CN115851195A - Elastic epoxy adhesive applied to encapsulation of new energy photovoltaic inductor and preparation method thereof - Google Patents

Elastic epoxy adhesive applied to encapsulation of new energy photovoltaic inductor and preparation method thereof Download PDF

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CN115851195A
CN115851195A CN202211593531.7A CN202211593531A CN115851195A CN 115851195 A CN115851195 A CN 115851195A CN 202211593531 A CN202211593531 A CN 202211593531A CN 115851195 A CN115851195 A CN 115851195A
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parts
new energy
energy photovoltaic
inductor
encapsulation
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伍时县
李妃文
吴小平
周群邦
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Dongguan Jiadi New Material Co ltd
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Dongguan Jiadi New Material Co ltd
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Abstract

The invention discloses an elastic epoxy adhesive for encapsulating a new energy photovoltaic inductor, which is formed by mixing a component A and a component B in a volume ratio of 5-6; the component A comprises the following components in parts by weight: 20 to 50 portions of organic silicon modified epoxy resin, 2 to 10 portions of reactive diluent, 0.5 to 5 portions of auxiliary agent and 40 to 70 portions of functional powder; the component B comprises the following components in parts by weight: 10-30 parts of a crosslinking curing agent; also discloses a preparation method of the elastic epoxy glue applied to the encapsulation of the new energy photovoltaic inductor. The elastic epoxy adhesive can be cured at normal temperature, has the performances of low hardness of 40-70A, resistance to high and low temperature of-50-150 ℃ and circulation for 1000 hours without cracking, resistance to high temperature and high humidity of 85 ℃ for 1000 hours without color change, resistance to salt spray without color change for 500 hours, hardness change after high temperature of 150 ℃ for 1000 hours is less than 10 percent of change rate, and good flame retardant V-0 and heat-conducting properties.

Description

Elastic epoxy adhesive applied to encapsulation of new energy photovoltaic inductor and preparation method thereof
Technical Field
The invention relates to the technical field of pouring sealant, in particular to elastic epoxy glue applied to new energy photovoltaic inductor pouring and a preparation method thereof.
Background
In recent years, with the instability of the world situation and the shortage of petrochemical energy supply, and the rising of petroleum price, people urgently need more clean energy to deal with the increasing petroleum crisis and achieve the common goal of reducing carbon emission, so that the world and China rapidly increase the demand for new photovoltaic energy, and the demand for related photovoltaic modules and parts is also rising. Because the photovoltaic module can be applied to severe environments such as desert zones, sea and river zones and the like, the photovoltaic module can adapt to environments such as high temperature, low temperature, high humidity and high salt fog, and higher requirements are provided for the pouring sealant of the photovoltaic module based on the requirements.
The types of glue applied to inductance encapsulation at present mainly comprise addition type silica gel pouring sealant, polyurethane pouring sealant and epoxy pouring sealant, wherein the addition type silica gel pouring sealant is widely applied by the advantages of good high and low temperature resistance, low viscosity, low price and the like, but the silica gel has poor moisture resistance due to low strength, poor bonding force, poor air permeability and the like, and the actual application requirements of high bonding, long-term water resistance and salt mist resistance are insufficient; the polyurethane pouring sealant has good adhesive property, flexibility and low-temperature resistance, but has a defect in the requirements on high-temperature resistance and hydrolysis resistance; the traditional high-hardness epoxy pouring sealant has the phenomenon of cracking at the edge of a base material due to shrinkage at high and low temperatures because of high hardness and high curing stress.
At the present stage, some epoxy potting soft rubbers on the market mostly adopt a mode of external addition of a plasticizer and the like to reduce the hardness of a product, or adopt a method of reducing the hardness by adopting sulfur-containing sulfydryl modified resin (see a patent with the patent number of CN 114806477A), and adopt the soft rubbers with the external addition of the plasticizer, so that the problems of cracking, obvious hardness increase and the like are often caused in the process of carrying out a long-time high-temperature test; secondly, the pouring sealant modified by the sulfydryl resin containing the sulfur element has good hardness, but the residual sulfydryl is combined with water to cause poor water resistance due to the problem of reaction rate, and meanwhile, the precipitation of the sulfur element at the later stage can cause the oxidation of a metal contact to influence the conductivity.
The scheme of modifying component A by adopting hydroxyl-terminated polyurethane prepolymer and grease (plasticizer) and modifying methyl nadic anhydride by adopting carboxyl-terminated polyurethane prepolymer requires heating and curing, and can not be cured at normal temperature or can be heated for a short time at a low temperature of less than 90 ℃.
Therefore, aiming at the requirements of current and future photovoltaic devices, it is necessary to develop an elastic epoxy pouring sealant which is cured at normal temperature and has good low-temperature flexibility, good high-temperature resistance, excellent salt and moisture resistance and other performances.
Disclosure of Invention
In order to overcome the technical problem, the invention discloses an elastic epoxy adhesive applied to new energy photovoltaic inductor encapsulation and a preparation method thereof.
