and an adsorption carrier, wherein the adsorption carrier is graphite or aerogel. .
In one embodiment of the method of the present invention,
50 to 83.3 parts of said moisture curable resin per 100 parts by weight of said carrier medium;
16.7 to 50 parts of said moisture curing agent per 100 parts by weight of said carrier medium.
In one embodiment, the combination of the moisture-curable resin and the moisture curing agent includes any one of:
isocyanate prepolymer resin and polyol; wherein the polyol comprises: polyether polyols, or polyester polyols;
polyol prepolymer resin and isocyanate; wherein the isocyanate comprises: at least one of polyisocyanate PAPI, MDI and TDI.
In one embodiment, if the combination of the moisture curable resin and moisture curing agent is an isocyanate prepolymer resin and a polyol, 66.7 to 83.3 parts of the isocyanate prepolymer resin are present per 100 parts by weight of the carrier medium; 16.7 to 33.3 parts of said polyol per 100 parts by weight of said carrier medium;
if the combination of the moisture curing resin and the moisture curing agent is polyol prepolymer resin and isocyanate, 50 to 83.3 parts of the polyol prepolymer resin is present per 100 parts by weight of the carrier medium; from 16.7 to 50 parts of said isocyanate per 100 parts by weight of said carrier medium.
In one embodiment, the one-component ambient temperature curing potting material further comprises: a thermally conductive filler;
the thermally conductive filler includes a combination of at least one of the following materials: aluminum oxide, aluminum nitride, boron nitride, magnesium oxide, zinc oxide, silicon carbide, graphite powder and carbon nanotubes;
the heat conductive filler is present in an amount of 1 to 70 parts per 100 parts by weight of the one-component room temperature-curing potting material.
In one embodiment, if the adsorbent support is graphite, the graphite is vermicular expanded graphite; 99 to 99.5 parts of the phase change powder exists in each 100 parts by weight of the phase change material; 0.5 to 1 parts by weight of the vermicular expanded graphite per 100 parts by weight of the phase change material;
the expansion rate of the vermicular expanded graphite is 100-600ml/g, the granularity is 100-200 meshes, the expansion multiple is 200-600 times, and the bulk density is 0.2-0.5 g/cm3。
In one embodiment, if the adsorption carrier is aerogel, 50 to 90 parts of the phase-change powder are present per 100 parts by weight of the phase-change material; 10 to 50 parts of said aerogel per 100 parts by weight of said phase change material;
the aerogel has the specific surface area of 100 square meters per gram and the particle size of 5-60 nm.
In one embodiment, the phase-change powder is selected from at least one of the following materials: alkane waxes having an alkane carbon number between 10 and 60, paraffin waxes, fatty acids, PE waxes and PP waxes.
In one embodiment, a method for preparing a one-component ambient temperature curing potting material includes:
heating the phase change powder to be molten, adding an adsorption carrier into the molten phase change powder in batches, and stirring, wherein after the adsorption carrier is added, vacuumizing a preparation environment, wherein the vacuum degree is-0.04 to-0.10 MPa, the vacuumizing time lasts for 5-40min, and the stirring time is 15-90 min; after stirring in a vacuum state, respectively cooling, crushing and sieving the mixed material of the phase-change powder and the adsorption carrier to obtain the phase-change substance;
placing the moisture curing resin and the phase change material in a vacuum kneader and stirring for 0.5-2 hours to obtain a mixed base material; the temperature in the vacuum kneading machine is 80-150 ℃, and the vacuum degree is-0.04-0.10 Mpa;
placing the mixed base material and the moisture curing agent in a stirrer to be uniformly stirred to obtain the single-component normal-temperature curing encapsulating material; the stirring conditions include: the rotating speed is 30 r/min, the vacuum degree is between-0.04 and-0.10 MPa, and the stirring time is 0.5 to 1.5 hours.
The second aspect of the embodiments of the present invention provides a single-component normal temperature curing potting material, which comprises a mixture of: a carrier medium and a phase change material;
wherein from 20 to 60 parts of said carrier medium are present per 100 parts by weight of said mixture;
wherein 40 to 80 parts of said phase change material are present per 100 parts by weight of said mixture;
the carrier medium comprises: temperature-sensitive curing resin and temperature-sensitive curing agent;
the phase change material includes: the phase-change powder comprises phase-change powder and an adsorption carrier, wherein the adsorption carrier is graphite or aerogel.
In one embodiment, 62.5 to 90 parts of the temperature sensitive curable resin is present per 100 parts by weight of the carrier medium;
10 to 37.5 parts of said temperature sensitive curing agent per 100 parts by weight of said carrier medium.
