WO2021097853A1 - 单组分常温固化灌封材料 - Google Patents

单组分常温固化灌封材料 Download PDF

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WO2021097853A1
WO2021097853A1 PCT/CN2019/120435 CN2019120435W WO2021097853A1 WO 2021097853 A1 WO2021097853 A1 WO 2021097853A1 CN 2019120435 W CN2019120435 W CN 2019120435W WO 2021097853 A1 WO2021097853 A1 WO 2021097853A1
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parts
phase change
weight
epoxy resin
room temperature
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PCT/CN2019/120435
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English (en)
French (fr)
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张立强
张秋兵
杨小玉
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张立强
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Priority to PCT/CN2019/120435 priority Critical patent/WO2021097853A1/zh
Publication of WO2021097853A1 publication Critical patent/WO2021097853A1/zh

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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
    • 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
    • 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

Definitions

  • the invention relates to the technical field of potting materials and preparation methods thereof, in particular to a single-component room temperature curing potting material.
  • the electronic potting glue is liquid before curing and has fluidity.
  • the viscosity of the glue varies according to the material, performance, and production process of the product.
  • the potting glue can only realize its use value after it is completely cured. After curing, it can play the role of waterproof, moisture-proof, dust-proof, insulation, heat conduction, confidentiality, corrosion resistance, temperature resistance and shock resistance.
  • One of the objectives of the present invention is to provide a one-component room temperature curing potting material to solve the heat dissipation problem of electronic potting glue in the prior art.
  • the one-component room temperature curing potting material provided by the first aspect of the embodiments of the present invention includes a mixture of the following substances: a carrier medium and a phase change substance;
  • phase change substance there are 40 to 80 parts of the phase change substance in every 100 parts by weight of the mixture;
  • the carrier medium includes: moisture curing resin and moisture curing agent
  • the phase change substance includes: a microencapsulated phase change powder, or a mixed powder of a phase change powder and an adsorption carrier, and the adsorption carrier is graphite or aerogel. .
  • the combination of the moisture curing resin and the moisture curing agent includes any one of the following:
  • Isocyanate prepolymer resin and polyol wherein, the polyol includes: polyether polyol or polyester polyol;
  • Polyol prepolymer resin and isocyanate wherein, the isocyanate includes at least one of polyisocyanate PAPI, MDI, and TDI.
  • the combination of the moisture curing resin and the moisture curing agent is an isocyanate prepolymer resin and a polyol
  • Prepolymer resin is present; 16.7 to 33.3 parts of the polyol are present in every 100 parts by weight of the carrier medium;
  • the combination of the moisture curing resin and the moisture curing agent is a polyol prepolymer resin and an isocyanate
  • the one-component room temperature curing potting material further includes: 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;
  • thermally conductive filler there are 1 to 70 parts of the thermally conductive filler in every 100 parts by weight of the one-component room temperature curing potting material.
  • the graphite is vermicular expanded graphite; 99 to 99.5 parts of the phase change powder are present in every 100 parts by weight of the phase change material; 0.5 to 1 part of the vermicular expanded graphite exists in 100 parts by weight of the phase change material;
  • the worm-like expanded graphite has an expansion ratio of 100-600 ml/g, a particle size of 100-200 mesh, an expansion ratio of 200-600 times, and a bulk density of 0.2-0.5 g/cm 3 .
  • the adsorption carrier is an aerogel
  • 50 to 90 parts of the phase change powder exists in every 100 parts by weight of the phase change material; every 100 parts by weight of the phase change There are 10 to 50 parts of the aerogel in the variable substance;
  • the specific surface area of the aerogel is 100-300 m 2 /g, and the particle size is 5-60 nm.
  • the phase change powder is selected from at least one of the following materials: alkane wax, paraffin wax, fatty acid, PE wax and PP wax, and the alkane carbon number of the alkane wax is between 10-60 between.
  • the preparation method of the one-component room temperature curing potting material includes:
  • phase change powder is heated to melt, and the adsorption carrier is added to the melted phase change powder in batches and stirred.
  • the preparation environment is evacuated, and the vacuum degree is between -0.04 and -0.10MPa
  • the vacuuming time lasts for 5-40min, and the stirring time is 15-90min; after the stirring is completed in the vacuum state, the mixed material of the phase change powder and the adsorption carrier is separately cooled, crushed and sieved to obtain the phase Change matter
  • the moisture curable resin and the phase change substance are placed in a vacuum kneader and stirred for 0.5 to 2 hours to obtain a mixed base material; the temperature in the vacuum kneader is 80 to 150°C, and the vacuum degree is between- 0.04 to -0.10Mpa;
  • the stirring conditions include: rotating speed 30 revolutions/min, vacuum degree between -0.04 to -0.10MPa, stirring time 0.5 to 1.5 hours.
  • the one-component room temperature curing potting material provided in the second aspect of the embodiments of the present invention includes a mixture of the following substances: a carrier medium and a phase change substance;
  • phase change substance there are 40 to 80 parts of the phase change substance in every 100 parts by weight of the mixture;
  • the carrier medium includes: a temperature-sensitive curing resin and a temperature-sensitive curing agent;
  • the phase change substance includes: a phase change powder and an adsorption carrier, and the adsorption carrier is graphite or aerogel.
  • 62.5 to 90 parts of the temperature-sensitive curable resin are present in every 100 parts by weight of the carrier medium;
  • the combination of the temperature-sensitive curing resin and the temperature-sensitive curing agent includes any one of the following:
  • Epoxy resin and imidazole curing agent wherein, the epoxy resin includes: bisphenol A type epoxy resin, modified epoxy resin, bisphenol S type epoxy resin, bisphenol F type epoxy resin, epoxy resin Epoxy resin
  • Epoxy resin and amine hydrazine curing agent wherein, the epoxy resin includes: bisphenol A type epoxy resin, modified epoxy resin, bisphenol S type epoxy resin, bisphenol F type epoxy resin, ring Oxidized epoxy resin.
  • the one-component room temperature curing potting material further includes: 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;
  • thermally conductive filler there are 1 to 70 parts of the thermally conductive filler in every 100 parts by weight of the one-component room temperature curing potting material.
  • the graphite is vermicular expanded graphite; 99 to 99.5 parts of the phase change powder are present in every 100 parts by weight of the phase change material; 0.5 to 1 part of the vermicular expanded graphite exists in 100 parts by weight of the phase change material;
  • the worm-like expanded graphite has an expansion ratio of 100-600 ml/g, a particle size of 100-200 mesh, an expansion ratio of 200-600 times, and a bulk density of 0.2-0.5 g/cm 3 .
  • the adsorption carrier is an aerogel
  • 50 to 90 parts of the phase change powder exists in every 100 parts by weight of the phase change material; every 100 parts by weight of the phase change There are 10 to 50 parts of the aerogel in the variable substance;
  • the specific surface area of the aerogel is 100-300 m 2 /g, and the particle size is 5-60 nm.
  • the phase change powder is selected from at least one of the following materials: alkane wax, paraffin wax, fatty acid, PE wax and PP wax, and the alkane carbon number of the alkane wax is between 10-60 between.
  • it includes:
  • phase change powder is heated to melt, and the adsorption carrier is added to the melted phase change powder in batches and stirred.
  • the preparation environment is evacuated, and the vacuum degree is between -0.04 and -0.10MPa
  • the vacuuming time lasts for 5-40min, and the stirring time is 15-90min; after the stirring is completed in the vacuum state, the mixed material of the phase change powder and the adsorption carrier is separately cooled, crushed and sieved to obtain the phase Change matter
  • the temperature-sensitive curing resin and the phase change material are placed in a vacuum kneader and stirred for 0.5 to 2 hours to obtain a mixed base material; the temperature in the vacuum kneader is 80 to 150°C, and the vacuum degree is between- 0.04 to -0.10Mpa;
  • the stirring conditions include: rotating speed 30 revolutions/min, vacuum degree between -0.04 to -0.10MPa, stirring time 0.5 to 1.5 hours.