The technical scheme adopted by the invention for realizing the purpose is as follows:
the elastic epoxy glue for encapsulating the new energy photovoltaic inductor comprises a component A and a component B which are mixed according to a volume ratio of 5;
the component A comprises the following components in parts by weight: 20 to 50 portions of organic silicon modified epoxy resin, 2 to 10 portions of reactive diluent, 0.5 to 5 portions of auxiliary agent and 40 to 70 portions of functional powder;
the component B comprises the following components in parts by weight: 10-30 parts of a crosslinking curing agent.
The elastic epoxy adhesive applied to the encapsulation of the new energy photovoltaic inductor comprises the following components in percentage by mass: 30-70% of organosilicon compound and epoxy compound;
optionally, the amino content of the organic compound is 5-20%, and the silicon content is 1-10%;
the organic compound comprises but is not limited to one or a combination of N-2 aminoethyl-3-aminopropylmethyldimethoxysilane, gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane and gamma-aminopropyltriethoxysilane;
optionally, the epoxy value of the epoxy compound is 0.45 to 0.7eq/100g;
the epoxy compound includes but is not limited to one or a combination of several of methyl tetrahydrophthalic acid diglycidyl ester, decyl glycidyl ether, hydantoin epoxy resin, butadiene modified epoxy resin and bisphenol A epoxy resin E51.
The elastic epoxy adhesive applied to the encapsulation of the new energy photovoltaic inductor is characterized in that the active diluent is a low-viscosity epoxy compound with an epoxy value of 0.3-0.7 eq/100g;
the reactive diluent comprises but is not limited to one or a combination of several of methoxypolyethylene glycol glycidyl ether, benzyl glycidyl ether, polypropylene glycol diglycidyl ether and propoxyglycerol triglycidyl ether.
The elastic epoxy adhesive applied to encapsulation of the new energy photovoltaic inductor comprises 0.1-2% by mass of an auxiliary agent: 1-10%: 1-5% of surfactant, promoter and color paste;
optionally, the surfactant is polyoxyethylene polyoxypropylene pentaerythritol ether, polydimethylsiloxane, polyethylene glycol 200;
the accelerator is dodecylphenol, and the molecular weight of the dodecylphenol is 550-1000;
the color paste is 10% of carbon black.
The elastic epoxy glue applied to encapsulation of the new energy photovoltaic inductor is characterized in that the functional powder comprises the following components in parts by weight: 65-75 parts of flame retardant, 17-22 parts of heat conducting powder and 17-22 parts of aluminum oxide;
optionally, the density of the flame retardant is 1.5-2.0 g/ml, and the particle size D50 is 5-20 μm;
the density of the heat conducting powder is 2.5-3.5 g/ml, and the particle size D50 is 1-3 mu m;
the density of the alumina is 3.0-4.0 g/ml, and the grain diameter D50 is 10-20 μm.
The elastic epoxy glue applied to the encapsulation of the new energy photovoltaic inductor is characterized in that the flame retardant comprises one or a combination of more of ammonium polyphosphate with the particle size of 10-20 microns, melamine with the particle size of 5-15 microns, aluminum hypophosphite with the particle size of 10-20 microns and aluminum hydroxide with the particle size of 8-12 microns;
the heat conducting powder is fused silica micropowder with the particle size of 10-20 mu m;
the alumina comprises one or a combination of more of 1-3 μm spherical alumina and 10-20 μm spherical alumina.
The elastic epoxy adhesive applied to the encapsulation of the new energy photovoltaic inductor comprises the following components in percentage by mass: 30-60%: 3-15% aliphatic amine curing agent, modifier and bridging agent;
optionally, the aliphatic amine curing agent comprises one or a combination of more of N- (3-aminopropyl) cyclohexylamine, polyetheramine D-230, polyetheramine D-400 and polyetheramine D-2000;
the modifier is one or a combination of several of dodecylphenol, polyhexamethylene lactone diol and 1,4 butanediol;
the bridging agent is HDI.
The elastic epoxy adhesive applied to the encapsulation of the new energy photovoltaic inductor is characterized in that the amine value of the N- (3-aminopropyl) cyclohexylamine is 1000-1200 mgKOH/g, the amine value of the polyetheramine D-230 is 398-489 mgKOH/g, the amine value of the polyetheramine D-400 is 220-300 mgKOH/g, and the amine value of the polyetheramine D-2000 is 50-70 mgKOH/g;
the molecular weight of the dodecylphenol is 260-400, the molecular weight of the polycaprolactone diol is 550-1000, and the purity of the 1, 4-butanediol is 95-99.9%;
the NCO content of the HDI was 23.5%.
A preparation method of elastic epoxy glue applied to new energy photovoltaic inductor encapsulation is used for preparing the elastic epoxy glue applied to new energy photovoltaic inductor encapsulation;
the preparation method comprises the following steps:
step 1, preparing organic silicon modified epoxy resin;
step 2, adding an active diluent and an auxiliary agent into the organic silicon modified epoxy resin, dispersing and premixing for 20-30 minutes at a high speed of 10-20 Hz/minute, adding functional powder, continuously stirring for 50-90 minutes at the conditions of 30-50 Hz/minute and 100-110 ℃, vacuumizing to remove bubbles, testing and packaging to obtain a component A;
and 3, taking the aliphatic amine curing agent, the accelerator and the HDI, carrying out addition reaction for 3 hours at 70-80 ℃ in a reaction kettle with nitrogen protection, cooling, testing and packaging to obtain the component B.