In one embodiment, the combination of the temperature-sensitive curing resin and the temperature-sensitive curing agent includes any one of:
epoxy resin and imidazole curing agent; wherein the epoxy resin comprises: bisphenol a type epoxy resin, modified epoxy resin, bisphenol S type epoxy resin, bisphenol F type epoxy resin, epoxidized epoxy resin;
epoxy resin and amine hydrazine curing agents; wherein the epoxy resin comprises: bisphenol a type epoxy resin, modified epoxy resin, bisphenol S type epoxy resin, bisphenol F type epoxy resin, epoxidized epoxy resin.
In one embodiment, the one-component ambient temperature curing potting material further comprises: a thermally conductive filler;
the thermally conductive filler includes a combination of at least one of the following materials: aluminum oxide, aluminum nitride, boron nitride, magnesium oxide, zinc oxide, silicon carbide, graphite powder and carbon nanotubes;
the heat conductive filler is present in an amount of 1 to 70 parts per 100 parts by weight of the one-component room temperature-curing potting material.
In one embodiment, if the adsorbent support is graphite, the graphite is vermicular expanded graphite; 99 to 99.5 parts of the phase change powder exists in each 100 parts by weight of the phase change material; 0.5 to 1 parts by weight of the vermicular expanded graphite per 100 parts by weight of the phase change material;
the expansion rate of the vermicular expanded graphite is 100-600ml/g, the granularity is 100-200 meshes, the expansion multiple is 200-600 times, and the bulk density is 0.2-0.5 g/cm3。
In one embodiment, if the adsorption carrier is aerogel, 50 to 90 parts of the phase-change powder are present per 100 parts by weight of the phase-change material; 10 to 50 parts of said aerogel per 100 parts by weight of said phase change material;
the aerogel has the specific surface area of 100 square meters per gram and the particle size of 5-60 nm.
In one embodiment, the phase-change powder is selected from at least one of the following materials: alkane waxes having an alkane carbon number between 10 and 60, paraffin waxes, fatty acids, PE waxes and PP waxes.
In one embodiment, the method comprises the following steps:
heating the phase change powder to be molten, adding an adsorption carrier into the molten phase change powder in batches, and stirring, wherein after the adsorption carrier is added, vacuumizing a preparation environment, wherein the vacuum degree is-0.04 to-0.10 MPa, the vacuumizing time lasts for 5-40min, and the stirring time is 15-90 min; after stirring in a vacuum state, respectively cooling, crushing and sieving the mixed material of the phase-change powder and the adsorption carrier to obtain the phase-change substance;
placing the temperature-sensitive curing resin and the phase change material in a vacuum kneader and stirring for 0.5-2 hours to obtain a mixed base material; the temperature in the vacuum kneading machine is 80-150 ℃, and the vacuum degree is-0.04-0.10 Mpa;
placing the mixed base material and the temperature-sensitive curing agent in a stirrer to be uniformly stirred to obtain the single-component normal-temperature curing encapsulating material; the stirring conditions include: the rotating speed is 30 r/min, the vacuum degree is between-0.04 and-0.10 MPa, and the stirring time is 0.5 to 1.5 hours.
Compared with the prior art, the single-component normal-temperature curing encapsulating material has the following beneficial effects: the performance is as follows, the specific heat capacity (J/(g.K)) > 1.5; the phase change enthalpy (J/g) is about 30-180, namely the heat absorption value; the phase transition temperature (DEG C) is 5-90; specific gravity (g/cc): 0.8-1.8 surface drying time: 5 min-25 min; curing time: 1 h-2 h; the complete curing time is more than or equal to 24 hours. The single-component normal-temperature curing encapsulating material adopting the formula has excellent heat absorption and temperature control performance, can effectively control electronic equipment in the electronic encapsulating glue within a proper temperature, and cannot overheat.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained from the drawings without inventive effort.
Fig. 1 is a schematic flow chart of a preparation method of a single-component normal-temperature-curing encapsulating material in an embodiment of the invention.
Detailed Description
The present invention will be further described with reference to the following examples, which are preferred embodiments of the present invention.
Classification about one-component normal-temperature curing encapsulating material
The electronic pouring sealant is used for wrapping electronic equipment in various scenes and shapes, and therefore the electronic pouring sealant is liquid before being solidified. In practical application, in order to facilitate sealing of electronic equipment and reduce the requirements on sealing environment, the pouring sealant material can be prepared to be cured at normal temperature.
In the embodiment of the invention, the single-component normal-temperature curing encapsulating material can be divided into a moisture curing encapsulating material and a temperature-sensitive curing encapsulating material.
Moisture-curing potting material
Moisture curing the potting material, i.e., when exposed to air, a curing reaction occurs upon exposure to water vapor in the air.
The moisture-curable potting material comprises a mixture of: a carrier medium and a phase change material.
