CN111533486A - Graphene modified resin packaging material and preparation method thereof - Google Patents
Graphene modified resin packaging material and preparation method thereof Download PDFInfo
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- CN111533486A CN111533486A CN202010288878.5A CN202010288878A CN111533486A CN 111533486 A CN111533486 A CN 111533486A CN 202010288878 A CN202010288878 A CN 202010288878A CN 111533486 A CN111533486 A CN 111533486A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
- C04B26/10—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B26/14—Polyepoxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/005—Impregnating or encapsulating
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/04—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing coils
- H01F41/12—Insulating of windings
- H01F41/127—Encapsulating or impregnating
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00844—Uses not provided for elsewhere in C04B2111/00 for electronic applications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/90—Electrical properties
- C04B2111/92—Electrically insulating materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
Abstract
The invention relates to a graphene modified resin packaging material and a preparation method thereof. The graphene modified resin packaging material is formed by combining a component A and a component B according to the mass ratio of 1: 0.9-1.4; wherein, the component A comprises: 18-25 parts of bisphenol A epoxy resin, 0.5-2 parts of toughening agent, 1-10 parts of graphene resin dispersion liquid and 48-52 parts of silicon micro powder; the component B comprises: 15-25 parts of curing agent, 0.05-0.15 part of accelerator and 1-5 parts of toughening agent. According to the graphene modified resin packaging material and the preparation method thereof, the graphene modified resin packaging material meets the electrical performance and has a good heat dissipation effect through the graphene pre-dispersion treatment, the controllable number and sheet diameter of the graphene layers and the components, the formula and the preparation method of the graphene modified resin packaging material of the dry-type transformer.
Description
Technical Field
The invention belongs to the technical field of resin materials, and particularly relates to a graphene modified resin packaging material and a preparation method thereof.
Background
The dry type transformer mainly comprises 4 components, namely an iron core, a high-voltage coil, a low-voltage coil and an epoxy resin packaging part, wherein the commonly used packaging layer is mainly made of epoxy resin, the epoxy resin is a widely used chemical raw material, has flame retardancy, flame retardance and excellent electrical performance, and has higher insulating strength than air and transformer oil, and the cast transformer coil has high mechanical strength and excellent moisture-proof and dust-proof performance, is widely applied to urban power grids, and particularly is applied to places with high requirements on fire prevention and safety.
At present, when a dry-type transformer operates, copper loss and iron loss are generated on a coil winding and an iron core, and the loss is converted into heat energy, so that the temperature of the iron core and the coil winding of the transformer is increased. If the temperature exceeds the allowable value for a long time, the mechanical elasticity of the insulation is lost and the insulation is deteriorated. Particularly, in the resin insulation dry type transformer, the high-voltage coil winding is poured in the epoxy resin insulation cylinder, and the heat conductivity of the insulation materials such as epoxy resin is low, so that the heat dissipation effect of the insulation cylinder is poor, the temperature of the coil winding is the highest, and the safety of the long-term continuous operation of the transformer under the rated capacity is threatened.
In industrial applications, it is common to add catalysts, diluents, tougheners, various fillers, and the like to epoxy resins to improve one or more of their properties. Fillers traditionally used to improve the electrical insulating properties of epoxy resins are mostly micron-sized inorganic oxides such as: micron-sized fillers such as phyllosilicate, aluminum trioxide, magnesium oxide, silicon dioxide and the like. In general, the micron filler needs to be added at a higher amount (mass fraction is more than 50%) to obviously improve the breakdown performance of the material. However, too high an amount of filler added leads to an increase in weight of the insulating material, which is not favorable for the progress toward weight reduction. High amounts of fillers also increase the brittleness of the polymer material and deteriorate the mechanical properties.
Prior art CN104119644A, provides an encapsulation material for a transformer, which comprises a graphene oxide-silica modified epoxy resin, a cross-linking agent, a toughening agent, a filler and an accelerator. The packaging material has good performance, can ensure that the integrity of the packaging part is not reduced, and prolongs the service life of the dry-type transformer. However, the invention adopts graphene oxide-silicon dioxide to modify epoxy resin; the dry-type transformer is prepared by adopting a vacuum casting method, although the method for preparing the modified epoxy resin is provided, the prepared epoxy resin system has low viscosity, high toughness, small heat release and excellent insulating property and electricity-saving property, the invention has no outstanding heat radiation performance and influences the service life of the material.
The prior art CN110184009A discloses a preparation method of an epoxy resin-based heat-conducting insulating adhesive, belonging to the technical field of high polymer materials. Weighing the following components in parts by weight: 60-80 parts of epoxy resin, 30-40 parts of diluent, 5-8 parts of silane coupling agent KH-550, 10-20 parts of additive and 10-12 parts of curing agent, mixing the epoxy resin and the diluent in a stirrer, adding the additive and the silane coupling agent into the stirrer, stirring and mixing for 30-50 min at the temperature of 30-50 ℃ and the rotating speed of 300-400 r/min to obtain a mixed blank, mixing the mixed blank with the curing agent, stirring and mixing for 20-50 min at the temperature of 30-60 ℃ and the rotating speed of 300-350 r/min, heating and curing for 30-60 min at the temperature of 150-180 ℃ to obtain the epoxy resin-based heat-conducting insulating adhesive. However, the additive is added when the epoxy resin-based heat-conducting insulating adhesive is prepared, firstly, the additive contains graphene oxide, and after the graphene oxide is added into a product, the heat-conducting property of the product cannot be improved, secondly, the surface of the graphene oxide microsphere is wrinkled after the graphene oxide in the additive is modified, and after subsequent treatment, a coating layer of polyethyleneimine is adsorbed on the surface of the wrinkled graphene oxide microsphere, so that the situation that a conductive path cannot be formed in the preparation process of the product by the wrinkled graphene oxide microsphere cannot be ensured, and the insulativity of the product is further influenced. And the mechanical property of the modified resin castable cannot be characterized.