The elastic epoxy glue applied to encapsulation of the new energy photovoltaic inductor is described above, wherein the step 1 specifically includes: adding the epoxy compound into a reaction kettle, heating to 60-100 ℃, introducing nitrogen for protection, keeping 0.01-0.3 mPa atmospheric pressure, discharging humid air, slowly adding the organic silicon compound at the flow rate of 1-10 kg/min, carrying out premixing reaction for 90-120 min at the rotation speed of 10-50 Hz/min, and cooling to normal temperature to obtain the organic silicon modified epoxy resin.
The beneficial effects of the invention include the following:
(1) The elastic epoxy adhesive can be cured at normal temperature, has the excellent performances of low hardness of 40-70A of Shore hardness, resistance to high and low temperature circulation (30 min high temperature and 30min low temperature) of-50-150 ℃ for 1000 hours without cracking, resistance to high temperature and high humidity of double 85 for 1000 hours without discoloring, resistance to salt spray for 500 hours without discoloring and the like, has the hardness change of less than 10 percent after the high temperature of 150 ℃ for 1000 hours, and has good flame retardant V-0 and heat-conducting properties;
(2) The viscosity of a reaction system can be adjusted by adding a proper amount of the low-molecular-weight reactive diluent, and the powder of the reaction system can be wetted and dispersed by a small amount of the auxiliary agent, so that the addition amount of the functional powder is increased, the affinity between the functional powder and resin molecules is increased, the sedimentation risk of the functional powder is reduced, and the storage time of a product is prolonged;
(3) The organosilicon modified epoxy resin with excellent weather resistance is prepared by initiatively adopting the reaction of the organosilicon compound and the flexible epoxy compound, amino groups and epoxy groups in the organosilicon compound are partially reacted to introduce Si-O bonds to generate the organosilicon modified epoxy resin, so that the temperature resistance of the organosilicon modified epoxy resin is effectively enhanced, and the organosilicon modified epoxy resin with different functions can be obtained by selecting the reaction with different types of epoxy compounds, so that the use requirements of multiple properties such as high temperature resistance, low temperature resistance, chemical resistance and the like can be met; and secondly, the reaction system reacts in the nitrogen protection atmosphere, so that the influence of the reaction of moisture in the air and amino can be isolated, unnecessary side reactions can be reduced, a more stable reaction product can be obtained, the reaction time can be shortened by utilizing a heating mode, and an industrial large-scale production mode is facilitated.
Drawings
The invention is further illustrated by the following examples in conjunction with the drawings.
FIG. 1 is a schematic diagram of the reaction principle of the silicone-modified epoxy resin of the present invention.
Detailed Description
The present invention is further illustrated by the following specific examples, which are intended to facilitate the understanding and appreciation of the technical solutions of the present invention, rather than to limit the invention thereto.
Referring to fig. 1, the elastic epoxy adhesive for encapsulating the new energy photovoltaic inductor provided by the invention comprises a component A and a component B which are mixed according to a volume ratio of 5;
the component A comprises the following components in parts by weight: 20 to 50 portions of organic silicon modified epoxy resin, 2 to 10 portions of reactive diluent, 0.5 to 5 portions of auxiliary agent and 40 to 70 portions of functional powder;
the component B comprises the following components in parts by weight: 10-30 parts of a crosslinking curing agent.
Preferably, the organosilicon modified epoxy resin comprises, by mass, 10 to 50%: 30-70% of organosilicon compound and epoxy compound;
optionally, the amino content of the organic compound is 5-20%, and the silicon content is 1-10%;
the organic compound comprises but is not limited to one or a combination of N-2 aminoethyl-3-aminopropylmethyldimethoxysilane (KBM-602), gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane (KH 560) and gamma-aminopropyltriethoxysilane (KH 550);
optionally, the epoxy value of the epoxy compound is 0.45 to 0.7eq/100g;
the epoxy compound includes but is not limited to one or a combination of several of methyl tetrahydrophthalic acid diglycidyl ester (XY 812), decyl glycidyl ether, hydantoin epoxy resin, butadiene modified epoxy resin and bisphenol A epoxy resin E51.
Preferably, the reactive diluent is a low-viscosity epoxy compound with an epoxy value of 0.3-0.7 eq/100g;
the reactive diluent comprises but is not limited to one or a combination of methoxy polyethylene glycol glycidyl ether (MPEG-EO), benzyl glycidyl ether (692), polypropylene glycol diglycidyl ether (207) and propoxyglycerol triglycidyl ether.