  • the single-component room temperature curing potting material of the present invention 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, which is the endothermic value; phase transition temperature (°C) 5 ⁇ 90; specific gravity (g/cc): 0.8 ⁇ 1.8, surface drying time: 5min ⁇ 25min; curing time: 1h ⁇ 2h; complete curing time ⁇ 24h.
  • the single-component room temperature curing potting material with the above formula has excellent heat absorption and temperature control performance, and can effectively control the electronic equipment in the electronic potting glue at a suitable temperature without overheating.
  • Fig. 1 is a schematic flow chart of a preparation method of a single-component room temperature curing potting material in an embodiment of the present invention.
  • Electronic potting glue is used to wrap and seal electronic devices in various scenes and shapes. Therefore, electronic potting glue is liquid before curing. In practical applications, in order to facilitate the sealing of electronic equipment and reduce the requirements for the sealing environment, the potting material can be prepared to be cured at room temperature.
  • the one-component room temperature curing potting material can be divided into moisture curing potting material and temperature curing potting material.
  • Moisture curing potting materials that is, when exposed to the air, the curing reaction will occur when they are exposed to water vapor in the air.
  • the moisture curing potting material includes a mixture of the following substances: carrier medium and phase change substance.
  • the carrier medium is a substance that binds and carries a phase change substance.
  • the phase change material is the material after adsorbing the phase change powder
  • the phase change powder is the powder material that absorbs or releases heat by changing the physical form.
  • phase change substance there are 40 to 80 parts of the phase change substance in every 100 parts by weight of the mixture;
  • the carrier medium includes: a moisture curing resin and a moisture curing agent; the moisture curing agent is a chemical additive that cures the moisture curing resin. Specifically, the combination of different moisture curing resins and moisture curing agents in practical applications, and the ratio range of related materials will be described in detail in Examples 1 to 10 below.
  • the phase change substance includes: a phase change powder and an adsorption carrier, and the adsorption carrier is graphite or aerogel.
  • the phase change powder is selected from at least one of the following materials: alkane wax, paraffin wax, fatty acid, PE wax and PP wax, and the alkane carbon number of the alkane wax is between 10-60.
  • the carrier medium there are 50 to 83.3 parts of the carrier medium per 100 parts by weight of the carrier medium
  • the moisture curing resin is present, and 16.7 to 50 parts of the moisture curing agent is present in every 100 parts by weight of the carrier medium, and the details are not limited here.
  • Temperature-sensitive curing potting material that is, a curing reaction will occur when the temperature is sensed in a normal temperature environment (20-40 degrees Celsius). Therefore, the temperature-sensitive curing potting material in the embodiment of the present invention requires refrigerated storage and transportation.
  • Thermal curing potting material including a mixture of the following substances: carrier medium and phase change substance;
  • phase change substance there are 40 to 80 parts of the phase change substance in every 100 parts by weight of the mixture;
  • the carrier medium includes: a temperature-sensitive curing resin and a temperature-sensitive curing agent; the temperature-sensitive curing agent is a chemical additive for curing the temperature-sensitive curing resin. Specifically, the combination of different temperature-sensitive curing resins and temperature-sensitive curing agents in practical applications, and the ratio range of related materials will be described in detail in the following embodiments 11-15.
  • the phase change substance includes: a microencapsulated phase change powder, or a mixed powder of a phase change powder and an adsorption carrier, and the adsorption carrier is graphite or aerogel.
  • the phase change powder is selected from at least one of the following materials: alkane wax, paraffin wax, fatty acid, PE wax and PP wax, and the alkane carbon number of the alkane wax is between 10-60.
  • the requirements for the hardness, toughness, plasticity, heat absorption, specific heat capacity, volume, and material cost of the potting material there are 62.5 to 90 parts of the carrier medium per 100 parts by weight of the carrier medium.
  • the temperature-sensitive curing resin is present; there are 10-37.5 parts of the temperature-sensitive curing agent in every 100 parts by weight of the carrier medium, and the details are not limited here.
  • the potting material Since the main function of the single-component room temperature curing potting material in the embodiment of the present invention is to absorb the heat of the electronic device, the potting material needs to have good thermal conductivity.
  • a single-component room temperature curing potting material is added with a thermally conductive filler to make it have good thermal conductivity.
  • 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.
  • a thermally conductive filler can be added to enhance the thermal conductivity of the potting material.
  • a one-component room temperature curing potting material needs to use a catalytic material to meet or strengthen the curing effect of the potting material.
  • certain curing agents have a catalytic effect (that is, the curing agent acts as both a curing material and a catalytic material at the same time), therefore, the catalyst is not a necessary additive material in the embodiments of the present invention.
  • the following is only an exemplary description of the catalyst. Whether to add, which type to add, and how much to add, all need to be determined according to actual needs, and there is no specific limitation here.
  • the catalyst may be any one of dibutyl tin dilaurate, stannous octoate, and 1,3-phenylenedioxy bis(ethyl acetoacetate) titanium.
  • phase change powder In the actual use of phase change powder, after the phase change powder is transformed from solid to liquid, it may leak out in the potting material. Therefore, it is necessary to adsorb and wrap the phase change powder through an adsorption carrier to prevent Overflow of phase change powder.
  • vermicular expanded graphite can be used as the adsorbent.
  • Vermicular expanded graphite is a loose and porous vermicular substance obtained by intercalation, washing, drying, and high temperature expansion of natural flake graphite. Expanded graphite has In addition to the excellent properties of natural graphite, such as heat resistance, corrosion resistance, self-lubrication, radiation resistance, electrical conductivity, etc., natural graphite also has softness, compression resilience, adsorption, ecological environment coordination, biocompatibility, etc. that natural graphite does not have. Radiation resistance and other characteristics, due to its looseness and porousness and large specific surface area, it has a very strong adsorption capacity for phase change powders.
  • Vermicular expanded graphite should not be too little, too little can not completely adsorb the phase change material; vermicular expanded graphite can not be too much, too much, on the one hand, increase the cost and reduce the enthalpy value of the product, and at the same time, reduce the graphite adsorption phase change
  • the phase change enthalpy of the energy storage powder reduces the heat storage performance of the product. Therefore, for different powders, the weight ratio of the phase change powder that can be completely absorbed is the optimal.
  • the graphite is vermicular expanded graphite; there are 99-99.5 parts of the phase change powder present in every 100 parts by weight of the phase change material; every 100 parts by weight There are 0.5 to 1 part of the vermicular expanded graphite in the phase change material; the expansion rate of the vermicular expanded graphite is 100-600ml/g, the particle size is 100-200 mesh, and the expansion ratio is 200-600 times , The bulk density is 0.2 ⁇ 0.5g/cm 3 .
  • aerogel can also be used as the adsorbent material.
  • Aerogel has low thermal conductivity, good thermal insulation effect, stable physical and chemical properties, non-combustible at high temperature, completely waterproof, non-toxic, green and environmentally friendly, and has a specific surface area. Large, the adsorption capacity for phase change powder is very strong. Only a small amount of aerogel can be used to complete the adsorption of phase change substances. Of course, there should not be too little aerogel, and too little aerogel can completely adsorb the phase. The aerogel should not be too much. If too much, it will increase the cost and the weight of the product.
  • the weight ratio of the phase change powders that can be completely absorbed is optimal.