Prior art CN103374207B provides an epoxy composite material and a method for preparing the same, the method comprises: (1) stirring and mixing a trace amount of conductive nano filler and a part of epoxy resin, and grinding a mixture obtained after stirring and mixing to obtain a master batch; (2) mixing the master batch obtained in the step (1), the other part of epoxy resin and a curing agent, and then removing bubbles; (3) solidifying and forming the material obtained after removing the bubbles; wherein the stirring and mixing conditions in the step (1) are such that the dynamic viscosity of the mixture obtained after stirring and mixing is 5-18pa.s at 60 ℃. The epoxy composite material film prepared by the method has high breakdown strength and good electricity-saving performance. However, the invention can uniformly disperse the conductive nano filler in the epoxy resin by controlling the stirring and mixing conditions of the conductive nano filler and the epoxy resin, and although the breakdown strength and the dielectric property can be improved, the bending strength and the heat dissipation performance of the epoxy resin cannot be ensured, and particularly, expensive additives or auxiliary agents are used in the preparation process, so that the preparation method has no industrial advantages.
In view of the above, the present invention provides a novel resin encapsulation material, which has good heat dissipation effect while satisfying electrical performance.
Disclosure of Invention
The invention aims to provide a graphene modified resin packaging material, which can not form conductive network connection in the material to play an insulating role by controlling the content of multilayer graphene in epoxy resin, and can greatly improve the heat dissipation performance and strength of the graphene modified resin packaging material by utilizing the structural strength and heat dissipation performance of graphene.
In order to realize the purpose, the adopted technical scheme is as follows:
the graphene modified resin packaging material is formed by combining a component A and a component B according to the mass ratio of 1: 0.9-1.4;
wherein, the component A comprises: 18-25 parts of bisphenol A epoxy resin, 0.5-2 parts of toughening agent, 1-10 parts of graphene resin dispersion liquid and 48-52 parts of silicon micro powder;
the component B comprises: 15-25 parts of curing agent, 0.05-0.15 part of accelerator and 1-5 parts of toughening agent.
Further, the bisphenol A type epoxy resin is E-51 type, or E-44 type, or a mixture of E-51 type and E-44 type;
the toughening agent is a DT series toughening agent;
the grain diameter of the silicon micro powder is less than 600 meshes;
the curing agent is an anhydride curing agent;
the accelerator is at least one of dimethylaminopropylamine, dimethylbenzylamine and dimethyl phthalate.
Further, the graphene resin dispersion liquid is composed of 75-85 parts by weight of epoxy resin, 1-5 parts by weight of dispersant and 15-25 parts by weight of graphene powder.
Still further, the size of the graphene sheet diameter in the graphene resin dispersion liquid is 1-10 μm.
Further, the graphene powder has an oxygen content of 8-12% and a number of layers within 10.
Further, the resin in the graphene resin dispersion liquid is E-51 type bisphenol A epoxy resin;
the dispersing agent in the graphene resin dispersion liquid is acetone.
Another object of the present invention is to provide a method for preparing the graphene modified resin packaging material, wherein a pre-dispersion method is adopted, a graphene three-dimensional new material is added into an epoxy resin packaging material to prepare the graphene modified resin packaging material, and meanwhile, the heat dissipation performance and strength of the graphene modified resin packaging material are greatly improved by utilizing the structural strength and heat dissipation performance of graphene.
In order to realize the purpose, the adopted technical scheme is as follows:
the preparation method of the graphene modified resin packaging material comprises the following steps:
s10 preparation of graphene resin dispersion liquid:
heating and dehumidifying graphene powder, mixing with epoxy resin and a dispersing agent, stirring at a high speed, and grinding to obtain a stable graphene resin dispersion liquid;
s20 preparation of component A:
sequentially adding bisphenol A type epoxy resin, a toughening agent and silicon micropowder into the graphene resin dispersion liquid, and uniformly mixing to obtain the component A;
s30, preparing the graphene modified resin packaging material:
and (2) sequentially adding a curing agent, an accelerator and a toughening agent into the component A, and stirring under a vacuum condition at 50-65 ℃ until no large amount of foam is generated to obtain the graphene modified resin packaging material.
Further, in the step S10, the temperature for heating and dehumidifying is 100 ℃, and the time is 2 hours;
in step S30, the vacuum degree is 20 mbar.
Further, the preparation method of the graphene powder comprises the following steps:
adding graphite into concentrated sulfuric acid in an ice water mixture, slowly adding potassium permanganate while stirring, controlling the reaction temperature to be less than 5 ℃, and preserving heat for 1-2 hours; slowly adding potassium ferrate under stirring, heating to 45 deg.C, and maintaining for 5-20 hr to obtain dark green liquid; wherein the graphite is crystalline flake graphite, microcrystalline graphite or expanded graphite; the mass-volume ratio of the graphite to the potassium permanganate to the potassium ferrate to the concentrated sulfuric acid is 10 g: 30g of: 0.1 g: 320 ml;
adding the dark green liquid into deionized water, and stirring and mixing uniformly; adding 30% hydrogen peroxide by mass and uniformly mixing to obtain a mixed solution; wherein the mass volume ratio of the graphite to the deionized water to the hydrogen peroxide is 10 g: 640 ml: 20ml of the solution;
washing the mixed solution by using a hydrochloric acid solution with the mass fraction of 5% and deionized water through a ceramic membrane filter in sequence, and repeating the washing process until the conductivity of the waste acid is reduced to be below 100us/cm, so as to obtain a graphene oxide feed liquid; wherein, the mixed solution is washed by 500ml of washing liquid in turn each time;
and carrying out centrifugal spray drying on the graphene oxide feed liquid, wherein the drying temperature is 120-280 ℃.