Preferably, the auxiliary agent comprises, by mass, 0.1 to 2%: 1-10%: 1-5% of surfactant, promoter and color paste;
optionally, the surfactant is polyoxyethylene polyoxypropylene pentaerythritol ether, polydimethylsiloxane, polyethylene glycol 200;
the accelerator is dodecylphenol, and the molecular weight of the dodecylphenol is 550-1000;
the color paste is 10% of carbon black.
Preferably, the functional powder comprises the following components in parts by weight: 65-75 parts of flame retardant, 17-22 parts of heat conducting powder and 17-22 parts of aluminum oxide;
optionally, the density of the flame retardant is 1.5-2.0 g/ml, and the particle size D50 is 5-20 μm;
the density of the heat conducting powder is 2.5-3.5 g/ml, and the particle size D50 is 1-3 mu m;
the density of the alumina is 3.0-4.0 g/ml, and the grain diameter D50 is 10-20 μm.
Preferably, the flame retardant comprises one or a combination of more of 10-20 μm ammonium polyphosphate, 5-15 μm melamine, 10-20 μm aluminum hypophosphite and 8-12 μm aluminum hydroxide;
the heat conducting powder is fused silica micropowder with the particle size of 10-20 mu m;
the alumina comprises one or a combination of more of 1-3 μm spherical alumina and 10-20 μm spherical alumina.
Preferably, the crosslinking curing agent comprises 20-40% by mass: 30-60%: 3-15% aliphatic amine curing agent, modifier and bridging agent;
optionally, the aliphatic amine curing agent comprises one or a combination of N- (3-aminopropyl) Cyclohexylamine (CHAPA), polyetheramine D-230, polyetheramine D-400 and polyetheramine D-2000;
the modifier is one or a combination of several of dodecylphenol, polyhexamethylene lactone diol and 1,4 butanediol;
the bridging agent is HDI (TLA-100).
Preferably, the amine value of the N- (3-aminopropyl) cyclohexylamine is 1000-1200 mgKOH/g, the amine value of the polyetheramine D-230 is 398-489 mgKOH/g, the amine value of the polyetheramine D-400 is 220-300 mgKOH/g, and the amine value of the polyetheramine D-2000 is 50-70 mgKOH/g;
the molecular weight of the dodecylphenol is 260-400, the molecular weight of the polycaprolactone diol is 550-1000, and the purity of the 1, 4-butanediol is 95-99.9%;
the NCO content of the HDI was 23.5%.
The invention also discloses a preparation method of the elastic epoxy glue for encapsulating the new energy photovoltaic inductor, and the preparation method is used for preparing the elastic epoxy glue for encapsulating the new energy photovoltaic inductor;
the preparation method comprises the following steps:
step 1, preparing organic silicon modified epoxy resin;
step 2, adding an active diluent into the organic silicon modified epoxy resin, adjusting the viscosity, adding an auxiliary agent, dispersing and premixing at a high speed of 10-20 Hz/min for 20-30 min, adding functional powder, continuously stirring for 50-90 min under the conditions of 30-50 Hz/min and 100-110 ℃, vacuumizing to remove bubbles, testing and packaging to obtain a component A; specifically, the viscosity of the reaction system can be adjusted by adding a proper amount of the low-molecular-weight reactive diluent, and a small amount of the auxiliary agent can wet and disperse the powder of the reaction system, so that the addition amount of the functional powder is increased, the affinity between the functional powder and resin molecules is increased, the sedimentation risk of the functional powder is reduced, and the storage time of the product is prolonged;
step 3, taking the aliphatic amine curing agent, the accelerator and the HDI, carrying out addition reaction for 3 hours at 70-80 ℃ in a reaction kettle with nitrogen protection, cooling, testing and packaging to obtain a component B;
preferably, the step 1 specifically includes: adding an epoxy compound into a reaction kettle, heating to 60-100 ℃, introducing nitrogen for protection, keeping 0.01-0.3 mPa atmospheric pressure, discharging humid air, slowly adding an organic silicon compound at a flow rate of 1-10 kg/min, carrying out premixing reaction for 90-120 min at a rotation speed of 10-50 Hz/min, and cooling to normal temperature to obtain the organic silicon modified epoxy resin; specifically, the organosilicon modified epoxy resin with excellent weather resistance is creatively prepared by reacting the organosilicon compound with a flexible epoxy compound, amino groups and epoxy groups in the organosilicon compound are partially reacted to introduce Si-O bonds to generate the organosilicon modified epoxy resin, so that the temperature resistance of the organosilicon modified epoxy resin is effectively enhanced, and the organosilicon modified epoxy resin with different functions can be obtained by selecting and reacting with different types of epoxy compounds, so that the use requirements of multiple properties such as high temperature resistance, low temperature resistance, chemical resistance and the like can be met; and secondly, the reaction system reacts in the nitrogen protective atmosphere, so that the influence of the reaction of moisture and amino in the air can be isolated, unnecessary side reactions can be reduced, a more stable reaction product can be obtained, in addition, the reaction time can be shortened by utilizing a heating mode, and an industrial large-scale production mode is facilitated.