  • the adsorption carrier is an aerogel
  • 50 to 90 parts of the phase change powder exists in every 100 parts by weight of the phase change material; every 100 parts by weight of the phase change material
  • the preparation method of the one-component room temperature curing potting material in the embodiment of the present invention includes:
  • the phase change powder is heated to melting, and the adsorption carrier is added to the melted phase change powder in batches and stirred.
  • the preparation environment is evacuated, and the vacuum degree is between -0.04 and -0.10MPa
  • the vacuuming time lasts for 5-40min, and the stirring time is 15-90min; after the completion of the stirring in the vacuum state, the phase change powder and the mixed material of the adsorption carrier are respectively cooled, crushed and sieved to obtain the phase Change matter.
  • the heating device for the phase change powder may be a reaction kettle, and the above cooling step may be cooled to normal temperature, and the sieving device may be a 10-100 mesh sieve device.
  • the temperature-sensitive curable resin (or moisture curable resin) and the phase change substance are placed in a vacuum kneader and stirred for 0.5 to 2 hours to obtain a mixed base material; the temperature in the vacuum kneader is 80 to 150°C , The vacuum degree is between -0.04 to -0.10Mpa.
  • the stirring conditions include: rotating speed 30 revolutions per minute, The vacuum degree is between -0.04 to -0.10MPa, and the stirring time is 0.5 to 1.5 hours.
  • a vacuum adsorption process is adopted in the preparation process of phase change material. Stir under vacuum conditions, and the melted phase change powder is easier to penetrate deeply. Penetrating into the fluffy deep pores of the worm-like expanded graphite, the adsorption of phase change substances in the deep pores is far greater than that of conventional immersion or stirring. After the phase change substances enter the deep pores, it is difficult to overflow under high temperature conditions, and has extraordinary characteristics.
  • the one-component room temperature curing potting material includes the following components 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 substance, of which,
  • the polyol includes: polyether polyol or polyester polyol;
  • the phase change material uses graphite as an adsorption carrier, and includes the following components by weight: 100 parts of paraffin wax and 5 parts of worm-like expanded graphite, so
  • the worm-like expanded graphite has an expansion rate of 500 ml/g, a particle size of 100 mesh, an expansion ratio of 400 times, and a bulk density of 0.2 g/cm 3 .
  • One-component room temperature curing potting material including the following components by weight: 13.29 parts of isocyanate prepolymer resin, 6.7 parts of polyol, 0.1 of dibutyl tin dilaurate and 80 parts of phase change substance, the polyol It includes: polyether polyol or polyester polyol; the phase change material uses graphite as an adsorption carrier, and includes the following components by weight: 100 parts of paraffin wax and 9 parts of vermicular expanded graphite, the vermicular expanded graphite The expansion rate is 600ml/g, the particle size is 200 mesh, the expansion ratio is 600 times, and the bulk density is 0.5g/cm 3 .
  • the one-component room temperature curing potting material includes 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 substance.
  • the polyol includes: polyol. Ether polyol or polyester polyol; the phase change material uses graphite as an adsorption carrier, and includes the following components by weight: 100 parts of fatty acid and 6 parts of worm-like expanded graphite, the expansion rate of the worm-like expanded graphite It is 100ml/g, the particle size is 150 mesh, the expansion ratio is 500 times, and the bulk density is 0.3g/cm 3 .
  • One-component room temperature curing potting material including the following components by weight: 29.7 parts of isocyanate prepolymer resin, 10 parts of polyol, 1,3-phenylenedioxy bis(ethyl acetoacetate) titanium 0.3 Parts and 60 parts of phase change material
  • the polyol includes: polyether polyol or polyester polyol
  • the phase change material uses graphite as the adsorption carrier, including the following parts by weight of each component: 100 parts of PE wax and 7 parts of vermicular expanded graphite, the expansion rate of the vermicular expanded graphite is 520 ml/g, the particle size is 120 mesh, the expansion ratio is 450 times, and the bulk density is 0.2 g/cm 3 .
  • the one-component room temperature curing potting material includes 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, the isocyanate Including: at least one of polyisocyanate PAPI, diphenylmethane diisocyanate MDI, and toluene diisocyanate TDI.
  • the phase change material uses graphite as an adsorption carrier and includes the following components by weight: 100 parts of PP wax and worms 8 parts of worm-like expanded graphite, the worm-like expanded graphite has an expansion rate of 550 ml/g, a particle size of 140 mesh, an expansion ratio of 460 times, and a bulk density of 0.2 g/cm 3 .
  • One-component room temperature curing potting material including the following components 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 substance, polyisocyanate PAPI
  • the phase change material uses graphite as the adsorption carrier, and includes the following components in parts by weight: 100 parts of C40 alkane wax and 8.5 parts of vermicular expanded graphite.
  • the expansion rate is 570ml/g
  • the particle size is 200 meshes
  • the expansion ratio is 600 times
  • the bulk density is 0.3g/cm 3 .
  • One-component room temperature curing potting material including the following components 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 substance, polyisocyanate PAPI
  • At least one of, MDI, TDI, the phase change material uses graphite as the adsorption carrier, and includes the following components by weight: 100 parts of C30 alkane wax and 8.8 parts of vermicular expanded graphite.
  • the expansion rate is 500ml/g
  • the particle size is 100 mesh
  • the expansion ratio is 400 times
  • the bulk density is 0.4g/cm 3 .
  • One-component room temperature curing potting material including the following 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 substance, polyisocyanate PAPI
  • the phase change material uses graphite as the adsorption carrier, and includes the following components in parts by weight: 100 parts of C20 alkane wax and 7.3 parts of vermicular expanded graphite.
  • the expansion rate is 600ml/g
  • the particle size is 200 meshes
  • the expansion ratio is 600 times
  • the bulk density is 0.2g/cm 3 .
  • One-component room temperature curing potting material including the following components by weight: 20 parts of polyol prepolymer resin, 9.7 parts of isocyanate, 0.3 parts of dibutyl tin dilaurate and 70 parts of phase change substance, polyisocyanate PAPI
  • At least one of MDI, TDI, the phase change material uses aerogel as the adsorption carrier, and includes the following components by weight: 100 parts of C30 alkane wax and 45 parts of aerogel, the ratio of the aerogel The surface area is 260 m 2 /g and the particle size is 12 nm.
  • One-component room temperature curing potting material including the following components 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 substance, polyisocyanate PAPI
  • the phase change material uses aerogel as the adsorption carrier, and includes the following components by weight: 100 parts of C10 alkane wax and 50 parts of aerogel, the ratio of the aerogel The surface area is 300m 2 /g and the particle size is 5nm.
  • the one-component room temperature curing potting material includes the following components 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, of which,
  • the epoxy resin includes: bisphenol A epoxy resin, modified epoxy resin, bisphenol S epoxy resin, bisphenol F epoxy resin, epoxidized epoxy resin;
  • the phase change material is graphite
  • the adsorption carrier it includes the following components in parts by weight: 100 parts of C20 alkane wax and 7.3 parts of worm-like expanded graphite.
  • the worm-like expanded graphite has an expansion rate of 600ml/g, a particle size of 200 mesh, and an expansion ratio of 600 times.
  • the bulk density is 0.2g/cm 3 .
  • One-component room temperature curing potting material including the following components 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, of which,
  • the epoxy resin includes: bisphenol A epoxy resin, modified epoxy resin, bisphenol S epoxy resin, bisphenol F epoxy resin, epoxidized epoxy resin;
  • the phase change material is graphite
  • the adsorption carrier it includes the following components in parts by weight: 100 parts of C30 alkane wax and 8.8 parts of worm-like expanded graphite.