Still another object of the present invention is to provide a method for manufacturing a dry type transformer.
In order to realize the purpose, the adopted technical scheme is as follows:
a preparation method of a dry-type transformer adopts a vacuum casting method to prepare the dry-type transformer, and comprises the following steps:
s10, batching: a castable material is obtained by the preparation method of claim 7, namely the graphene modified resin packaging material; placing the casting material in a casting tank;
s20 pouring: after the wound coil is loaded into a casting mold, the casting tank is added and opened, the temperature is raised to 70-80 ℃, the casting tank is vacuumized for 2-4 times, then the casting material is added, and the feeding speed is controlled to be 0.5-1kg/min until the feeding is finished;
s10 curing and demolding: and heating and curing the cast mold in a curing furnace, keeping the curing temperature at 90-110 ℃ for 20-30min, discharging the coil out of the furnace after curing is finished, dismantling the mold, and slowly cooling to room temperature.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, graphene and epoxy resin are subjected to pre-dispersion treatment, a graphene three-dimensional new material is added into an epoxy resin packaging material in advance to prepare the graphene modified resin packaging material, and the heat dissipation performance and strength of the graphene modified resin packaging material are greatly improved by utilizing the three-dimensional structural strength and heat dissipation performance of the graphene.
2. According to the invention, a pre-dispersion method is adopted, graphene is soaked in resin, and then the graphene is added into dissolved epoxy resin (EP), so that the graphene nano-sized filler can be uniformly dispersed in the epoxy resin, and the finally prepared epoxy composite material is favorably cured and formed; in addition, by utilizing the excellent characteristics of rigidity, dimensional stability, thermal conductivity and the like of the graphene, the graphene serving as an EP modifier can remarkably improve the mechanical property and heat dissipation performance of the composite material, and overcomes the defects of large mixing amount of common inorganic fillers, low modification efficiency and the like.
3. According to the invention, the oxygen content of graphene is controlled, the graphene is uniformly dispersed in epoxy resin, and the number of layers and the sheet diameter of the graphene material are further controlled, so that the graphene material cannot form conductive network connection in the material, and the insulating effect is achieved, the insulating resistance of the graphene modified resin material is further improved, and the dielectric loss factor is reduced. Meanwhile, the heat dissipation performance and strength of the graphene modified resin packaging material are greatly improved by utilizing the self structural strength and heat dissipation performance of the graphene.
4. The graphene modified resin packaging material prepared by the invention can be suitable for dry-type transformer modified resin casting materials, and has good heat dissipation effect while meeting the electrical performance.
Detailed Description
In order to further illustrate the graphene modified resin packaging material and the preparation method thereof according to the present invention to achieve the intended purpose, the following detailed description is given to the graphene modified resin packaging material and the preparation method thereof according to the present invention, and the detailed implementation, structure, features and effects thereof will be described in detail. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
The graphene modified resin packaging material and the preparation method thereof according to the present invention will be further described in detail with reference to the following specific embodiments:
the technical scheme of the invention is as follows:
the graphene modified resin packaging material is formed by combining a component A and a component B according to the mass ratio of 1: 0.9-1.4;
wherein, the component A comprises: 18-25 parts of bisphenol A epoxy resin, 0.5-2 parts of toughening agent, 1-10 parts of graphene resin dispersion liquid and 48-52 parts of silicon micro powder;
the component B comprises: 15-25 parts of curing agent, 0.05-0.15 part of accelerator and 1-5 parts of toughening agent.
According to the invention, the components of the graphene modified resin packaging material are divided into the component A and the component B, so that the cross-linking density in the packaging resin can be improved, the capability of preventing moisture intrusion of the packaging resin can be improved, and the moisture absorption performance of the packaging resin can be reduced.
Preferably, the bisphenol A type epoxy resin is E-51 type, or E-44 type, or a mixture of E-51 type and E-44 type;
the toughening agent is a DT series toughening agent;
the grain diameter of the silicon micro powder is less than 600 meshes;
the curing agent is an anhydride curing agent;
the accelerator is at least one of dimethylaminopropylamine, dimethylbenzylamine and dimethyl phthalate.
Preferably, the graphene resin dispersion liquid consists of 75-85 parts by weight of epoxy resin, 1-5 parts by weight of dispersant and 15-25 parts by weight of graphene powder.
More preferably, the graphene sheet diameter in the graphene resin dispersion liquid is 1-10 μm.
More preferably, the graphene powder has an oxygen content of 8-12% and a number of layers of 10 or less.
According to the invention, the oxygen content of graphene is controlled, the graphene is uniformly dispersed in epoxy resin, and the number of layers and the sheet diameter of the graphene material are further controlled, so that the graphene material cannot form conductive network connection in the material, and the insulating effect is achieved, the insulating resistance of the graphene modified resin material is further improved, and the dielectric loss factor is reduced.
More preferably, the resin in the graphene resin dispersion liquid is E-51 type bisphenol A epoxy resin;
the dispersing agent in the graphene resin dispersion liquid is acetone.
The preparation method of the graphene modified resin packaging material comprises the following steps:
s10 preparation of graphene resin dispersion liquid:
heating and dehumidifying graphene powder, mixing with epoxy resin and a dispersing agent, stirring at a high speed, and grinding to obtain a stable graphene resin dispersion liquid;
s20 preparation of component A:
sequentially adding bisphenol A type epoxy resin, a toughening agent and silicon micropowder into the graphene resin dispersion liquid, and uniformly mixing to obtain the component A;
s30, preparing the graphene modified resin packaging material:
and (2) sequentially adding a curing agent, an accelerator and a toughening agent into the component A, and stirring under a vacuum condition at 50-65 ℃ until no large amount of foam is generated to obtain the graphene modified resin packaging material.
