CN111925763A - Anti-cracking epoxy pouring sealant with improved heat-conducting property - Google Patents
Anti-cracking epoxy pouring sealant with improved heat-conducting property Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
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- C08G59/5033—Amines aromatic
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- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
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Abstract
The invention discloses an anti-cracking epoxy pouring sealant with improved heat-conducting property, and relates to the technical field of electronic and electrical insulating materials. The epoxy resin toughening agent comprises 100 parts of liquid epoxy resin, 5-12 parts of a toughening agent, 30-50 parts of a curing agent, 700-1100 parts of inorganic powder and 0-15 parts of a pigment; the inorganic powder comprises a mixture of spherical silica powder with a median particle size of 25-35 mu m, spherical alumina powder A with a median particle size of more than 15 and less than or equal to 30 mu m, spherical alumina powder B with a median particle size of more than 5 and less than or equal to 15 mu m and spherical alumina powder C with a median particle size of more than 1 and less than or equal to 5 mu m, wherein the weight ratio of the spherical silica powder to the spherical alumina powder A to the spherical alumina powder B to the spherical alumina powder C is (5-20): 20-40): 30-60): 10-30. According to the inventionThe heat conductivity coefficient of the cured product of the high-heat-conductivity anti-cracking epoxy pouring sealant can reach 1.8-2.5W/(m.K), and the linear expansion coefficient can be controlled to be (10-25) multiplied by 10‑6K‑1Within the range of-35 ℃ to 180 ℃ and has the capability of resisting cold and hot shock.
Description
Technical Field
The invention relates to the technical field of electronic and electrical insulating materials, in particular to an anti-cracking epoxy pouring sealant with improved heat-conducting property.
Background
The epoxy pouring sealant has excellent sealing property, electrical insulation property, chemical corrosion resistance and weather resistance, and higher mechanical strength and thermal conductivity, so that the epoxy pouring sealant is widely used for the pouring protection treatment of important parts of electronic and electrical equipment or integrated components. The epoxy pouring sealant on the market at present has a plurality of varieties, can basically meet the requirements of most applications, but along with the development of new energy vehicles, magnetic suspension, electromagnetic ejection, aerospace and navigation and other technologies in recent years, the existing epoxy pouring sealant has some defects in some special occasions, particularly in application occasions with severe operation conditions, large workpiece sizes and complex internal insert geometric shapes. One of the outstanding disadvantages is that the encapsulated workpiece is easy to crack, and some cracks occur when the temperature is reduced to room temperature after the curing is finished; some of the encapsulating workpieces are subjected to repeated impact of high and low temperature or mechanical stress, internal stress of the encapsulating workpieces is accumulated continuously, cracks are developed continuously, and finally, the encapsulating sealant cracks to fail frequently.
Researches prove that the cracking resistance of the epoxy pouring sealant is closely related to the linear expansion coefficient of the epoxy pouring sealant after curing. The linear expansion coefficient of the metal insert made of iron, copper and the like is (10-25) multiplied by 10-6K-1In the range of (60-85). times.10 for unmodified polymers-6K-1The difference between the two is several times, and when the temperature of the workpiece frequently changes greatly, large internal stress is easily generated. In addition, the cracking resistance of the epoxy pouring sealant is closely related to the thermal conductivity coefficient of the epoxy pouring sealant after curing, and the higher thermal conductivity coefficient can improve the heat dissipation of electronic and electrical equipment and improve the distribution of a thermal field and mechanical stress in a workpiece, so that the cracking probability of the pouring workpiece is reduced.
In order to reduce the linear expansion coefficient of the pouring sealant and improve the heat conductivity coefficient of the pouring sealant, the adopted technical scheme is considered at the present stage to add more inorganic powder with smaller expansion coefficient and larger heat conductivity coefficient into the pouring sealant. However, studies have shown that when the amount of powder added reaches a certain amount, the viscosity of the sizing material increases sharply, thereby affecting the operability of the potting process, so that the desired amount of powder added cannot be achieved. Meanwhile, if the existing curing system of the epoxy resin is not necessarily improved, the adhesive force of the matrix resin to the inorganic powder is enhanced, and the excessive powder addition amount can cause the brittleness increase of a cured product, and the anti-cracking capability of the epoxy pouring sealant is weakened.
Disclosure of Invention
The invention solves the technical problems that epoxy pouring sealant in the prior art is poor in cracking resistance, the viscosity of sizing materials is increased to influence the operability of pouring and sealing, and the brittleness of the sizing materials is increased after curing to weaken the cracking resistance, and provides the high-thermal-conductivity cracking-resistant epoxy pouring sealant with the linear expansion coefficient similar to that of metal. The invention adopts the mixed powder of the spherical silicon micropowder, the spherical alumina powder A, the spherical alumina powder B and the spherical alumina powder C as the inorganic powder, and can greatly improve the addition of the inorganic powder without excessively increasing the viscosity of the sizing material. The heat conductivity coefficient of the cured product of the high-heat-conductivity anti-cracking epoxy pouring sealant can reach 1.8-2.5W/(m.K), and the linear expansion coefficient can be controlled to be (10-25) multiplied by 10-6K-1Within the range of-35 ℃ to 180 ℃ and has the capability of resisting cold and hot shock.