  • the worm-like expanded graphite has an expansion rate of 500ml/g, a particle size of 100 mesh, and an expansion ratio of 400 times.
  • the bulk density is 0.4g/cm 3 .
  • the one-component room temperature curing potting material includes the following components in parts by weight: 49.9 parts by weight of epoxy resin, 10 parts by polyol, 0.1 part by dibutyl tin dilaurate and 40 parts by phase change substance, wherein the ring Oxygen resins include: bisphenol A type epoxy resin, modified epoxy resin, bisphenol S type epoxy resin, bisphenol F type epoxy resin, and epoxidized epoxy resin; the phase change substance uses graphite as an adsorbent
  • the carrier includes the following components in parts by weight: 100 parts of C40 alkane wax and 8.5 parts of worm-like expanded graphite.
  • the worm-like expanded graphite has an expansion rate of 570ml/g, a particle size of 200 mesh, and an expansion ratio of 600 times.
  • the density is 0.3g/cm 3 .
  • the one-component room temperature curing potting material includes the following components in parts by weight: 29.8 parts by weight of epoxy resin, 10 parts by polyol, 0.2 parts by dibutyl tin dilaurate and 60 parts by phase change substance, wherein the ring Oxygen resins include: 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 is an aerogel As the adsorption carrier, it includes the following components in parts by weight: 100 parts of C20 alkane wax and 40 parts of aerogel. The aerogel has a specific surface area of 220 m 2 /g and a particle size of 15 nm.
  • One-component room temperature curing potting material including the following components in parts by weight: 25 parts of epoxy resin, 24.9 parts of methyltriethoxysilane, 0.1 part of dibutyl tin dilaurate and 10 parts of phase change substance
  • the epoxy resin includes: bisphenol A type epoxy resin, modified epoxy resin, bisphenol S type epoxy resin, bisphenol F type epoxy resin, and epoxidized epoxy resin
  • the substance uses aerogel as an adsorption carrier, and includes the following components in parts by weight: 100 parts of C30 alkane wax and 45 parts of aerogel.
  • the aerogel has a specific surface area of 260 m 2 /g and a particle size of 12 nm.

Abstract

单组分常温固化灌封材料，包括以下物质的混合物：载体介质和相变物质；其中，每100份重量的所述混合物中有20至60份所述载体介质存在；其中，每100份重量的所述混合物中有40至80份所述相变物质存在；所述载体介质包括：湿气固化树脂和湿气固化剂；所述相变物质包括：微胶囊化相变粉体，或相变粉体和吸附载体的混合粉体，所述吸附载体为石墨或气凝胶。采用上述配方的单组分常温固化灌封材料具备了优异的吸热和控温性能，可以有效地将电子灌封胶内电子设备控制在合适的温度内，不会发生过热的情况。

Description

单组分常温固化灌封材料 技术领域
本发明涉及灌封材料及其制备方法技术领域，尤其涉及一种单组分常温固化灌封材料。
背景技术
电子灌封胶在未固化前属于液体状，具有流动性，胶液黏度根据产品的材质、性能、生产工艺的不同而有所区别。灌封胶完全固化后才能实现它的使用价值，固化后可以起到防水防潮、防尘、绝缘、导热、保密、防腐蚀、耐温、防震的作用。
然而，由于现在对电子设备的性能要求越来越高，因而电子设备的发热问题越来越严重，现有的电子灌封胶的散热性能远远达不到要求。
发明内容
本发明的目的之一是提供一种单组分常温固化灌封材料，以解决现有技术中电子灌封胶散热问题。
为实现上述目的，本发明采用如下的技术方案：
本发明实施例第一方面提供的单组分常温固化灌封材料，包括以下物质的混合物：载体介质和相变物质；
其中，每100份重量的所述混合物中有20至60份所述载体介质存在；
其中，每100份重量的所述混合物中有40至80份所述相变物质存在；
所述载体介质包括：湿气固化树脂和湿气固化剂；
所述相变物质包括：微胶囊化相变粉体，或相变粉体和吸附载体的混合粉体，所述吸附载体为石墨或气凝胶。。
在一种实施方式中，
每100份重量的所述载体介质中有50至83.3份所述湿气固化树脂存在；
每100份重量的所述载体介质中有16.7至50份所述湿气固化剂存在。
在一种实施方式中，所述湿气固化树脂和湿气固化剂的组合包括以下任一种：
异氰酸酯预聚体树脂和多元醇；其中，所述多元醇包括：聚醚多元醇、或聚酯多元醇；
多元醇预聚体树脂和异氰酸酯；其中，所述异氰酸酯包括：多异氰酸酯PAPI、MDI、TDI中的至少一种。
在一种实施方式中，若所述湿气固化树脂和湿气固化剂的组合为异氰酸酯预聚体树脂和多元醇，则每100份重量的所述载体介质中有66.7至83.3份所述异氰酸酯预聚体树脂存在；每100份重量的所述载体介质中有16.7至33.3份所述多元醇存在；