Preferably, in step S10, the temperature for heating and dehumidifying is 100 ℃ for 2 hours;
in step S30, the vacuum degree is 20 mbar.
Preferably, the preparation method of the graphene powder comprises the following steps:
adding graphite into concentrated sulfuric acid in an ice water mixture, slowly adding potassium permanganate while stirring, controlling the reaction temperature to be less than 5 ℃, and preserving heat for 1-2 hours; slowly adding potassium ferrate under stirring, heating to 45 deg.C, and maintaining for 5-20 hr to obtain dark green liquid; wherein the graphite is crystalline flake graphite, microcrystalline graphite or expanded graphite; the mass-volume ratio of the graphite to the potassium permanganate to the potassium ferrate to the concentrated sulfuric acid is 10 g: 30g of: 0.1 g: 320 ml;
adding the dark green liquid into deionized water, and stirring and mixing uniformly; adding 30% hydrogen peroxide by mass and uniformly mixing to obtain a mixed solution; wherein the mass volume ratio of the graphite to the deionized water to the hydrogen peroxide is 10 g: 640 ml: 20ml of the solution;
washing the mixed solution by using a hydrochloric acid solution with the mass fraction of 5% and deionized water through a ceramic membrane filter in sequence, and repeating the washing process until the conductivity of the waste acid is reduced to be below 100us/cm, so as to obtain a graphene oxide feed liquid; wherein, the mixed solution is washed by 500ml of washing liquid in turn each time;
and carrying out centrifugal spray drying on the graphene oxide feed liquid, wherein the drying temperature is 120-280 ℃.
According to the preparation method, the reaction time and the drying temperature of graphene preparation are controlled, the number of graphene layers and the oxygen content are further controlled, the graphene is soaked in resin in advance, then the graphene is added into dissolved epoxy resin (EP), a composite intermediate with the advantages of the graphene and the graphene is prepared through a multi-layer three-dimensional graphene/EP synergistic effect, the strength and the heat dissipation performance of the graphene three-dimensional structure are utilized, and the heat dissipation performance and the strength of the graphene modified resin packaging material are greatly improved. In addition, the number of layers, the oxygen content and the addition amount of the graphene material are controlled, so that the graphene material cannot form conductive network connection in the material, an insulating effect is achieved, the insulation resistance of the graphene modified resin material is further improved, and the dielectric loss factor is reduced.
A preparation method of a dry-type transformer adopts a vacuum casting method to prepare the dry-type transformer, and comprises the following steps:
s10, batching: obtaining a castable material, namely the graphene modified resin packaging material, by adopting the preparation method; placing the casting material in a casting tank;
s20 pouring: after the wound coil is loaded into a casting mold, the casting tank is added and opened, the temperature is raised to 70-80 ℃, the casting tank is vacuumized for 2-4 times, then the casting material is added, and the feeding speed is controlled to be 0.5-1kg/min until the feeding is finished;
s10 curing and demolding: and heating and curing the cast mold in a curing furnace, keeping the curing temperature at 90-110 ℃ for 20-30min, discharging the coil out of the furnace after curing is finished, dismantling the mold, and slowly cooling to room temperature.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Example 1.
The specific operation steps are as follows:
(1) preparing graphene powder:
in an ice-water mixture, 10g of flake graphite is added into 320mL of concentrated sulfuric acid, 30g of potassium permanganate is slowly added while stirring by an electric stirrer, the reaction temperature is controlled to be less than 5 ℃, and the temperature is kept for 2 hours.
Slowly adding 0.1g of potassium ferrate into the mixed solution under the stirring condition, heating to 45 ℃, and preserving the temperature for 5 hours to obtain dark green liquid.
Adding the obtained dark green liquid into 640ml of deionized water, stirring and mixing uniformly, and then adding 20ml of hydrogen peroxide with the mass fraction of 30%; and (3) sequentially adopting 500ml of 5% hydrochloric acid and deionized water for the mixed solution, washing by using a ceramic membrane filter, and repeating the washing process until the conductivity of the waste acid is reduced to be less than 100us/cm, so as to obtain the graphene oxide feed liquid.
And (3) carrying out centrifugal spray drying on the graphene oxide feed liquid at the drying temperature of 120 ℃, and finally obtaining graphene powder.
(2) Preparing a graphene resin dispersion liquid:
heating and dehumidifying 20 parts by weight of graphene powder at 100 ℃ for 2h, premixing with 80 parts by weight of epoxy resin and 2 parts by weight of dispersing agent, stirring at high speed for 35min, and grinding by using a three-roll mill to obtain a stable graphene resin dispersion liquid.
(3) Preparing a graphene modified resin packaging material:
adding 5 parts by weight of the prepared graphene resin dispersion liquid into a mixing tank, sequentially adding 20 parts by weight of E-51 type bisphenol A epoxy resin, 1 part by weight of DT series toughening agent and 49 parts by weight of silica powder with the particle size less than 600 meshes in the component A according to the proportion, and uniformly stirring the casting material by using a dispersion machine for about 20min to obtain the component A.
According to the mass ratio of the component A to the component B of 1: 1, sequentially adding an acid anhydride curing agent, a dimethylaminopropylamine accelerator and a DT-series toughener (the using amount of each raw material in the component B is 20 parts by weight of the acid anhydride curing agent, 0.1 part by weight of the dimethylaminopropylamine accelerator and 1 part by weight of the DT-series toughener), keeping the vacuum degree at 20mbar and the temperature at 50-65 ℃, uniformly stirring, and obtaining a casting material when no large amount of foam is generated and the temperature is kept at 50-65 ℃, namely the graphene modified resin packaging material.