Wherein, the carrier medium is a substance for binding and carrying the phase-change substance.
The phase-change material is a material which absorbs the phase-change powder, and the phase-change powder is a powder material which absorbs or releases heat through changing a physical form.
Wherein from 20 to 60 parts of said carrier medium are present per 100 parts by weight of said mixture;
wherein 40 to 80 parts of said phase change material are present per 100 parts by weight of said mixture;
the carrier medium comprises: moisture-curable resins and moisture curing agents; the moisture curing agent is a chemical additive that cures the moisture curing resin. Specifically, the combination of the moisture-curable resin and the moisture curing agent, and the range of the mixture ratio of the relevant materials in practical use will be described in detail in the following examples 1 to 10.
The phase change material includes: the phase-change powder comprises phase-change powder and an adsorption carrier, wherein the adsorption carrier is graphite or aerogel.
Illustratively, the phase-change powder is selected from at least one of the following materials: alkane waxes having an alkane carbon number between 10 and 60, paraffin waxes, fatty acids, PE waxes and PP waxes.
Illustratively, according to the requirements of the practical application on the hardness, toughness, plasticity, heat absorption capacity, specific heat capacity, volume and material cost of the potting material, 50 to 83.3 parts of the moisture curing resin is present per 100 parts by weight of the carrier medium, and 16.7 to 50 parts of the moisture curing agent is present per 100 parts by weight of the carrier medium, and the requirement is not limited herein.
Temperature-sensitive curing encapsulating material
The encapsulating material is cured in a temperature-sensitive manner, that is, when the encapsulating material is sensed to have a temperature in a normal temperature environment (20 to 40 ℃), a curing reaction occurs. Therefore, the temperature-sensitive curing potting material in the embodiment of the present invention needs to be stored and transported under refrigeration.
A temperature-sensitive curable potting material comprising a mixture of: a carrier medium and a phase change material;
wherein from 20 to 60 parts of said carrier medium are present per 100 parts by weight of said mixture;
wherein 40 to 80 parts of said phase change material are present per 100 parts by weight of said mixture;
the carrier medium comprises: temperature-sensitive curing resin and temperature-sensitive curing agent; the temperature-sensitive curing agent is a chemical additive for curing the temperature-sensitive curing resin. Specifically, the combination of the temperature-sensitive curing resin and the temperature-sensitive curing agent, and the range of the mixture ratio of the relevant materials, which are different in practical applications, will be described in detail in the following examples 11 to 15.
The phase change material includes: microencapsulated phase-change powder or mixed powder of the phase-change powder and an adsorption carrier, wherein the adsorption carrier is graphite or aerogel.
Illustratively, the phase-change powder is selected from at least one of the following materials: alkane waxes having an alkane carbon number between 10 and 60, paraffin waxes, fatty acids, PE waxes and PP waxes.
Illustratively, the temperature-sensitive curable resin is present in an amount of 62.5 to 90 parts per 100 parts by weight of the carrier medium, depending on the requirements of the potting material for hardness, toughness, moldability, heat absorption, specific heat capacity, volume, and material cost in practical use; the temperature-sensitive curing agent is present in an amount of 10 to 37.5 parts by weight per 100 parts by weight of the carrier medium, and is not particularly limited herein.
About heat conductive filler
In the embodiment of the invention, the single-component normal-temperature curing encapsulating material has the main function of absorbing heat of electronic equipment, so that the encapsulating material needs to have good heat-conducting property. According to the embodiment of the invention, the heat-conducting filler is added into the single-component normal-temperature curing encapsulating material, so that the encapsulating material has good heat-conducting property.
The thermally conductive filler may include a combination of at least one of the following materials: aluminum oxide, aluminum nitride, boron nitride, magnesium oxide, zinc oxide, silicon carbide, graphite powder, and carbon nanotubes.
Illustratively, the heat conductive filler is present in an amount of 1 to 70 parts per 100 parts by weight of the one-component ambient temperature curing potting material, depending on the requirements of the potting material for hardness, toughness, moldability, heat absorption, specific heat capacity, volume and material cost in practical applications, and is not limited herein.
It should be noted that, in either the embodiment of the moisture-curing potting material or the embodiment of the temperature-sensitive curing potting material, the heat conductive filler may be added to enhance the heat conductive performance of the potting material.
About catalyst
In practical application, the single-component normal-temperature curing encapsulating material needs to meet or strengthen the curing effect of the encapsulating material through a catalytic material. However, in some embodiments, some curing agents have a catalytic effect (i.e. the curing agents serve as both a curing material and a catalytic material), therefore, the catalyst is not a necessary additive in the embodiments of the present invention, and the following only illustrates an example of the catalyst, and whether the catalyst is added, what type of the catalyst is added, and how much the catalyst is added are determined according to actual needs, and the details are not limited herein.