若所述湿气固化树脂和湿气固化剂的组合为多元醇预聚体树脂和异氰酸酯，则每100份重量的所述载体介质中有50至83.3份所述多元醇预聚体树脂存；每100份重量的所述载体介质中有16.7至50份所述异氰酸酯存在。
在一种实施方式中，所述单组分常温固化灌封材料，还包括：导热填料；
所述导热填料包括以下至少一种材料的组合：氧化铝、氮化铝、氮化硼、 氧化镁、氧化锌、碳化硅、石墨粉和碳纳米管；
每100份重量的所述单组分常温固化灌封材料中有1至70份所述导热填料存在。
在一种实施方式中，若所述吸附载体为石墨，则所述石墨为蠕虫状膨胀石墨；每100份重量的所述相变物质中有99至99.5份所述相变粉体存在；每100份重量的所述相变物质中有0.5至1份所述蠕虫状膨胀石墨存在；
所述蠕虫状膨胀石墨的膨胀率为100-600ml/g，粒度为100-200目，膨胀倍数为200-600倍，堆积密度为0.2～0.5g/cm 3。
在一种实施方式中，若所述吸附载体为气凝胶，则每100份重量的所述相变物质中有50至90份所述相变粉体存在；每100份重量的所述相变物质中有10至50份所述气凝胶存在；
所述气凝胶的比表面积为100-300m 2/g，粒径为5-60nm。
在一种实施方式中，所述相变粉体选自以下材料的至少一种：烷烃蜡、石蜡、脂肪酸、PE蜡和PP蜡，所述烷烃蜡的烷烃碳原子数介于10-60之间。
在一种实施方式中，单组分常温固化灌封材料的制备方法，包括：
将相变粉体加热至熔化，将吸附载体分批加入至熔化后的相变粉体中搅拌，所述吸附载体添加完成后，将制备环境抽真空，真空度介于-0.04至-0.10MPa，抽真空的时间持续5-40min，搅拌时间为15-90min；在真空状态搅拌完成后，将相变粉体和吸附载体的混合材料分别进行冷却、粉碎以及过筛的步骤，得到所述相变物质；
将所述湿气固化树脂和所述相变物质置于真空捏合机内搅拌0.5～2小时，得到混合基料；所述真空捏合机内的温度为80～150℃，真空度为介于-0.04至 -0.10Mpa；
将所述混合基料，所述湿气固化剂置于搅拌机内进行搅拌均匀，得到所述单组分常温固化灌封材料；搅拌条件包括：转速30转/分钟，真空度介于-0.04至-0.10MPa，搅拌时间0.5～1.5小时。
本发明实施例第二方面提供的单组分常温固化灌封材料，包括以下物质的混合物：载体介质和相变物质；
其中，每100份重量的所述混合物中有20至60份所述载体介质存在；
其中，每100份重量的所述混合物中有40至80份所述相变物质存在；
所述载体介质包括：温感固化树脂和温感固化剂；
所述相变物质包括：相变粉体和吸附载体，所述吸附载体为石墨或气凝胶。
在一种实施方式中，每100份重量的所述载体介质中有62.5至90份所述温感固化树脂存在；
每100份重量的所述载体介质中有10至37.5份所述温感固化剂存在。
在一种实施方式中，所述温感固化树脂和温感固化剂的组合包括以下任一种：
环氧树脂和咪唑类固化剂；其中，所述环氧树脂包括：双酚A型环氧树脂、改性环氧树脂、双酚S型环氧树脂、双酚F型环氧树脂、环氧化环氧树脂；
环氧树脂和胺肼类固化剂；其中，所述环氧树脂包括：双酚A型环氧树脂、改性环氧树脂、双酚S型环氧树脂、双酚F型环氧树脂、环氧化环氧树脂。
在一种实施方式中，所述单组分常温固化灌封材料，还包括：导热填料；
所述导热填料包括以下至少一种材料的组合：氧化铝、氮化铝、氮化硼、氧化镁、氧化锌、碳化硅、石墨粉和碳纳米管；
每100份重量的所述单组分常温固化灌封材料中有1至70份所述导热填料存在。
在一种实施方式中，若所述吸附载体为石墨，则所述石墨为蠕虫状膨胀石墨；每100份重量的所述相变物质中有99至99.5份所述相变粉体存在；每100份重量的所述相变物质中有0.5至1份所述蠕虫状膨胀石墨存在；
所述蠕虫状膨胀石墨的膨胀率为100-600ml/g，粒度为100-200目，膨胀倍数为200-600倍，堆积密度为0.2～0.5g/cm 3。
在一种实施方式中，若所述吸附载体为气凝胶，则每100份重量的所述相变物质中有50至90份所述相变粉体存在；每100份重量的所述相变物质中有10至50份所述气凝胶存在；
所述气凝胶的比表面积为100-300m 2/g，粒径为5-60nm。
在一种实施方式中，所述相变粉体选自以下材料的至少一种：烷烃蜡、石蜡、脂肪酸、PE蜡和PP蜡，所述烷烃蜡的烷烃碳原子数介于10-60之间。
在一种实施方式中，包括：
将相变粉体加热至熔化，将吸附载体分批加入至熔化后的相变粉体中搅拌，所述吸附载体添加完成后，将制备环境抽真空，真空度介于-0.04至-0.10MPa，抽真空的时间持续5-40min，搅拌时间为15-90min；在真空状态搅拌完成后，将相变粉体和吸附载体的混合材料分别进行冷却、粉碎以及过筛的步骤，得到所述相变物质；
将所述温感固化树脂和所述相变物质置于真空捏合机内搅拌0.5～2小时，得到混合基料；所述真空捏合机内的温度为80～150℃，真空度为介于-0.04至-0.10Mpa；
将所述混合基料，所述温感固化剂置于搅拌机内进行搅拌均匀，得到所述单组分常温固化灌封材料；搅拌条件包括：转速30转/分钟，真空度介于-0.04至-0.10MPa，搅拌时间0.5～1.5小时。
与现有技术相比，本发明的单组分常温固化灌封材料具有以下有益效果：性能如下，比热容(J/(g·K))≥1.5；相变焓(J/g)约30～180，即吸热值；相变温度(℃)5～90；比重(g/cc)：0.8～1.8表干时间：5min～25min；固化时间：1h～2h；完全固化时间≥24h。采用上述配方的单组分常温固化灌封材料具备了优异的吸热和控温性能，可以有效地将电子灌封胶内电子设备控制在合适的温度内，不会发生过热的情况。
附图说明
为了更清楚地说明本申请实施例的技术方案，下面将对实施例中所需要使用的附图作简单地介绍，应当理解，以下附图仅示出了本申请的某些实施例，因此不应被看作是对范围的限定，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他相关的附图。
图1为本发明实施例中单组分常温固化灌封材料的制备方法的流程示意图。
具体实施方式
下面结合实施例对本发明作进一步的说明，这是本发明的较佳实施例。
关于单组分常温固化灌封材料的分类
电子灌封胶用于对各种场景、形状的电子设备进行包裹封胶，因此，电子灌封胶在未固化前是液体的。在实际应用中，为了便于对电子设备进行封胶，降低对封胶环境的要求，灌封胶材料是可以制备成在常温下固化的。
在本发明实施例中，单组分常温固化灌封材料可以分为湿气固化灌封材料和温感固化灌封材料。
湿气固化灌封材料
湿气固化灌封材料，即在暴露在空气中时，接触到空气中的水蒸气时，会发生固化反应。
湿气固化灌封材料包括以下物质的混合物：载体介质和相变物质。
其中，载体介质为黏合及承载相变物质的物质。
其中，相变物质为吸附了相变粉体后的物质，相变粉体为通过转变物理形态吸收或释放热量的粉体材料。
其中，每100份重量的所述混合物中有20至60份所述载体介质存在；
其中，每100份重量的所述混合物中有40至80份所述相变物质存在；
所述载体介质包括：湿气固化树脂和湿气固化剂；湿气固化剂为使得所述湿气固化树脂固化的化学添加剂。具体的，在实际应用中不同的湿气固化树脂和湿气固化剂间的组合，以及相关材料的配比范围，将在以下实施例1至10中详细描述。
所述相变物质包括：相变粉体和吸附载体，所述吸附载体为石墨或气凝胶。