(4) Preparing a dry-type transformer:
before pouring, the wound coil is loaded into a pouring mold, then the coil is transferred into a pouring tank, then the pouring tank is opened, the temperature is heated to 70-80 ℃, the vacuum pumping is carried out for 2-4 times, then the pouring material is added, and the feeding speed is controlled to be 0.5-1kg/min until the feeding is finished.
And heating and curing the poured mould in a curing furnace, keeping the curing temperature at 90-110 ℃, keeping for 20-30 minutes, discharging the coil out of the furnace after curing is finished, dismantling the mould at a higher speed, lifting the coil into the curing furnace, and slowly cooling to room temperature.
Example 2.
The specific operation steps are as follows:
(1) preparing graphene powder:
in an ice-water mixture, 10g of flake graphite is added into 320mL of concentrated sulfuric acid, 30g of potassium permanganate is slowly added while stirring by an electric stirrer, the reaction temperature is controlled to be less than 5 ℃, and the temperature is kept for 1 h.
Slowly adding 0.1g of potassium ferrate into the mixed solution under the stirring condition, heating to 45 ℃, and preserving the temperature for 10 hours to obtain dark green liquid.
Adding the obtained dark green liquid into 640ml of deionized water, stirring and mixing uniformly, and then adding 20ml of hydrogen peroxide with the mass fraction of 30%; and (3) sequentially adopting 500ml of 5% hydrochloric acid and deionized water for the mixed solution, washing by using a ceramic membrane filter, and repeating the washing process until the conductivity of the waste acid is reduced to be less than 100us/cm, so as to obtain the graphene oxide feed liquid.
And (3) carrying out centrifugal spray drying on the graphene oxide feed liquid at the drying temperature of 180 ℃, and finally obtaining graphene powder.
(2) Preparation of graphene resin dispersion
Heating and dehumidifying 15 parts by weight of graphene powder at 100 ℃ for 2 hours, premixing 80 parts by weight of epoxy resin and 2 parts by weight of dispersant, stirring at high speed for 35min, and grinding by using a three-roll mill to obtain a stable graphene resin dispersion liquid.
(3) Preparation of graphene modified resin packaging material
Adding 5 parts by weight of the prepared graphene resin dispersion liquid into a mixing tank, sequentially adding 22 parts by weight of E-44 type bisphenol A epoxy resin, 1.2 parts by weight of DT series toughening agent and 50 parts by weight of silica powder with the particle size less than 600 meshes in the component A according to the proportion, and uniformly stirring the casting material by using a dispersion machine for about 20min to obtain the component A.
According to the mass ratio of the component A to the component B of 1: 1, sequentially adding an acid anhydride curing agent, a dimethylaminopropylamine accelerator and a DT-series toughener (the using amount of each raw material in the component B is 20 parts by weight of the acid anhydride curing agent, 0.11 part by weight of the dimethylaminopropylamine accelerator and 2 parts by weight of the DT-series toughener), keeping the vacuum degree at 20mbar and the temperature at 50-65 ℃, uniformly stirring, and obtaining a casting material when no large amount of foam is generated and the temperature is kept at 50-65 ℃, namely the graphene modified resin packaging material.
(4) Preparing a dry-type transformer:
before pouring, the wound coil is loaded into a pouring mold, then the coil is transferred into a pouring tank, then the pouring tank is opened, the temperature is heated to 70-80 ℃, the vacuum pumping is carried out for 2-4 times, then the pouring material is added, and the feeding speed is controlled to be 0.5-1kg/min until the feeding is finished.
And heating and curing the poured mould in a curing furnace, keeping the curing temperature at 90-110 ℃, keeping for 20-30 minutes, discharging the coil out of the furnace after curing is finished, dismantling the mould at a higher speed, lifting the coil into the curing furnace, and slowly cooling to room temperature.
Example 3.
The specific operation steps are as follows:
(1) preparing graphene powder:
in an ice-water mixture, 10g of flake graphite is added into 320mL of concentrated sulfuric acid, 30g of potassium permanganate is slowly added while stirring by an electric stirrer, the reaction temperature is controlled to be less than 5 ℃, and the temperature is kept for 1 h.
Slowly adding 0.1g of potassium ferrate into the mixed solution under the stirring condition, heating to 45 ℃, and preserving the temperature for 15 hours to obtain dark green liquid.
Adding the obtained dark green liquid into 640ml of deionized water, stirring and mixing uniformly, and then adding 20ml of hydrogen peroxide with the mass fraction of 30%; and (3) sequentially adopting 500ml of 5% hydrochloric acid and deionized water for the mixed solution, washing by using a ceramic membrane filter, and repeating the washing process until the conductivity of the waste acid is reduced to be less than 100us/cm, so as to obtain the graphene oxide feed liquid.
And (3) carrying out centrifugal spray drying on the graphene oxide feed liquid at the drying temperature of 250 ℃, and finally obtaining graphene powder.
(2) Preparation of graphene resin dispersion
And (2) heating and dehumidifying 15 parts by weight of graphene powder at 100 ℃ for 2h, premixing with 80 parts by weight of epoxy resin and 2 parts by weight of dispersant, stirring at high speed for 35min, and grinding by using a three-roll mill to obtain a stable graphene resin dispersion liquid.
(3) Preparation of graphene modified resin packaging material
Adding 10 parts by weight of the prepared graphene resin dispersion liquid into a mixing tank, sequentially adding 22 parts by weight of bisphenol A epoxy resin, 1.2 parts by weight of DT series toughening agent and 50 parts by weight of 600-mesh silica powder in the component A according to the proportion, and uniformly stirring the casting material by using a dispersion machine for about 20min to obtain the component A.