Illustratively, the catalyst may be any one of dibutyl tin dilaurate, stannous octoate, and 1, 3-phenylenedioxybis (ethyl acetoacetate) titanium.
About an adsorption carrier
In actual use to the phase change powder, the phase change powder is likely to leak out in the potting material after changing from solid state to liquid, so, need adsorb the parcel through the adsorption carrier with the phase change powder, prevent overflowing of phase change powder.
In the embodiment of the application, vermicular expanded graphite can be selected as an adsorbing material, the vermicular expanded graphite is a loose and porous vermicular substance obtained by intercalating, washing, drying and high-temperature expanding natural crystalline flake graphite, the expanded graphite has the excellent performances of cold and heat resistance, corrosion resistance, self-lubrication, radiation resistance, conductivity and the like of the natural graphite, and also has the characteristics of softness, compression resilience, adsorptivity, ecological environment harmony, biocompatibility, radiation resistance and the like which are not possessed by the natural graphite, and the vermicular expanded graphite is loose and porous and has a large specific surface area, so that the adsorbing capacity on phase-change powder is very strong, the phase-change substance can be adsorbed by only using a small amount of vermicular expanded graphite in parts by weight, and certainly, the vermicular expanded graphite cannot be too little and cannot completely adsorb the phase-change substance; the worm-shaped expanded graphite cannot be too much, so that the cost is increased and the enthalpy value of the product is reduced on the one hand, meanwhile, the phase change enthalpy of the graphite adsorption phase change energy storage powder is reduced, and the heat storage performance of the product is reduced, therefore, the weight ratio of the graphite adsorption phase change energy storage powder to different powder is optimal.
Illustratively, if the adsorbent support is graphite, the graphite is vermicular expanded graphite; 99 to 99.5 parts of the phase change powder exists in each 100 parts by weight of the phase change material; 0.5 to 1 parts by weight of the vermicular expanded graphite per 100 parts by weight of the phase change material; the expansion rate of the vermicular expanded graphite is 100-600ml/g, the granularity is 100-200 meshes, the expansion multiple is 200-600 times, and the bulk density is 0.2-0.5 g/cm3。
In the embodiment of the application, aerogel can be selected as the adsorbing material, the aerogel has low heat conductivity coefficient, good heat preservation and insulation effects, stable physicochemical properties, high-temperature non-combustibility, complete water resistance, no toxicity, environmental friendliness, large specific surface area and very strong adsorption capacity to the phase-change powder, and the adsorption of the phase-change substance can be completed only by adopting a small amount of aerogel by weight, and certainly, the aerogel cannot be too little and cannot completely adsorb the phase-change substance; the aerogel also can not be too many, if too many increases the weight of cost and product on the one hand, simultaneously, has reduced the phase transition enthalpy that the aerogel adsorbs phase transition energy storage powder, has reduced the heat-retaining property of product, consequently, to different phase transition powder, the weight ratio that can adsorb phase transition powder completely just is the optimum.
Illustratively, if the adsorption carrier is aerogel, 50 to 90 parts by weight of the phase-change powder exist in each 100 parts by weight of the phase-change material; 10 to 50 parts of said aerogel per 100 parts by weight of said phase change material; the aerogel has the specific surface area of 100 square meters per gram and the particle size of 5-60 nm.
Relating to the preparation method
Referring to fig. 1, a method for preparing a single-component normal-temperature-curing encapsulating material according to an embodiment of the present invention includes:
101. preparing a phase change material;
heating the phase change powder to be molten, adding an adsorption carrier into the molten phase change powder in batches, and stirring, wherein after the adsorption carrier is added, vacuumizing a preparation environment, wherein the vacuum degree is-0.04 to-0.10 MPa, the vacuumizing time lasts for 5-40min, and the stirring time is 15-90 min; and after stirring in a vacuum state, respectively cooling, crushing and sieving the mixed material of the phase change powder and the adsorption carrier to obtain the phase change material.
For example, the heating device for the phase-change powder may be a reaction kettle, the cooling step may be performed to normal temperature, and the sieving device may be a device with a sieve of 10-100 meshes.
102. Mixing resin and the phase change material to obtain a mixed base material;
placing the temperature-sensitive curing resin (or moisture curing resin) and the phase change material in a vacuum kneader and stirring for 0.5-2 hours to obtain a mixed base material; the temperature in the vacuum kneading machine is 80-150 ℃, and the vacuum degree is-0.04-0.10 Mpa.
103. Stirring and mixing the base material and the curing agent, and the like to obtain the single-component normal-temperature curing encapsulating material.