The preparation process according to the invention is now described in detail in the following examples:
example 1: this example synthesizes an organosilicon modified epoxy resin, including the following steps: adding 100 parts of methyl tetrahydrophthalic acid diglycidyl ester into a reaction kettle, heating to 90 ℃, introducing nitrogen for protection, keeping 0.1mPa atmospheric pressure, discharging humid air, slowly adding 20 parts of KBM-602 at the flow rate of 5 kg/min, carrying out premixing reaction at the rotation speed of 50 Hz/min for 100 min, and cooling to normal temperature to obtain the organic silicon modified epoxy resin.
Example 2: this example synthesizes an organosilicon modified epoxy resin, including the following steps: adding 100 parts of decyl glycidyl ether into a reaction kettle, heating to 90 ℃, introducing nitrogen for protection, keeping 0.1mPa atmospheric pressure, discharging humid air, slowly adding 20 parts of KBM-602 at the flow rate of 5 kg/min, carrying out premixing reaction for 100 min at the rotation speed of 50 Hz/min, and cooling to normal temperature to obtain the organic silicon modified epoxy resin.
Example 3: this example synthesizes an organosilicon modified epoxy resin, including the following steps: adding 100 parts of decyl glycidyl ether into a reaction kettle, heating to 90 ℃, introducing nitrogen for protection, keeping 0.1mPa atmospheric pressure, discharging humid air, slowly adding 35 parts of KBM-602 at the flow rate of 5 kg/min, carrying out premixing reaction for 100 min at the rotation speed of 50 Hz/min, and cooling to normal temperature to obtain the organic silicon modified epoxy resin.
Example 4: this example synthesizes an organosilicon modified epoxy resin, including the following steps: adding 100 parts of hydantoin epoxy resin into a reaction kettle, heating to 90 ℃, introducing nitrogen for protection, keeping 0.1mPa atmospheric pressure, discharging humid air, slowly adding 20 parts of KBM-602 at a flow rate of 5 kg/min, carrying out premixing reaction for 100 min at a rotation speed of 50 Hz/min, and cooling to normal temperature to obtain the organosilicon modified epoxy resin.
Example 5: this example synthesizes an organosilicon modified epoxy resin, including the following steps: adding 100 parts of butadiene modified epoxy resin into a reaction kettle, heating to 90 ℃, introducing nitrogen for protection, keeping the atmospheric pressure of 0.1mPa, discharging wet air, slowly adding 20 parts of gamma-aminopropyl triethoxysilane at the flow rate of 5 kg/min, carrying out premixing reaction at the rotation speed of 50 Hz/min for 100 min, and cooling to normal temperature to obtain the organosilicon modified epoxy resin.
The silicone-modified epoxy resins obtained in examples 1 to 5 were subjected to viscosity property parameter measurement at 25 ℃ and the detailed test results are shown in Table 1.
TABLE 1 measurement results of viscosity Performance parameters
Figure BDA0003995931400000091
Example 6: this example prepares component a, including the following steps: adding 5 parts of methoxypolyethylene glycol glycidyl ether, 0.5 part of polyoxyethylene polyoxypropylene pentaerythritol ether and 0.3 part of U carbon into 35 parts of the organosilicon modified epoxy resin prepared in example 1, dispersing and premixing for 30 minutes at a high speed of 20 Hz/minute, adding 8 parts of 15-micron ammonium polyphosphate, 50 parts of 15-micron fused silica powder and 1.2 parts of 3-micron spherical alumina, continuously stirring for 60 minutes at the conditions of 50 Hz/minute and 110 ℃, vacuumizing to remove bubbles, testing and packaging to obtain a component A; wherein the density of the ammonium polyphosphate is 1.5g/ml, and the particle size D50 is 15 mu m; the density of the silicon micro powder is 3g/ml, and the particle size D50 is 2 mu m; the alumina had a density of 3.0g/ml and a particle size D50 of 10 μm.
Example 7: this example prepares component a, including the following steps: adding 5 parts of methoxypolyethylene glycol glycidyl ether, 0.5 part of polyoxyethylene polyoxypropylene pentaerythritol ether and 0.3 part of U carbon into 35 parts of the organosilicon modified epoxy resin prepared in example 2, dispersing and premixing for 30 minutes at a high speed of 20 Hz/minute, adding 8 parts of 15 mu m melamine, 50 parts of 15 mu m fused silica powder and 1.2 parts of 3 mu m ball-like alumina, continuously stirring for 60 minutes at the conditions of 50 Hz/minute and 110 ℃, vacuumizing to remove bubbles, testing and packaging to obtain a component A; wherein the density of the melamine is 1.5g/ml, and the particle size D50 is 15 μm; the density of the silicon micro powder is 3g/ml, and the particle size D50 is 2 mu m; the alumina had a density of 3.0g/ml and a particle size D50 of 10 μm.