According to the mass ratio of the component A to the component B of 1:0.9, sequentially adding 20 parts by weight of anhydride curing agent, 0.11 part by weight of dimethylaminopropylamine accelerator and 2 parts by weight of DT toughening agent (the raw materials in the component B comprise 20 parts by weight of anhydride curing agent, 0.11 part by weight of dimethylaminopropylamine accelerator and 2 parts by weight of DT toughening agent), keeping the vacuum degree at 20mbar and the temperature at 50-65 ℃, uniformly stirring, and obtaining the casting material when no large amount of foam is generated and the temperature is kept at 50-65 ℃, namely the graphene modified resin packaging material.
(4) Preparing a dry-type transformer:
before pouring, the wound coil is loaded into a pouring mold, then the coil is transferred into a pouring tank, then the pouring tank is opened, the temperature is heated to 70-80 ℃, the vacuum pumping is carried out for 2-4 times, then the pouring material is added, and the feeding speed is controlled to be 0.5-1kg/min until the feeding is finished.
And heating and curing the poured mould in a curing furnace, keeping the curing temperature at 90-110 ℃, keeping for 20-30 minutes, discharging the coil out of the furnace after curing is finished, dismantling the mould at a higher speed, lifting the coil into the curing furnace, and slowly cooling to room temperature.
Example 4.
The specific operation steps are as follows:
(1) preparing graphene powder:
and (2) adding 10g of microcrystalline graphite into 320mL of concentrated sulfuric acid in an ice-water mixture, slowly adding 30g of potassium permanganate while stirring by using an electric stirrer, controlling the reaction temperature to be less than 5 ℃, and preserving heat for 1 h.
Slowly adding 0.1g of potassium ferrate into the mixed solution under the stirring condition, heating to 45 ℃, and preserving the temperature for 10 hours to obtain dark green liquid.
Adding the obtained dark green liquid into 640ml of deionized water, and stirring and mixing uniformly; then adding 20ml of hydrogen peroxide with the mass fraction of 30 percent, and uniformly mixing; and (3) sequentially adopting 500ml of 5% hydrochloric acid and deionized water for the mixed solution, washing by using a ceramic membrane filter, and repeating the washing process until the conductivity of the waste acid is reduced to be less than 100us/cm, so as to obtain the graphene oxide feed liquid.
And (3) carrying out centrifugal spray drying on the graphene oxide feed liquid at the drying temperature of 180 ℃, and finally obtaining graphene powder.
(2) Preparation of graphene resin dispersion
Heating and dehumidifying 15 parts by weight of graphene powder at 100 ℃ for 2h, premixing 75 parts by weight of epoxy resin and 1 part by weight of dispersant, stirring at high speed for 35min, and grinding by using a three-roll mill to obtain a stable graphene resin dispersion liquid.
(3) Preparation of graphene modified resin packaging material
Adding 10 parts by weight of the prepared graphene resin dispersion liquid into a mixing tank, sequentially adding 25 parts by weight of bisphenol A epoxy resin, 2 parts by weight of DT series toughening agent and 52 parts by weight of 600-mesh silica micropowder in the component A according to the proportion, and uniformly stirring the casting material by using a dispersion machine for about 20min to obtain the component A.
According to the mass ratio of the component A to the component B of 1: 1.4, adding an acid anhydride curing agent, a dimethylaminopropylamine accelerator and a DT-series flexibilizer in sequence (the raw materials in the component B comprise, by weight, 25 parts of the acid anhydride curing agent, 0.15 part of the dimethylbenzylamine accelerator and 5 parts of the DT-series flexibilizer, keeping the vacuum degree at 20mbar and the temperature at 50-65 ℃, uniformly stirring, and obtaining a casting material when no large amount of foam is generated and the temperature is kept at 50-65 ℃, namely the graphene modified resin packaging material.
(4) Preparing a dry-type transformer:
before pouring, the wound coil is loaded into a pouring mold, then the coil is transferred into a pouring tank, then the pouring tank is opened, the temperature is heated to 70-80 ℃, the vacuum pumping is carried out for 2-4 times, then the pouring material is added, and the feeding speed is controlled to be 0.5-1kg/min until the feeding is finished.
And heating and curing the poured mould in a curing furnace, keeping the curing temperature at 90-110 ℃, keeping for 20-30 minutes, discharging the coil out of the furnace after curing is finished, dismantling the mould at a higher speed, lifting the coil into the curing furnace, and slowly cooling to room temperature.
Example 5.
The specific operation steps are as follows:
(1) preparing graphene powder:
in an ice-water mixture, 10g of expanded graphite is added into 320mL of concentrated sulfuric acid, 30g of potassium permanganate is slowly added while stirring by an electric stirrer, the reaction temperature is controlled to be less than 5 ℃, and the temperature is kept for 1 h.
Slowly adding 0.1g of potassium ferrate into the mixed solution under the stirring condition, heating to 45 ℃, and preserving the temperature for 15 hours to obtain dark green liquid.
Adding the obtained dark green liquid into 640ml of deionized water, and stirring and mixing uniformly; then 20ml of hydrogen peroxide with the mass fraction of 30 percent is added; and (3) sequentially adopting 500ml of 5% hydrochloric acid and deionized water for the mixed solution, washing by using a ceramic membrane filter, and repeating the washing process until the conductivity of the waste acid is reduced to be less than 100us/cm, so as to obtain the graphene oxide feed liquid.
And (3) carrying out centrifugal spray drying on the graphene oxide feed liquid at the drying temperature of 280 ℃ to finally obtain graphene powder.
(2) Preparation of graphene resin dispersion
Heating and dehumidifying 25 parts by weight of graphene powder at 100 ℃ for 2h, premixing with 85 parts by weight of epoxy resin and 5 parts by weight of dispersant, stirring at high speed for 35min, and grinding by using a three-roll mill to obtain stable graphene resin dispersion.