Placing the mixed base material and the temperature-sensitive curing agent (or moisture curing agent) into a stirrer to be uniformly stirred to obtain the single-component normal-temperature curing encapsulating material; the stirring conditions include: the rotating speed is 30 r/min, the vacuum degree is between-0.04 and-0.10 MPa, and the stirring time is 0.5 to 1.5 hours.
It is understood that the preparation method of the moisture-curing potting material and the temperature-sensitive curing potting material are similar and will not be described herein.
In order to further reduce the usage amount of an adsorption carrier (vermicular expanded graphite or aerogel), in the phase change material preparation process, a vacuum adsorption process is adopted, stirring is carried out under a vacuum condition, the melted phase change powder can more easily and deeply permeate into a fluffy deep hole of the vermicular expanded graphite, the adsorption effect on the phase change material in the deep hole is far greater than that of conventional impregnation or stirring, the phase change material is difficult to overflow under a high-temperature condition after entering the deep hole, and the adsorption performance is superior, so that the vermicular expanded graphite adsorbs more phase change materials as few as possible, the phase change enthalpy of the graphite adsorption phase change energy storage powder is increased by 5-10%, the performance is greatly improved, and the cost is greatly reduced due to the reduction of the usage amount of the vermicular expanded graphite.
Example 1
The single-component normal-temperature curing encapsulating material comprises the following components in parts by weight: 40 parts of isocyanate prepolymer resin, 19.9 parts of polyol, 0.1 part of dibutyl tin dilaurate and 40 parts of phase change material, wherein the polyol comprises: polyether polyols, or polyester polyols; the phase change material takes graphite as an adsorption carrier and comprises the following components in parts by weight: 100 parts of paraffin and 5 parts of vermicular expanded graphite, wherein the vermicular expanded graphite has the expansion rate of 500ml/g, the granularity of 100 meshes, the expansion multiple of 400 times and the bulk density of 0.2g/cm3。
Example 2
The single-component normal-temperature curing encapsulating material comprises the following components in parts by weight: 13.29 parts of isocyanate prepolymer resin, 6.7 parts of polyol, 0.1 part of dibutyl tin dilaurate and 80 parts of phase change material, wherein the polyol comprises: polyether polyols, or polyester polyols; the phase change material takes graphite as an adsorption carrier and comprises the following components in parts by weight: 100 parts of paraffin and 9 parts of vermicular expanded graphite, wherein the vermicular expanded graphite has the expansion rate of 600ml/g, the granularity of 200 meshes, the expansion multiple of 600 times and the bulk density of 0.5g/cm3。
Example 3
The single-component normal-temperature curing encapsulating material comprises the following components in parts by weight: 49.9 parts of isocyanate prepolymer resin, 10 parts of polyol, 0.1 part of stannous octoate and 40 parts of phase change material, wherein the polyol comprises the following components in parts by weight: polyether polyols, or polyester polyols; the phase change material takes graphite as an adsorption carrier and comprises the following components in parts by weight: 100 parts of fatty acid and 6 parts of vermicular expanded graphite, wherein the vermicular expanded graphite has the expansion rate of 100ml/g, the granularity of 150 meshes, the expansion multiple of 500 times and the bulk density of 0.3g/cm3。
Example 4
The single-component normal-temperature curing encapsulating material comprises the following components in parts by weight: 29.7 parts of isocyanate prepolymer resin, 10 parts of polyol and 1, 3-phenylenedioxy bis (ethyl acetoacetate)0.3 part of titanium and 60 parts of phase change materials, wherein the polyol comprises: polyether polyols, or polyester polyols; the phase change material takes graphite as an adsorption carrier and comprises the following components in parts by weight: 100 parts of PE wax and 7 parts of vermicular expanded graphite, wherein the vermicular expanded graphite has the expansion rate of 520ml/g, the granularity of 120 meshes, the expansion multiple of 450 times and the bulk density of 0.2g/cm3。
Example 5
The single-component normal-temperature curing encapsulating material comprises the following components in parts by weight: 25 parts of polyol prepolymer resin, 24.9 parts of isocyanate, 0.1 part of dibutyl tin dilaurate and 50 parts of phase change material, wherein the isocyanate comprises the following components in parts by weight: at least one of polyisocyanate PAPI, diphenylmethane diisocyanate MDI and toluene diisocyanate TDI, wherein the phase change material takes graphite as an adsorption carrier and comprises the following components in parts by weight: 100 parts of PP wax and 8 parts of vermicular expanded graphite, wherein the vermicular expanded graphite has the expansion rate of 550ml/g, the granularity of 140 meshes, the expansion multiple of 460 times and the bulk density of 0.2g/cm3。
Example 6
The single-component normal-temperature curing encapsulating material comprises the following components in parts by weight: 25 parts of polyol prepolymer resin, 5.5 parts of isocyanate, 0.1 part of dibutyl tin dilaurate and 40 parts of phase change material, wherein the phase change material takes graphite as an adsorption carrier and comprises the following components in parts by weight: 100 parts of C40 alkane wax and 8.5 parts of vermicular expanded graphite, wherein the vermicular expanded graphite has the expansion rate of 570ml/g, the granularity of 200 meshes, the expansion multiple of 600 times and the bulk density of 0.3g/cm3。