Example 8: this example prepares component a, including the following steps: adding 3 parts of methoxypolyethylene glycol glycidyl ether, 0.5 part of polyoxyethylene polyoxypropylene pentaerythritol ether and 0.3 part of U carbon into 37 parts of the organosilicon modified epoxy resin prepared in example 3, dispersing and premixing for 30 minutes at a high speed of 20 Hz/minute, adding 8 parts of 15-micron aluminum hypophosphite, 50 parts of 15-micron fused silica powder and 1.2 parts of 3-micron spherical alumina, continuously stirring for 60 minutes at the conditions of 50 Hz/minute and 110 ℃, vacuumizing to remove bubbles, testing and packaging to obtain a component A; wherein the density of the aluminum hypophosphite is 1.5g/ml, and the particle size D50 is 15 mu m; the density of the silicon micro powder is 3g/ml, and the particle size D50 is 2 mu m; the alumina had a density of 3.0g/ml and a particle size D50 of 10 μm.
Example 9: this example prepares component a, including the following steps: adding 3 parts of polypropylene glycol diglycidyl ether, 0.5 part of polydimethylsiloxane and 0.3 part of U carbon into 30 parts of the organosilicon modified epoxy resin prepared in example 1 and 7 parts of example 4, dispersing and premixing at a high speed of 20 Hz/min for 30 minutes, adding 8 parts of 15-micron aluminum hypophosphite, 50 parts of 15-micron fused silica powder and 1.2 parts of 3-micron spherical alumina, continuously stirring at the temperature of 110 ℃ for 60 minutes at the speed of 50 Hz/min, vacuumizing to remove bubbles, testing and packaging to obtain a component A; wherein the density of the aluminum hypophosphite is 1.5g/ml, and the particle size D50 is 15 mu m; the density of the silicon micro powder is 3g/ml, and the particle size D50 is 2 mu m; the alumina had a density of 3.0g/ml and a particle size D50 of 10 μm.
Example 10: this example prepares component a, including the following steps: adding 3 parts of methoxypolyethylene glycol glycidyl ether, 0.5 part of polyethylene glycol 200 and 0.3 part of U carbon into 30 parts of the organosilicon modified epoxy resin prepared in examples 1 and 7 parts of example 5, dispersing and premixing at a high speed of 20 Hz/min for 30 minutes, adding 8 parts of 15-micron aluminum hypophosphite, 50 parts of 15-micron fused silica powder and 1.2 parts of 3-micron spherical alumina, continuously stirring for 60 minutes at the conditions of 50 Hz/min and 110 ℃, vacuumizing to remove bubbles, testing and packaging to obtain a component A; wherein the density of the aluminum hypophosphite is 1.5g/ml, and the particle size D50 is 15 mu m; the density of the silicon micro powder is 3g/ml, and the particle size D50 is 2 mu m; the alumina had a density of 3.0g/ml and a particle size D50 of 10 μm.
Example 11: this example prepares component a, including the following steps: adding 3 parts of methoxypolyethylene glycol glycidyl ether, 0.5 part of dodecylphenol with the molecular weight of 900 and 0.3 part of U carbon into 30 parts of the organosilicon modified epoxy resin prepared in example 2 and 5.2 parts of example 4, dispersing and premixing at a high speed of 20 Hz/min for 30 minutes, adding 8 parts of aluminum hypophosphite with the diameter of 15 mu m, 50 parts of spherical alumina with the diameter of 15 mu m and 3 parts of spheroidal alumina with the diameter of 3 mu m, continuously stirring for 60 minutes at the temperature of 110 ℃ at the speed of 50 Hz/min, vacuumizing to remove bubbles, testing and packaging to obtain a component A; wherein the density of the aluminum hypophosphite is 1.5g/ml, and the particle size D50 is 15 mu m; the alumina had a density of 3.0g/ml and a particle size D50 of 10 μm.
The A components obtained in examples 6 to 11 were subjected to the measurement of basic performance parameters, and the detailed test results are shown in Table 2.
TABLE 2 basic Performance parameter test results
Figure BDA0003995931400000111
Example 12: this example prepares component B, including the following steps: taking 30 parts of N- (3-aminopropyl) cyclohexylamine with an amine value of 1000mgKOH/g, 40 parts of polyetheramine D-230 with an amine value of 450mgKOH/g, 20 parts of 1,4 butanediol and 10 parts of HDI with NCO content of 23.5%, carrying out addition reaction for 3 hours at 80 ℃ in a reaction kettle with nitrogen protection, cooling, testing and packaging to obtain the component B.
Example 13: this example prepares component B, including the following steps: taking 30 parts of N- (3-aminopropyl) cyclohexylamine with amine value of 1000mgKOH/g, 40 parts of polyetheramine D-400 with amine value of 250mgKOH/g, 20 parts of polycaprolactone diol and 10 parts of HDI with NCO content of 23.5%, carrying out addition reaction for 3 hours at 80 ℃ in a reaction kettle with nitrogen protection, cooling, testing and packaging to obtain the component B.