示例性的，所述相变粉体选自以下材料的至少一种：烷烃蜡、石蜡、脂肪酸、PE蜡和PP蜡，所述烷烃蜡的烷烃碳原子数介于10-60之间。
示例性的，根据实际应用中，对灌封材料的硬度、韧性、可塑性、吸热量、比热容、体积以及材料成本的需求，每100份重量的所述载体介质中有50至83.3份所述湿气固化树脂存在，每100份重量的所述载体介质中有16.7至50份所述湿气固化剂存在，具体此处不做限定。
温感固化灌封材料
温感固化灌封材料，即感应到温度在常温环境(20至40摄氏度)的情况下，会发生固化反应。因此，本发明实施例中的温感固化灌封材料需要冷藏存储及运输。
温感固化灌封材料，包括以下物质的混合物：载体介质和相变物质；
其中，每100份重量的所述混合物中有20至60份所述载体介质存在；
其中，每100份重量的所述混合物中有40至80份所述相变物质存在；
所述载体介质包括：温感固化树脂和温感固化剂；温感固化剂为使得所述温感固化树脂固化的化学添加剂。具体的，在实际应用中不同的温感固化树脂和温感固化剂间的组合，以及相关材料的配比范围，将在以下实施例11至15中详细描述。
所述相变物质包括：微胶囊化相变粉体，或相变粉体和吸附载体的混合粉体，所述吸附载体为石墨或气凝胶。
示例性的，所述相变粉体选自以下材料的至少一种：烷烃蜡、石蜡、脂肪酸、PE蜡和PP蜡，所述烷烃蜡的烷烃碳原子数介于10-60之间。
示例性的，根据实际应用中，对灌封材料的硬度、韧性、可塑性、吸热量、比热容、体积以及材料成本的需求，每100份重量的所述载体介质中有62.5至90份所述温感固化树脂存在；每100份重量的所述载体介质中有10至37.5份所述温感固化剂存在，具体此处不做限定。
关于导热填料
由于本发明实施例中单组分常温固化灌封材料的主要功能是用于吸收电子设备的热量，因此，灌封材料需要有良好的导热性能。本发明实施例通过在 单组分常温固化灌封材料中添加导热填料使其具备良好导热性能。
所述导热填料可以包括以下至少一种材料的组合：氧化铝、氮化铝、氮化硼、氧化镁、氧化锌、碳化硅、石墨粉和碳纳米管。
示例性的，根据实际应用中，对灌封材料的硬度、韧性、可塑性、吸热量、比热容、体积以及材料成本的需求，每100份重量的所述单组分常温固化灌封材料中有1至70份所述导热填料存在，具体此处不做限定。
需要说明的是，无论是湿气固化灌封材料的实施例，还是温感固化灌封材料的实施例，都可以添加导热填料以增强灌封材料的导热性能。
关于催化剂
在实际应用中，单组分常温固化灌封材料需要通过催化材料来满足或强化灌封材料的固化效果。但是，在某些实施例中，某些固化剂就具有了催化的效果(即固化剂同时充当了固化材料和催化材料的角色)，因此，催化剂并不是本发明实施例中的必备添加材料，以下仅对催化剂进行示例性说明，具体是否添加，添加哪些类型，添加多少，都需要根据实际需求而定，此处具体不做限定。
示例性的，所述催化剂可以为二丁基二月桂酸锡、辛酸亚锡和1，3-亚苯基二氧基双(乙酰乙酸乙酯)钛中的任意一种。
关于吸附载体
在实际对相变粉体的使用中，相变粉体从固态转变为液体后，有可能会在灌封材料中渗漏出来，因此，需要通过吸附载体将相变粉体进行吸附包裹，防止相变粉体的溢出。
在本申请实施例中，可以选用蠕虫状膨胀石墨作为吸附材料，蠕虫状膨胀 石墨由天然鳞片石墨经插层、水洗、干燥、高温膨化得到的一种疏松多孔的蠕虫状物质，膨胀石墨除了具备天然石墨本身的耐冷热、耐腐蚀、自润滑、耐辐射、导电性等优良性能以外，还具有天然石墨所没有的柔软、压缩回弹性、吸附性、生态环境协调性、生物相容性、耐辐射性等特性，由于疏松多孔，比表面积大，因此对相变粉体的吸附能力非常强，只需要采用较少重量份的蠕虫状膨胀石墨就可以完成对相变物质的吸附，当然，蠕虫状膨胀石墨不能太少，太少无法完全吸附住相变物质；蠕虫状膨胀石墨也不能太多，太多的话一方面增加成本和降低产品的热焓值，同时，降低了石墨吸附相变储能粉体相变焓，降低了产品的储热性能，因此，针对不同的粉体，恰好能够完全吸附完相变粉体的重量比是最优的。
示例性的，若所述吸附载体为石墨，则所述石墨为蠕虫状膨胀石墨；每100份重量的所述相变物质中有99至99.5份所述相变粉体存在；每100份重量的所述相变物质中有0.5至1份所述蠕虫状膨胀石墨存在；所述蠕虫状膨胀石墨的膨胀率为100-600ml/g，粒度为100-200目，膨胀倍数为200-600倍，堆积密度为0.2～0.5g/cm 3。
在本申请实施例中，也可以选用气凝胶作为吸附材料，气凝胶导热系数低，保温隔热效果好，理化性质稳定，高温不燃，完全防水，且无毒害，绿色环保，且比表面积大，对相变粉体的吸附能力非常强，只需要采用较少重量份的气凝胶就可以完成对相变物质的吸附，当然，气凝胶不能太少，太少无法完全吸附住相变物质；气凝胶也不能太多，太多的话一方面增加成本和产品的重量，同时，降低了气凝胶吸附相变储能粉体的相变焓，降低了产品的储热性能，因此，针对不同的相变粉体，恰好能够完全吸附完相变粉体的重量比是最优的。
示例性的，若所述吸附载体为气凝胶，则每100份重量的所述相变物质中有50至90份所述相变粉体存在；每100份重量的所述相变物质中有10至50份所述气凝胶存在；所述气凝胶的比表面积为100-300m 2/g，粒径为5-60nm。
关于制备方法
请参阅图1，本发明实施例中单组分常温固化灌封材料的制备方法，包括：
101、制备相变物质；
将相变粉体加热至熔化，将吸附载体分批加入至熔化后的相变粉体中搅拌，所述吸附载体添加完成后，将制备环境抽真空，真空度介于-0.04至-0.10MPa，抽真空的时间持续5-40min，搅拌时间为15-90min；在真空状态搅拌完成后，将相变粉体和吸附载体的混合材料分别进行冷却、粉碎以及过筛的步骤，得到所述相变物质。
示例性的，相变粉体的加热设备可以为反应釜，并且上述冷却的步骤可以冷却至常温，过筛的设备可以为10～100目筛的设备。
102、混合树脂和所述相变物质，得到混合基料；
将所述温感固化树脂(或湿气固化树脂)和所述相变物质置于真空捏合机内搅拌0.5～2小时，得到混合基料；所述真空捏合机内的温度为80～150℃，真空度为介于-0.04至-0.10Mpa。
103、搅拌混合基料和固化剂置等材料，得到单组分常温固化灌封材料。
将所述混合基料，所述温感固化剂(或湿气固化剂)置于搅拌机内进行搅拌均匀，得到所述单组分常温固化灌封材料；搅拌条件包括：转速30转/分钟，真空度介于-0.04至-0.10MPa，搅拌时间0.5～1.5小时。
可以理解的是，湿气固化灌封材料和温感固化灌封材料的制备方法相似， 此处不展开描述。
为了进一步减少吸附载体(蠕虫状膨胀石墨或气凝胶)的使用量，在相变物质制备过程中，采用了真空吸附的工艺，在真空条件下搅拌，熔化的相变粉体更容易深入地渗透到蠕虫状膨胀石墨蓬松的深孔内，深孔内对相变物质的吸附作用远远大于常规的浸渍或者搅拌，相变物质进入深孔内之后，在高温条件下也难以溢出，具有超常的吸附性能，如此，尽量少的蠕虫状膨胀石墨吸附了更多的相变物质，石墨吸附相变储能粉体的相变焓增加了5％-10％，性能得到了大幅提升，由于减少了蠕虫状膨胀石墨的用量，成本也大幅降低。
实施例1
单组分常温固化灌封材料，包括以下重量份的各组分：异氰酸酯预聚体树脂40份、多元醇19.9份、二丁基二月桂酸锡0.1份和相变物质40份，其中，其中，所述多元醇包括：聚醚多元醇、或聚酯多元醇；所述相变物质以石墨作为吸附载体，包括以下重量份的各组分：石蜡100份和蠕虫状膨胀石墨5份，所述蠕虫状膨胀石墨的膨胀率为500ml/g，粒度为100目，膨胀倍数为400倍，堆积密度为0.2g/cm 3。
实施例2