Example 7
The single-component normal-temperature curing encapsulating material comprises the following components in parts by weight: 50 parts of polyol prepolymer resin, 9.9 parts of isocyanate, 0.1 part of dibutyl tin dilaurate and 40 parts of phase change material, wherein the phase change material takes graphite as an adsorption carrier and comprises the following components in parts by weight: 100 parts of C30 alkane wax and 8.8 parts of vermicular expanded graphiteThe ink has an expansion rate of 500ml/g, a particle size of 100 mesh, an expansion factor of 400 times, and a bulk density of 0.4g/cm3。
Example 8
The single-component normal-temperature curing encapsulating material comprises the following components in parts by weight: 30 parts of polyol prepolymer resin, 9 parts of isocyanate, 1 part of dibutyl tin dilaurate and 60 parts of phase change material, and at least one of polyisocyanate PAPI, MDI and TDI, wherein the phase change material takes graphite as an adsorption carrier and comprises the following components in parts by weight: 100 parts of C20 alkane wax and 7.3 parts of vermicular expanded graphite, wherein the vermicular expanded graphite has the expansion rate of 600ml/g, the granularity of 200 meshes, the expansion multiple of 600 times and the bulk density of 0.2g/cm3。
Example 9
The single-component normal-temperature curing encapsulating material comprises the following components in parts by weight: 20 parts of polyol prepolymer resin, 9.7 parts of isocyanate, 0.3 part of dibutyl tin dilaurate and 70 parts of phase change material, wherein the phase change material takes aerogel as an adsorption carrier and comprises the following components in parts by weight: 100 parts of C30 paraffin wax and 45 parts of aerogel, wherein the aerogel has a specific surface area of 260 square meters per gram and a particle size of 12 nm.
Example 10
The single-component normal-temperature curing encapsulating material comprises the following components in parts by weight: 20 parts of polyol prepolymer resin, 14.5 parts of isocyanate, 0.5 part of dibutyl tin dilaurate and 65 parts of phase change material, wherein the phase change material takes aerogel as an adsorption carrier and comprises the following components in parts by weight: 100 parts of C10 paraffin wax and 50 parts of aerogel, wherein the aerogel has a specific surface area of 300 square meters per gram and a particle size of 5 nm.
Example 11
The single-component normal-temperature curing encapsulating material comprises the following components in parts by weight: 40 parts of epoxy resin, 19.9 parts of imidazole curing agent, 0.1 part of dibutyl tin dilaurate and 40 parts of phase change substance, wherein the epoxy resin comprises: bisphenol A epoxy resin, modified epoxy resin, bisphenol S epoxy resin, bisphenol F type ringOxygen resins, epoxidized epoxy resins; the phase change material takes graphite as an adsorption carrier and comprises the following components in parts by weight: 100 parts of C20 alkane wax and 7.3 parts of vermicular expanded graphite, wherein the vermicular expanded graphite has the expansion rate of 600ml/g, the granularity of 200 meshes, the expansion multiple of 600 times and the bulk density of 0.2g/cm3。
Example 12
The single-component normal-temperature curing encapsulating material comprises the following components in parts by weight: 13.29 parts of epoxy resin, 6.7 parts of imidazole curing agent, 0.1 part of dibutyl tin dilaurate and 80 parts of phase change substance, wherein the epoxy resin comprises: bisphenol a type epoxy resin, modified epoxy resin, bisphenol S type epoxy resin, bisphenol F type epoxy resin, epoxidized epoxy resin; the phase change material takes graphite as an adsorption carrier and comprises the following components in parts by weight: 100 parts of C30 alkane wax and 8.8 parts of vermicular expanded graphite, wherein the vermicular expanded graphite has the expansion rate of 500ml/g, the granularity of 100 meshes, the expansion multiple of 400 times and the bulk density of 0.4g/cm3。
Example 13
The single-component normal-temperature curing encapsulating material comprises the following components in parts by weight: 49.9 parts of epoxy resin, 10 parts of polyol, 0.1 part of dibutyl tin dilaurate and 40 parts of phase change material, wherein the epoxy resin comprises the following components in parts by weight: bisphenol a type epoxy resin, modified epoxy resin, bisphenol S type epoxy resin, bisphenol F type epoxy resin, epoxidized epoxy resin; the phase change material takes graphite as an adsorption carrier and comprises the following components in parts by weight: 100 parts of C40 alkane wax and 8.5 parts of vermicular expanded graphite, wherein the vermicular expanded graphite has the expansion rate of 570ml/g, the granularity of 200 meshes, the expansion multiple of 600 times and the bulk density of 0.3g/cm3。
Example 14
The single-component normal-temperature curing encapsulating material comprises the following components in parts by weight: 29.8 parts of epoxy resin, 10 parts of polyol, 0.2 part of dibutyl tin dilaurate and 60 parts of phase change material, wherein the epoxy resin comprises: bisphenol a type epoxy resin, modified epoxy resin, bisphenol S type epoxy resin, bisphenol F type epoxy resin, epoxidized epoxy resin; the phase change material takes aerogel as an adsorption carrier and comprises the following components in parts by weight: 100 parts of C20 paraffin wax and 40 parts of aerogel, wherein the aerogel has a specific surface area of 220 square meters per gram and a particle size of 15 nm.