Example 14: this example prepares component B, including the following steps: 40 parts of N- (3-aminopropyl) cyclohexylamine with an amine value of 1000mgKOH/g, 20 parts of polyetheramine D-2000 with an amine value of 60mgKOH/g, 25 parts of 1, 4-butanediol, 5 parts of dodecylphenol with a molecular weight of 300 and 10 parts of HDI with an NCO content of 23.5 percent are subjected to addition reaction for 3 hours at 80 ℃ in a reaction kettle with nitrogen protection, cooled, tested and packaged to obtain the component B.
Example 15: this example, the preparation of component B, includes the following steps: taking 20 parts of N- (3-aminopropyl) cyclohexylamine with the amine value of 1000mgKOH/g, 30 parts of polyetheramine D-230 with the amine value of 400mgKOH/g, 20 parts of polyetheramine D-2000 with the amine value of 60mgKOH/g, 20 parts of 1,4 butanediol and 10 parts of HDI with the NCO content of 23.5 percent, carrying out addition reaction in a reaction kettle with nitrogen protection at 80 ℃ for 3 hours, cooling, testing and packaging to obtain the component B.
Viscosity performance parameters were determined for the A-side components prepared in examples 12-15, and the detailed test results are shown in Table 3.
TABLE 3 measurement results of viscosity Performance parameters
Figure BDA0003995931400000121
The above a components (examples 8, 9, 11) and B components (examples 12, 13, 14, 15) were mixed and cured as required (a: B = 5) and left at room temperature for 25℃ for 24 hours, including the curing hardness (durometer), thermal conductivity (HODISK tester), flame retardancy (3 mm thick slab), curing shrinkage (density before and after curing is compared), salt fog test (5% nacl) for 500 hours, cold and heat cycle (-50 to 150℃ 1000 times), high temperature and high humidity 85℃ +85RH%, and the like, and the test results are shown in table 4.
TABLE 4 measurement results of comprehensive Property parameters
Figure BDA0003995931400000122
The combination of example 11 and example 13, tested by repeated experiments, gave the best overall performance. The resin synthesized by the organosilicon modified epoxy resin in the component A by selecting decyl glycidyl ether and KBM-602 as modifiers has the best flexibility, the addition amount in the component A is 30 parts, and the flame retardant property of the pouring sealant can be improved by a small amount of adduct of hydantoin epoxy resin and KBM-602, and the addition amount is 5.2 parts; methoxy polyethylene glycol glycidyl ether is used as an active diluent, and the addition amount is 3 parts, so that the viscosity of a system can be effectively adjusted, the addition amount of powder is increased, and the curing shrinkage rate is reduced; dodecyl phenol is selected as an accelerator, and the addition amount is 0.5 part; 0.3 part of color paste; the functional powder material selects high-temperature-resistant and high-stability aluminum hypophosphite with the addition of 8 parts, the heat conducting powder selects 10-20 microns of spherical alumina with the addition of 50 parts, a small amount of 1-3 microns of spherical alumina with fine particles is matched to play a role in anti-sedimentation, and the addition of 3 parts is adopted. The component B is aliphatic amine curing agent which selects N- (3-aminopropyl) cyclohexylamine, the addition amount is 30 parts, the addition amount of polyetheramine D-400 is 40 parts, the modifier is polyhexamethylene lactone diol, the addition amount is 20 parts, the bridging agent is HDI, the addition amount is 10 parts, and the aliphatic amine curing agent can react with amino groups in the curing agent and hydroxyl groups of polyhydric alcohols at the same time to achieve the characteristic of increasing flexibility.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner. Those skilled in the art can make many possible variations and modifications to the invention using the above disclosed technical means and teachings, or can modify equivalent embodiments with equivalent variations, without departing from the scope of the invention. Therefore, all equivalent changes made according to the shape, structure and principle of the present invention should be covered by the protection scope of the present invention without departing from the contents of the technical scheme of the present invention.

Claims (10)

1. The elastic epoxy glue for encapsulating the new energy photovoltaic inductor is characterized by comprising a component A and a component B which are mixed according to a volume ratio of 5-6;
the component A comprises the following components in parts by weight: 20 to 50 portions of organic silicon modified epoxy resin, 2 to 10 portions of reactive diluent, 0.5 to 5 portions of auxiliary agent and 40 to 70 portions of functional powder;
the component B comprises the following components in parts by weight: 10-30 parts of a crosslinking curing agent.
2. The elastic epoxy glue applied to encapsulation of the new energy photovoltaic inductor according to claim 1, wherein the organic silicon modified epoxy resin comprises, by mass, 10-50%: 30-70% of organosilicon compound and epoxy compound;
optionally, the amino content of the organic compound is 5-20%, and the silicon content is 1-10%;
the organic compound comprises but is not limited to one or a combination of N-2 aminoethyl-3-aminopropylmethyldimethoxysilane, gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane and gamma-aminopropyltriethoxysilane;
optionally, the epoxy value of the epoxy compound is 0.45 to 0.7eq/100g;
the epoxy compound includes but is not limited to one or a combination of several of methyl tetrahydrophthalic acid diglycidyl ester, decyl glycidyl ether, hydantoin epoxy resin, butadiene modified epoxy resin and bisphenol A epoxy resin E51.