单组分常温固化灌封材料，包括以下重量份的各组分：异氰酸酯预聚体树脂13.29份、多元醇6.7份、二丁基二月桂酸锡0.1和相变物质80份，所述多元醇包括：聚醚多元醇、或聚酯多元醇；所述相变物质以石墨作为吸附载体，包括以下重量份的各组分：石蜡100份和蠕虫状膨胀石墨9份，所述蠕虫状膨 胀石墨的膨胀率为600ml/g，粒度为200目，膨胀倍数为600倍，堆积密度为0.5g/cm 3。
实施例3
单组分常温固化灌封材料，包括以下重量份的各组分：异氰酸酯预聚体树脂49.9份、多元醇10份、辛酸亚锡0.1份和相变物质40份，所述多元醇包括：聚醚多元醇、或聚酯多元醇；所述相变物质以石墨作为吸附载体，包括以下重量份的各组分：脂肪酸100份和蠕虫状膨胀石墨6份，所述蠕虫状膨胀石墨的膨胀率为100ml/g，粒度为150目，膨胀倍数为500倍，堆积密度为0.3g/cm 3。
实施例4
单组分常温固化灌封材料，包括以下重量份的各组分：异氰酸酯预聚体树脂29.7份、多元醇10份、1，3-亚苯基二氧基双(乙酰乙酸乙酯)钛0.3份和相变物质60份，所述多元醇包括：聚醚多元醇、或聚酯多元醇；所述相变物质以石墨作为吸附载体，包括以下重量份的各组分：PE蜡100份和蠕虫状膨胀石墨7份，所述蠕虫状膨胀石墨的膨胀率为520ml/g，粒度为120目，膨胀倍数为450倍，堆积密度为0.2g/cm 3。
实施例5
单组分常温固化灌封材料，包括以下重量份的各组分：多元醇预聚体树脂25份、异氰酸酯24.9份、二丁基二月桂酸锡0.1份和相变物质50份，所述异氰酸酯包括：多异氰酸酯PAPI、二苯基甲烷二异氰酸酯MDI、甲苯二异氰酸酯TDI中的至少一种，所述相变物质以石墨作为吸附载体，包括以下重量份的各组分：PP蜡100份和蠕虫状膨胀石墨8份，所述蠕虫状膨胀石墨的膨胀率为550ml/g，粒度为140目，膨胀倍数为460倍，堆积密度为0.2g/cm 3。
实施例6
单组分常温固化灌封材料，包括以下重量份的各组分：多元醇预聚体树脂25份、异氰酸酯5.5份、二丁基二月桂酸锡0.1份和相变物质40份，多异氰酸酯PAPI、MDI、TDI中的至少一种，所述相变物质以石墨作为吸附载体，包括以下重量份的各组分：C40烷烃蜡100份和蠕虫状膨胀石墨8.5份，所述蠕虫状膨胀石墨的膨胀率为570ml/g，粒度为200目，膨胀倍数为600倍，堆积密度为0.3g/cm 3。
实施例7
单组分常温固化灌封材料，包括以下重量份的各组分：多元醇预聚体树脂50份、异氰酸酯9.9份、二丁基二月桂酸锡0.1份和相变物质40份，多异氰酸酯PAPI、MDI、TDI中的至少一种，所述相变物质以石墨作为吸附载体，包括以下重量份的各组分：C30烷烃蜡100份和蠕虫状膨胀石墨8.8份，所述蠕虫状膨胀石墨的膨胀率为500ml/g，粒度为100目，膨胀倍数为400倍，堆积密度为0.4g/cm 3。
实施例8
单组分常温固化灌封材料，包括以下重量份的各组分：多元醇预聚体树脂30份、异氰酸酯9份、二丁基二月桂酸锡1份和相变物质60份，多异氰酸酯PAPI、MDI、TDI中的至少一种，所述相变物质以石墨作为吸附载体，包括以下重量份的各组分：C20烷烃蜡100份和蠕虫状膨胀石墨7.3份，所述蠕虫状膨胀石墨的膨胀率为600ml/g，粒度为200目，膨胀倍数为600倍，堆积密 度为0.2g/cm 3。
实施例9
单组分常温固化灌封材料，包括以下重量份的各组分：多元醇预聚体树脂20份、异氰酸酯9.7份、二丁基二月桂酸锡0.3份和相变物质70份，多异氰酸酯PAPI、MDI、TDI中的至少一种，所述相变物质以气凝胶作为吸附载体，包括以下重量份的各组分：C30烷烃蜡100份和气凝胶45份，所述气凝胶的比表面积为260m 2/g，粒径为12nm。
实施例10
单组分常温固化灌封材料，包括以下重量份的各组分：多元醇预聚体树脂20份、异氰酸酯14.5份、二丁基二月桂酸锡0.5份和相变物质65份，多异氰酸酯PAPI、MDI、TDI中的至少一种，所述相变物质以气凝胶作为吸附载体，包括以下重量份的各组分：C10烷烃蜡100份和气凝胶50份，所述气凝胶的比表面积300m 2/g，粒径为5nm。
实施例11
单组分常温固化灌封材料，包括以下重量份的各组分：环氧树脂40份、咪唑类固化剂19.9份、二丁基二月桂酸锡0.1份和相变物质40份，其中，所述环氧树脂包括：双酚A型环氧树脂、改性环氧树脂、双酚S型环氧树脂、双酚F型环氧树脂、环氧化环氧树脂；所述相变物质以石墨作为吸附载体，包括以下重量份的各组分：C20烷烃蜡100份和蠕虫状膨胀石墨7.3份，所述蠕虫状膨胀石墨的膨胀率为600ml/g，粒度为200目，膨胀倍数为600倍，堆积 密度为0.2g/cm 3。
实施例12
单组分常温固化灌封材料，包括以下重量份的各组分：环氧树脂13.29份、咪唑类固化剂6.7份、二丁基二月桂酸锡0.1份和相变物质80份，其中，所述环氧树脂包括：双酚A型环氧树脂、改性环氧树脂、双酚S型环氧树脂、双酚F型环氧树脂、环氧化环氧树脂；所述相变物质以石墨作为吸附载体，包括以下重量份的各组分：C30烷烃蜡100份和蠕虫状膨胀石墨8.8份，所述蠕虫状膨胀石墨的膨胀率为500ml/g，粒度为100目，膨胀倍数为400倍，堆积密度为0.4g/cm 3。
实施例13
单组分常温固化灌封材料，包括以下重量份的各组分：环氧树脂49.9份、多元醇10份、二丁基二月桂酸锡0.1份和相变物质40份，其中，所述环氧树脂包括：双酚A型环氧树脂、改性环氧树脂、双酚S型环氧树脂、双酚F型环氧树脂、环氧化环氧树脂；所述相变物质以石墨作为吸附载体，包括以下重量份的各组分：C40烷烃蜡100份和蠕虫状膨胀石墨8.5份，所述蠕虫状膨胀石墨的膨胀率为570ml/g，粒度为200目，膨胀倍数为600倍，堆积密度为0.3g/cm 3。
实施例14
单组分常温固化灌封材料，包括以下重量份的各组分：环氧树脂29.8份、多元醇10份、二丁基二月桂酸锡0.2份和相变物质60份，其中，所述环氧树 脂包括：双酚A型环氧树脂、改性环氧树脂、双酚S型环氧树脂、双酚F型环氧树脂、环氧化环氧树脂；所述相变物质以气凝胶作为吸附载体，包括以下重量份的各组分：C20烷烃蜡100份和气凝胶40份，所述气凝胶的比表面积为220m 2/g，粒径为15nm。
实施例15
单组分常温固化灌封材料，包括以下重量份的各组分：环氧树脂25份、甲基三乙氧基硅烷24.9份、二丁基二月桂酸锡0.1份和相变物质10份，其中，所述环氧树脂包括：双酚A型环氧树脂、改性环氧树脂、双酚S型环氧树脂、双酚F型环氧树脂、环氧化环氧树脂；所述相变物质以气凝胶作为吸附载体，包括以下重量份的各组分：C30烷烃蜡100份和气凝胶45份，所述气凝胶的比表面积为260m 2/g，粒径为12nm。
以上所述实施例的各技术特征可以进行任意的组合，为使描述简洁，未对上述实施例中的各个技术特征所有可能的组合都进行描述，然而，只要这些技术特征的组合不存在矛盾，都应当认为是本说明书记载的范围。
最后应当说明的是，以上实施例仅用以说明本发明的技术方案，而非对本发明保护范围的限制，尽管参照较佳实施例对本发明作了详细地说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的实质和范围。

Claims (10)

  1. 一种单组分常温固化灌封材料，其特征在于，包括以下物质的混合物：载体介质和相变物质；
    其中，每100份重量的所述混合物中有20至60份所述载体介质存在；
    其中，每100份重量的所述混合物中有40至80份所述相变物质存在；
    所述载体介质包括：湿气固化树脂和湿气固化剂；
    所述相变物质包括：微胶囊化相变粉体，或相变粉体和吸附载体的混合粉体，所述吸附载体为石墨或气凝胶。