Example 15
The single-component normal-temperature curing encapsulating material comprises the following components in parts by weight: 25 parts of epoxy resin, 24.9 parts of methyl triethoxysilane, 0.1 part of dibutyl tin dilaurate and 10 parts of phase change substance, wherein the epoxy resin comprises the following components in parts by weight: bisphenol a type epoxy resin, modified epoxy resin, bisphenol S type epoxy resin, bisphenol F type epoxy resin, epoxidized epoxy resin; the phase change material takes aerogel as an adsorption carrier and comprises the following components in parts by weight: 100 parts of C30 paraffin wax and 45 parts of aerogel, wherein the aerogel has a specific surface area of 260 square meters per gram and a particle size of 12 nm.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims (10)

1. The single-component normal-temperature curing encapsulating material is characterized by comprising a mixture of the following substances: a carrier medium and a phase change material;
wherein from 20 to 60 parts of said carrier medium are present per 100 parts by weight of said mixture;
wherein 40 to 80 parts of said phase change material are present per 100 parts by weight of said mixture;
the carrier medium comprises: moisture-curable resins and moisture curing agents;
the phase change material includes: microencapsulated phase-change powder or mixed powder of the phase-change powder and an adsorption carrier, wherein the adsorption carrier is graphite or aerogel.
2. The single-component normal-temperature-curing potting material of claim 1, wherein:
50 to 83.3 parts of said moisture curable resin per 100 parts by weight of said carrier medium;
16.7 to 50 parts of said moisture curing agent per 100 parts by weight of said carrier medium;
the combination of the moisture-curable resin and the moisture curing agent includes any one of:
isocyanate prepolymer resin and polyol; wherein the polyol comprises: polyether polyols, or polyester polyols;
polyol prepolymer resin and isocyanate; wherein the isocyanate comprises: at least one of polyisocyanate PAPI, diphenylmethane diisocyanate MDI and toluene diisocyanate TDI;
if the combination of the moisture-curable resin and the moisture curing agent is an isocyanate prepolymer resin and a polyol, 66.7 to 83.3 parts of the isocyanate prepolymer resin are present per 100 parts by weight of the carrier medium; 16.7 to 33.3 parts of said polyol per 100 parts by weight of said carrier medium;
if the combination of the moisture curing resin and the moisture curing agent is polyol prepolymer resin and isocyanate, 50 to 83.3 parts of the polyol prepolymer resin is present per 100 parts by weight of the carrier medium; from 16.7 to 50 parts of said isocyanate per 100 parts by weight of said carrier medium.
3. The single-component normal-temperature-curing potting material of claim 1, further comprising: a thermally conductive filler;
the thermally conductive filler includes a combination of at least one of the following materials: aluminum oxide, aluminum nitride, boron nitride, magnesium oxide, zinc oxide, silicon carbide, graphite powder and carbon nanotubes; the heat conductive filler is present in an amount of 1 to 70 parts per 100 parts by weight of the one-component room temperature-curing potting material.
4. The one-component ambient temperature-curing potting material of claim 1,
if the adsorption carrier is graphite, the graphite is vermicular expanded graphite; 99 to 99.5 parts of the phase change powder exists in each 100 parts by weight of the phase change material; 0.5 to 1 parts by weight of the vermicular expanded graphite per 100 parts by weight of the phase change material;
the expansion rate of the vermicular expanded graphite is 100-600ml/g, the granularity is 100-200 meshes, the expansion multiple is 200-600 times, and the bulk density is 0.2-0.5 g/cm3；
If the adsorption carrier is aerogel, 50 to 90 parts of the phase-change powder exists in every 100 parts by weight of the phase-change substance; 10 to 50 parts of said aerogel per 100 parts by weight of said phase change material;
the aerogel has the specific surface area of 100 square meters per gram and the particle size of 5-60 nm.