3. The elastic epoxy glue applied to encapsulation of the new energy photovoltaic inductor as claimed in claim 2, wherein the reactive diluent is a low viscosity epoxy compound with an epoxy value of 0.3-0.7 eq/100g;
the reactive diluent comprises but is not limited to one or a combination of several of methoxypolyethylene glycol glycidyl ether, benzyl glycidyl ether, polypropylene glycol diglycidyl ether and propoxyglycerol triglycidyl ether.
4. The elastic epoxy glue applied to encapsulation of the new energy photovoltaic inductor according to claim 3, wherein the auxiliary agent comprises, by mass, 0.1-2%: 1-10%: 1-5% of surfactant, promoter and color paste;
optionally, the surfactant is polyoxyethylene polyoxypropylene pentaerythritol ether, polydimethylsiloxane, polyethylene glycol 200;
the accelerator is dodecylphenol, and the molecular weight of the dodecylphenol is 550-1000;
the color paste is 10% of carbon black.
5. The elastic epoxy glue applied to encapsulation of the new energy photovoltaic inductor according to claim 4, wherein the functional powder comprises the following components in parts by weight: 65-75 parts of flame retardant, 17-22 parts of heat-conducting powder and 17-22 parts of aluminum oxide;
optionally, the density of the flame retardant is 1.5-2.0 g/ml, and the particle size D50 is 5-20 μm;
the density of the heat conducting powder is 2.5-3.5 g/ml, and the particle size D50 is 1-3 mu m;
the density of the alumina is 3.0-4.0 g/ml, and the grain diameter D50 is 10-20 μm.
6. The elastic epoxy glue applied to the encapsulation of the new energy photovoltaic inductor as claimed in claim 5, wherein the flame retardant comprises one or a combination of more of ammonium polyphosphate of 10-20 μm, melamine of 5-15 μm, aluminum hypophosphite of 10-20 μm and aluminum hydroxide of 8-12 μm;
the heat conducting powder is fused silica micropowder with the particle size of 10-20 mu m;
the alumina comprises one or a combination of more of 1-3 μm spherical alumina and 10-20 μm spherical alumina.
7. The elastic epoxy glue applied to encapsulation of the new energy photovoltaic inductor according to claim 6, wherein the crosslinking curing agent comprises 20-40% by mass: 30-60%: 3-15% aliphatic amine curing agent, modifier and bridging agent;
optionally, the aliphatic amine curing agent comprises one or a combination of more of N- (3-aminopropyl) cyclohexylamine, polyetheramine D-230, polyetheramine D-400 and polyetheramine D-2000;
the modifier is one or a combination of several of dodecylphenol, polyhexamethylene lactone diol and 1,4 butanediol;
the bridging agent is HDI.
8. The elastic epoxy glue applied to the encapsulation of the new energy photovoltaic inductor in claim 7, wherein the amine value of the N- (3-aminopropyl) cyclohexylamine is 1000-1200 mgKOH/g, the amine value of the polyetheramine D-230 is 398-489 mgKOH/g, the amine value of the polyetheramine D-400 is 220-300 mgKOH/g, and the amine value of the polyetheramine D-2000 is 50-70 mgKOH/g;
the molecular weight of the dodecylphenol is 260-400, the molecular weight of the polycaprolactone diol is 550-1000, and the purity of the 1, 4-butanediol is 95-99.9%;
the NCO content of the HDI was 23.5%.
9. A preparation method of the elastic epoxy glue applied to new energy photovoltaic inductor potting is characterized in that the preparation method is used for preparing the elastic epoxy glue applied to new energy photovoltaic inductor potting according to any one of claims 1 to 8;
the preparation method comprises the following steps:
step 1, preparing organic silicon modified epoxy resin;
step 2, adding an active diluent and an auxiliary agent into the organic silicon modified epoxy resin, dispersing and premixing for 20-30 minutes at a high speed of 10-20 Hz/minute, adding functional powder, continuously stirring for 50-90 minutes at the conditions of 30-50 Hz/minute and 100-110 ℃, vacuumizing to remove bubbles, testing and packaging to obtain a component A;
and 3, taking the aliphatic amine curing agent, the accelerator and the HDI, carrying out addition reaction for 3 hours at 70-80 ℃ in a reaction kettle with nitrogen protection, cooling, testing and packaging to obtain the component B.
10. The elastic epoxy glue applied to encapsulation of the new energy photovoltaic inductor according to claim 6, wherein the step 1 specifically comprises: adding the epoxy compound into a reaction kettle, heating to 60-100 ℃, introducing nitrogen for protection, keeping 0.01-0.3 mPa atmospheric pressure, discharging humid air, slowly adding the organic silicon compound at the flow rate of 1-10 kg/min, carrying out premixing reaction for 90-120 min at the rotation speed of 10-50 Hz/min, and cooling to normal temperature to obtain the organic silicon modified epoxy resin.
CN202211593531.7A 2022-12-13 2022-12-13 Elastic epoxy adhesive applied to encapsulation of new energy photovoltaic inductor and preparation method thereof Pending CN115851195A (en)

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