(3) Preparation of graphene modified resin packaging material
Adding 1 part by weight of the prepared graphene resin dispersion liquid into a mixing tank, sequentially adding 18 parts by weight of bisphenol A epoxy resin, 0.5 part by weight of DT series toughening agent and 48 parts by weight of 600-mesh silica micropowder in the component A according to the proportion, and uniformly stirring the casting material by using a dispersion machine for about 20min to obtain the component A.
According to the mass ratio of the component A to the component B of 1:0.9, adding 15 parts by weight of anhydride curing agent, 0.05 part by weight of dimethyl phthalate accelerator and 2 parts by weight of DT toughening agent in the component B, keeping the vacuum degree at 20mbar and the temperature at 50-65 ℃, uniformly stirring, and obtaining the casting material, namely the graphene modified resin packaging material when no large amount of foam is generated and the temperature is kept at 50-65 ℃.
(4) Preparing a dry-type transformer:
before pouring, the wound coil is loaded into a pouring mold, then the coil is transferred into a pouring tank, then the pouring tank is opened, the temperature is heated to 70-80 ℃, the vacuum pumping is carried out for 2-4 times, then the pouring material is added, and the feeding speed is controlled to be 0.5-1kg/min until the feeding is finished.
And heating and curing the poured mould in a curing furnace, keeping the curing temperature at 90-110 ℃, keeping for 20-30 minutes, discharging the coil out of the furnace after curing is finished, dismantling the mould at a higher speed, lifting the coil into the curing furnace, and slowly cooling to room temperature.
Comparative example
Preparing a dry-type transformer resin packaging material:
and (2) sequentially adding 22 parts by weight of bisphenol A epoxy resin, 1.2 parts by weight of DT series toughening agent and 50 parts by weight of 600-mesh silica micropowder in the component A according to the proportion, and uniformly stirring the castable by a dispersion machine for about 20min to obtain the component A.
According to the mass ratio of the component A to the component B of 1:0.9, sequentially adding 20 parts by weight of anhydride curing agent, 0.1 part by weight of dimethylaminopropylamine accelerator and 2 parts by weight of DT series toughening agent, keeping the vacuum degree at 20mbar, uniformly stirring, and obtaining the casting material when no large amount of foam is generated and the temperature is kept at 50-65 ℃.
Before pouring, the wound coil is loaded into a pouring mold, then the coil is transferred into a pouring tank, then the pouring tank is opened, the temperature is heated to 70-80 ℃, the vacuum pumping is carried out for 2-4 times, then the pouring material is added, and the feeding speed is controlled to be 0.5-1kg/min until the feeding is finished. And heating and curing the poured mould in a curing furnace, keeping the curing temperature at 90-110 ℃, keeping for 20-30 minutes, discharging the coil out of the furnace after curing is finished, dismantling the mould at a higher speed, lifting the coil into the curing furnace, and slowly cooling to room temperature.
For a temperature rise test of a sample piece of the graphene modified resin packaging material, comparing the thermal conductivity of the graphene modified resin at different temperatures with a comparative example, specifically, temperature rise temperature difference Δ T in table 1 is the temperature of example 1(2 or 3) in the process of temperature rise or temperature reduction-the temperature of the comparative example under the same condition;
the detection results are shown in table 1 after the packaging material is cured according to the GB/T15022.5-2011 standard requirements for sample resistivity, dielectric factor loss and relative dielectric constant of the graphene modified resin packaging material.
Table 1 graphene modified resin encapsulation material sample property detection
| Detecting items | Example 1 | Example 2 | Example 3 | Comparative example |
| Flexural strength (Mpa) | 228.9 | 255.4 | 270.7 | 241.7 |
| Hardness (shored) | 86.5 | 90.1 | 86.5 | 90.6 |
| Tensile strength (Mpa) | 1850.4 | 2595.5 | 2520.3 | 2196.8 |
| Temperature difference of △ T (DEG C) | 1.7 | 6.9 | 2.3 | 0 |
| Volume resistivity (omega. m) | 2.33*1013 | 1.73*1014 | 2.05*1013 | 6.69*1014 |
| Surface resistivity (omega) | 2.86*1015 | 9.56*1016 | 2.86*1015 | 5.12*1015 |
| Dielectric loss factor | 0.018 | 0.0198 | 0.0181 | 0.0154 |
| Relative dielectric constant | 6.078 | 4.637 | 8.52 | 3.727 |
As can be seen from the above table, the mechanical property indexes such as the bending strength and the tensile strength of the sample of the graphene modified resin packaging material in example 2 are superior to those of the comparative example, and it is further shown that the mechanical property of the resin packaging material can be improved by adding the graphene with the controllable number of layers into the resin material.
Temperature rise tests performed on graphene modified resin packaging material samples show that the temperature difference between the embodiment and the comparative example is improved to different extents, wherein the temperature difference in the embodiment 2 is more 6.9 ℃, and further shows that the composite intermediate prepared by the multilayer three-dimensional graphene/EP synergistic effect has the advantages of utilizing the strength and the heat dissipation performance of the graphene three-dimensional structure, and the heat dissipation performance and the strength of the graphene modified resin packaging material are greatly improved. The method has positive significance for reducing energy consumption and prolonging service life of the dry-type transformer in operation.
In the aspect of insulation verification of the graphene modified resin packaging material, according to GB/T15022.5-2011 resin-based active compound for electrical insulation part 5: in the quartz filler epoxy resin compound table 2, the volume resistivity of the cured epoxy resin compound containing the quartz filler is more than or equal to 1.0 x 1012 omega-m, the dielectric loss is less than or equal to 0.02, and the relative dielectric constant is less than or equal to 5, and the insulativity of the epoxy resin compound is superior to the standard in the embodiment 2 of the invention. Further, the number of layers, the oxygen content and the addition amount of the graphene material are controlled, so that the graphene material cannot form conductive network connection in the material, an insulating effect is achieved, the insulation resistance of the graphene modified resin material is further improved, and the dielectric loss factor is reduced.