5. The single-component normal-temperature-curing encapsulating material as claimed in any one of claims 1 to 4, wherein the phase-change powder is selected from at least one of the following materials: alkane waxes having an alkane carbon number between 10 and 60, paraffin waxes, fatty acids, PE waxes and PP waxes.
6. The single-component normal-temperature curing encapsulating material is characterized by comprising a mixture of the following substances: a carrier medium and a phase change material;
wherein from 20 to 60 parts of said carrier medium are present per 100 parts by weight of said mixture;
wherein 40 to 80 parts of said phase change material are present per 100 parts by weight of said mixture;
the carrier medium comprises: temperature-sensitive curing resin and temperature-sensitive curing agent;
the phase change material includes: the phase-change powder comprises phase-change powder and an adsorption carrier, wherein the adsorption carrier is graphite or aerogel.
7. The single-component normal-temperature-curing potting material of claim 6, wherein:
62.5 to 90 parts of said temperature sensitive curable resin per 100 parts by weight of said carrier medium;
10 to 37.5 parts of said temperature sensitive curing agent per 100 parts by weight of said carrier medium;
the combination of the temperature-sensitive curing resin and the temperature-sensitive curing agent comprises any one of the following components:
epoxy resin and imidazole curing agent; wherein the epoxy resin comprises: bisphenol a type epoxy resin, modified epoxy resin, bisphenol S type epoxy resin, bisphenol F type epoxy resin, epoxidized epoxy resin;
epoxy resin and amine hydrazine curing agents; wherein the epoxy resin comprises: bisphenol a type epoxy resin, modified epoxy resin, bisphenol S type epoxy resin, bisphenol F type epoxy resin, epoxidized epoxy resin.
8. The single-component normal-temperature-curing potting material of claim 6, further comprising: a thermally conductive filler;
the thermally conductive filler includes a combination of at least one of the following materials: aluminum oxide, aluminum nitride, boron nitride, magnesium oxide, zinc oxide, silicon carbide, graphite powder and carbon nanotubes;
the heat conductive filler is present in an amount of 1 to 70 parts per 100 parts by weight of the one-component room temperature-curing potting material.
9. The one-component ambient temperature-curing potting material of claim 6,
if the adsorption carrier is graphite, the graphite is vermicular expanded graphite; 99 to 99.5 parts of the phase change powder exists in each 100 parts by weight of the phase change material; 0.5 to 1 parts by weight of the vermicular expanded graphite per 100 parts by weight of the phase change material;
the expansion rate of the vermicular expanded graphite is 100-600ml/g, the granularity is 100-200 meshes, the expansion multiple is 200-600 times, and the bulk density is 0.2-0.5 g/cm3；
If the adsorption carrier is aerogel, 50 to 90 parts of the phase-change powder exists in every 100 parts by weight of the phase-change substance; 10 to 50 parts of said aerogel per 100 parts by weight of said phase change material;
the aerogel has the specific surface area of 100 square meters per gram and the particle size of 5-60 nm.
10. The single-component normal-temperature-curing encapsulating material as claimed in any one of claims 6 to 9, wherein the phase-change powder is selected from at least one of the following materials: alkane waxes having an alkane carbon number between 10 and 60, paraffin waxes, fatty acids, PE waxes and PP waxes.
CN201911159033.XA 2019-11-22 2019-11-22 Single-component normal-temperature curing encapsulating material Withdrawn CN110724489A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111303821A (en) * 2020-03-14 2020-06-19 广东力王新材料有限公司 Single-component heat storage potting material
CN111826129A (en) * 2020-07-16 2020-10-27 广东力王新材料有限公司 Preparation method of phase-change sheet
CN111978679A (en) * 2020-08-31 2020-11-24 广东力王新材料有限公司 Crystalline hydrated salt phase-change material and preparation method thereof
CN116200044A (en) * 2023-03-06 2023-06-02 广东力王新材料有限公司 Resin type phase change energy storage material and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111303821A (en) * 2020-03-14 2020-06-19 广东力王新材料有限公司 Single-component heat storage potting material
CN111826129A (en) * 2020-07-16 2020-10-27 广东力王新材料有限公司 Preparation method of phase-change sheet
CN111978679A (en) * 2020-08-31 2020-11-24 广东力王新材料有限公司 Crystalline hydrated salt phase-change material and preparation method thereof
CN116200044A (en) * 2023-03-06 2023-06-02 广东力王新材料有限公司 Resin type phase change energy storage material and preparation method thereof

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