  2. 根据权利要求1所述的单组分常温固化灌封材料，其特征在于：
    每100份重量的所述载体介质中有50至83.3份所述湿气固化树脂存在；
    每100份重量的所述载体介质中有16.7至50份所述湿气固化剂存在；
    所述湿气固化树脂和湿气固化剂的组合包括以下任一种：
    异氰酸酯预聚体树脂和多元醇；其中，所述多元醇包括：聚醚多元醇、或聚酯多元醇；
    多元醇预聚体树脂和异氰酸酯；其中，所述异氰酸酯包括：多异氰酸酯PAPI、二苯基甲烷二异氰酸酯MDI、甲苯二异氰酸酯TDI中的至少一种；
    若所述湿气固化树脂和湿气固化剂的组合为异氰酸酯预聚体树脂和多元醇，则每100份重量的所述载体介质中有66.7至83.3份所述异氰酸酯预聚体树脂存在；每100份重量的所述载体介质中有16.7至33.3份所述多元醇存在；
    若所述湿气固化树脂和湿气固化剂的组合为多元醇预聚体树脂和异氰酸酯，则每100份重量的所述载体介质中有50至83.3份所述多元醇预聚体树脂存；每100份重量的所述载体介质中有16.7至50份所述异氰酸酯存在。
  3. 根据权利要求1所述的单组分常温固化灌封材料，其特征在于，所述单组分常温固化灌封材料，还包括：导热填料；
    所述导热填料包括以下至少一种材料的组合：氧化铝、氮化铝、氮化硼、氧化镁、氧化锌、碳化硅、石墨粉和碳纳米管；每100份重量的所述单组分常温固化灌封材料中有1至70份所述导热填料存在。
  4. 根据权利要求1所述的单组分常温固化灌封材料，其特征在于，
    若所述吸附载体为石墨，则所述石墨为蠕虫状膨胀石墨；每100份重量的所述相变物质中有99至99.5份所述相变粉体存在；每100份重量的所述相变物质中有0.5至1份所述蠕虫状膨胀石墨存在；
    所述蠕虫状膨胀石墨的膨胀率为100-600ml/g，粒度为100-200目，膨胀倍数为200-600倍，堆积密度为0.2～0.5g/cm 3；
    若所述吸附载体为气凝胶，则每100份重量的所述相变物质中有50至90份所述相变粉体存在；每100份重量的所述相变物质中有10至50份所述气凝胶存在；
    所述气凝胶的比表面积为100-300㎡/g，粒径为5-60nm。
  5. 根据权利要求1至4任一项所述的单组分常温固化灌封材料，其特征在于，所述相变粉体选自以下材料的至少一种：烷烃蜡、石蜡、脂肪酸、PE蜡和PP蜡，所述烷烃蜡的烷烃碳原子数介于10-60之间。
  6. 一种单组分常温固化灌封材料，其特征在于，包括以下物质的混合物：载体介质和相变物质；
    其中，每100份重量的所述混合物中有20至60份所述载体介质存在；
    其中，每100份重量的所述混合物中有40至80份所述相变物质存在；
    所述载体介质包括：温感固化树脂和温感固化剂；
    所述相变物质包括：相变粉体和吸附载体，所述吸附载体为石墨或气凝胶。
  7. 根据权利要求6所述的单组分常温固化灌封材料，其特征在于：
    每100份重量的所述载体介质中有62.5至90份所述温感固化树脂存在；
    每100份重量的所述载体介质中有10至37.5份所述温感固化剂存在；
    所述温感固化树脂和温感固化剂的组合包括以下任一种：
    环氧树脂和咪唑类固化剂；其中，所述环氧树脂包括：双酚A型环氧树脂、改性环氧树脂、双酚S型环氧树脂、双酚F型环氧树脂、环氧化环氧树脂；
    环氧树脂和胺肼类固化剂；其中，所述环氧树脂包括：双酚A型环氧树脂、改性环氧树脂、双酚S型环氧树脂、双酚F型环氧树脂、环氧化环氧树脂。
  8. 根据权利要求6所述的单组分常温固化灌封材料，其特征在于，所述单组分常温固化灌封材料，还包括：导热填料；
    所述导热填料包括以下至少一种材料的组合：氧化铝、氮化铝、氮化硼、氧化镁、氧化锌、碳化硅、石墨粉和碳纳米管；
    每100份重量的所述单组分常温固化灌封材料中有1至70份所述导热填料存在。
  9. 根据权利要求6所述的单组分常温固化灌封材料，其特征在于，
    若所述吸附载体为石墨，则所述石墨为蠕虫状膨胀石墨；每100份重量的所述相变物质中有99至99.5份所述相变粉体存在；每100份重量的所述相变物质中有0.5至1份所述蠕虫状膨胀石墨存在；
    所述蠕虫状膨胀石墨的膨胀率为100-600ml/g，粒度为100-200目，膨胀倍数为200-600倍，堆积密度为0.2～0.5g/cm 3；
    若所述吸附载体为气凝胶，则每100份重量的所述相变物质中有50至90份所述相变粉体存在；每100份重量的所述相变物质中有10至50份所述气凝胶存在；
    所述气凝胶的比表面积为100-300㎡/g，粒径为5-60nm。
  10. 根据权利要求6至9任一项所述的单组分常温固化灌封材料，其特征在于，所述相变粉体选自以下材料的至少一种：烷烃蜡、石蜡、脂肪酸、PE蜡和PP蜡，所述烷烃蜡的烷烃碳原子数介于10-60之间。
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* Cited by examiner, † Cited by third party
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WO2003050155A1 (de) * 2001-12-13 2003-06-19 Henkel Kommanditgesellschaft Auf Aktien Schneller, aktivierbarer polyurethanklebstoff
CN107815286A (zh) * 2017-11-03 2018-03-20 航天特种材料及工艺技术研究所 一种基于相变微胶囊的导热灌封硅胶及其制备方法
CN109722215A (zh) * 2017-10-27 2019-05-07 宁德时代新能源科技股份有限公司 一种吸热灌封胶及其电池
WO2019102383A1 (en) * 2017-11-22 2019-05-31 Scg Chemicals Co., Ltd. Low-void polyurethanes
CN110408157A (zh) * 2019-08-26 2019-11-05 张立强 双组份储热灌封材料及其制备方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003050155A1 (de) * 2001-12-13 2003-06-19 Henkel Kommanditgesellschaft Auf Aktien Schneller, aktivierbarer polyurethanklebstoff
CN109722215A (zh) * 2017-10-27 2019-05-07 宁德时代新能源科技股份有限公司 一种吸热灌封胶及其电池
CN107815286A (zh) * 2017-11-03 2018-03-20 航天特种材料及工艺技术研究所 一种基于相变微胶囊的导热灌封硅胶及其制备方法
WO2019102383A1 (en) * 2017-11-22 2019-05-31 Scg Chemicals Co., Ltd. Low-void polyurethanes
CN110408157A (zh) * 2019-08-26 2019-11-05 张立强 双组份储热灌封材料及其制备方法

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