According to the preparation method, the reaction time and the drying temperature of graphene preparation are controlled, the number of graphene layers and the oxygen content are further controlled, the graphene is soaked in resin in advance, then the graphene is added into dissolved epoxy resin (EP), a composite intermediate with the advantages of the graphene and the graphene is prepared through a multi-layer three-dimensional graphene/EP synergistic effect, the strength and the heat dissipation performance of the graphene three-dimensional structure are utilized, and the heat dissipation performance and the strength of the graphene modified resin packaging material are greatly improved. In addition, the number of layers, the oxygen content and the addition amount of the graphene material are controlled, so that the graphene material cannot form conductive network connection in the material, an insulating effect is achieved, the insulation resistance of the graphene modified resin material is further improved, and the dielectric loss factor is reduced.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (10)
1. The graphene modified resin packaging material is characterized by being formed by combining a component A and a component B according to the mass ratio of 1: 0.9-1.4;
wherein, the component A comprises: 18-25 parts of bisphenol A epoxy resin, 0.5-2 parts of toughening agent, 1-10 parts of graphene resin dispersion liquid and 48-52 parts of silicon micro powder;
the component B comprises: 15-25 parts of curing agent, 0.05-0.15 part of accelerator and 1-5 parts of toughening agent.
2. The graphene-modified resin encapsulation material according to claim 1,
the bisphenol A type epoxy resin is E-51 type, or E-44 type, or a mixture of E-51 type and E-44 type;
the toughening agent is a DT series toughening agent;
the grain diameter of the silicon micro powder is less than 600 meshes;
the curing agent is an anhydride curing agent;
the accelerator is at least one of dimethylaminopropylamine, dimethylbenzylamine and dimethyl phthalate.
3. The graphene-modified resin encapsulation material according to claim 1,
the graphene resin dispersion liquid is composed of 75-85 parts by weight of epoxy resin, 1-5 parts by weight of dispersant and 15-25 parts by weight of graphene powder.
4. The graphene-modified resin encapsulation material according to claim 3,
the graphene sheet diameter in the graphene resin dispersion liquid is 1-10 mu m.
5. The graphene-modified resin encapsulation material according to claim 4,
the graphene powder has the oxygen content of 8-12% and the number of layers within 10.
6. The graphene-modified resin encapsulation material according to claim 3,
the resin in the graphene resin dispersion liquid is E-51 type bisphenol A epoxy resin;
the dispersing agent in the graphene resin dispersion liquid is acetone.
7. The method for preparing the graphene modified resin encapsulation material according to claim 1, comprising the steps of:
s10 preparation of graphene resin dispersion liquid:
heating and dehumidifying graphene powder, mixing with epoxy resin and a dispersing agent, stirring at a high speed, and grinding to obtain a stable graphene resin dispersion liquid;
s20 preparation of component A:
sequentially adding bisphenol A type epoxy resin, a toughening agent and silicon micropowder into the graphene resin dispersion liquid, and uniformly mixing to obtain the component A;
s30, preparing the graphene modified resin packaging material:
and (2) sequentially adding a curing agent, an accelerator and a toughening agent into the component A, and stirring under a vacuum condition at 50-65 ℃ until no large amount of foam is generated to obtain the graphene modified resin packaging material.
8. The graphene-modified resin encapsulation material according to claim 7,
in the step S10, the heating and dehumidifying temperature is 100 ℃, and the time is 2 h;
in step S30, the vacuum degree is 20 mbar.
9. The graphene-modified resin encapsulation material according to claim 7,
the preparation method of the graphene powder comprises the following steps:
adding graphite into concentrated sulfuric acid in an ice water mixture, slowly adding potassium permanganate while stirring, controlling the reaction temperature to be less than 5 ℃, and preserving heat for 1-2 hours; slowly adding potassium ferrate under stirring, heating to 45 deg.C, and maintaining for 5-20 hr to obtain dark green liquid; wherein the graphite is crystalline flake graphite, microcrystalline graphite or expanded graphite; the mass-volume ratio of the graphite to the potassium permanganate to the potassium ferrate to the concentrated sulfuric acid is 10 g: 30g of: 0.1 g: 320 ml;
adding the dark green liquid into deionized water, and stirring and mixing uniformly; adding 30% hydrogen peroxide by mass and uniformly mixing to obtain a mixed solution; wherein the mass volume ratio of the graphite to the deionized water to the hydrogen peroxide is 10 g: 640 ml: 20ml of the solution;
washing the mixed solution by using a hydrochloric acid solution with the mass fraction of 5% and deionized water through a ceramic membrane filter in sequence, and repeating the washing process until the conductivity of the waste acid is reduced to be below 100us/cm, so as to obtain a graphene oxide feed liquid; wherein, the mixed solution is washed by 500ml of washing liquid in turn each time;
and carrying out centrifugal spray drying on the graphene oxide feed liquid, wherein the drying temperature is 120-280 ℃.
10. The preparation method of the dry-type transformer is characterized in that the dry-type transformer is prepared by adopting a vacuum casting method, and comprises the following steps:
s10, batching: a castable material is obtained by the preparation method of claim 7, namely the graphene modified resin packaging material; placing the casting material in a casting tank;
s20 pouring: after the wound coil is loaded into a casting mold, the casting tank is added and opened, the temperature is raised to 70-80 ℃, the casting tank is vacuumized for 2-4 times, then the casting material is added, and the feeding speed is controlled to be 0.5-1kg/min until the feeding is finished;
s10 curing and demolding: and heating and curing the cast mold in a curing furnace, keeping the curing temperature at 90-110 ℃ for 20-30min, discharging the coil out of the furnace after curing is finished, dismantling the mold, and slowly cooling to room temperature.
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