According to the purpose of the invention, the crack-resistant epoxy pouring sealant with improved heat-conducting property is provided, and comprises the following components in parts by weight: 100 parts of liquid epoxy resin, 5-12 parts of toughening agent, 30-50 parts of curing agent, 700-1100 parts of inorganic powder and 0-15 parts of pigment;
the inorganic powder comprises spherical silicon powder with the median particle size of 25-35 mu m, spherical alumina powder A with the median particle size of more than 15 and less than or equal to 30 mu m, spherical alumina powder B with the median particle size of more than 5 and less than or equal to 15 mu m and spherical alumina powder C with the median particle size of more than 1 and less than or equal to 5 mu m, wherein the weight ratio of the spherical silicon powder to the spherical alumina powder A to the spherical alumina powder B to the spherical alumina powder C is (5-20): 20-40): 30-60): 10-30.
Preferably, the curing agent is an aromatic amine to which a benzophenone, diphenyl ether, or diphenyl sulfone structure is attached.
Preferably, the curing agent is at least one of 4, 4' -diaminobenzophenone, 3,4' -diaminobenzophenone, 4' -diaminodiphenyl ether, 3,4' -diaminodiphenyl ether, 4' -diaminodiphenyl sulfone, 3 ' -diaminodiphenyl sulfone, and p, p ' -diaminotriphenyl diether.
Preferably, the liquid epoxy resin is at least one of a bisphenol a epoxy resin, a bisphenol F epoxy resin, and a cycloaliphatic epoxy resin.
Preferably, the toughening agent is an aliphatic glycidyl ether containing two or more epoxy groups.
Preferably, the toughening agent is at least one of hexanediol diglycidyl ether, butanediol diglycidyl ether, propylene glycol diglycidyl ether, ethylene glycol diglycidyl ether, diethylene glycol diglycidyl ether, neopentyl glycol diglycidyl ether, glycerol triglycidyl ether, and trimethylolpropane triglycidyl ether.
Preferably, the colorant is at least one of red iron oxide, carbon black, phthalocyanine blue, graphite, scarlet powder, green iron oxide, and blue iron oxide.
Generally, compared with the prior art, the above technical solution conceived by the present invention mainly has the following technical advantages:
(1) according to the invention, by referring to the Horsfield close packing principle, spherical inorganic powder with proper particle size distribution is adopted to replace inorganic powder used in the prior art, and spherical powder particles with smaller particle size are filled in gaps among spherical powder with larger particle size, so that the purpose of enabling the pouring sealant to have higher powder filling rate while reducing the specific surface area of the powder is achieved, and the viscosity of the rubber material tends to be minimized; the addition amount of the inorganic powder can be greatly increased without excessively increasing the viscosity of the rubber compound.
(2) The invention adopts the curing agent which can react with the epoxy resin at high temperature to replace the medium-temperature or room-temperature curing agents used in the prior art, such as methyl tetrahydrochysene anhydride, methyl hexahydrobenzene anhydride, phthalic anhydride, tetrahydrochysene anhydride, aniline, alkyl aniline, diaminodiphenylmethane, imidazole, fatty amine and the like, so that the temperature of the mixed material can be increased to 105-120 ℃, the pot life of more than 1h can be kept while the viscosity of the rubber material is effectively reduced, the filling and sealing operations of the mixed material, vacuum defoaming, rubber material transfer and the like can be conveniently completed, and meanwhile, excellent performance of the cured material can be obtained; and the adhesive force of the matrix resin to the inorganic powder is improved, so that the purpose of improving the performance of the cured product is achieved.
(3) Book (I)The heat conductivity coefficient of the cured product of the high-heat-conductivity anti-cracking epoxy pouring sealant can reach 1.8-2.5W/(m.K), and the linear expansion coefficient can be controlled to be (10-25) multiplied by 10-6K-1Within the range of-35 ℃ to 180 ℃ and has the capability of resisting cold and hot shock.
(4) The high-thermal-conductivity anti-cracking epoxy pouring sealant cured product also has excellent mechanical strength and electrical insulation performance, the thermal deformation temperature of the cured product is not lower than 180 ℃, the bending strength is not lower than 150MPa, and the electrical strength is not lower than 15 kV/mm.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The invention relates to an anti-cracking epoxy pouring sealant with improved heat-conducting property, which comprises the following components in parts by weight: 100 parts of liquid epoxy resin, 5-12 parts of toughening agent, 30-50 parts of curing agent, 700-1100 parts of inorganic powder and 0-15 parts of pigment;
the inorganic powder comprises spherical silicon powder with the median particle size of 25-35 mu m, spherical alumina powder A with the median particle size of more than 15 and less than or equal to 30 mu m, spherical alumina powder B with the median particle size of more than 5 and less than or equal to 15 mu m and spherical alumina powder C with the median particle size of more than 1 and less than or equal to 5 mu m, wherein the weight ratio of the spherical silicon powder to the spherical alumina powder A to the spherical alumina powder B to the spherical alumina powder C is (5-20): 20-40): 30-60): 10-30.
The pigment is at least one of iron oxide red, carbon black, phthalocyanine blue, graphite, scarlet powder, iron oxide green and iron oxide blue.
Example 1
In the embodiment, 100 parts of liquid epoxy resin, 6.4 parts of toughening agent, 36 parts of curing agent, 700 parts of inorganic powder and 8 parts of pigment;
the inorganic powder comprises a mixture of spherical silica powder with a median particle size of 30 micrometers, spherical alumina powder A with a median particle size of 20 micrometers, spherical alumina powder B with a median particle size of 10 micrometers and spherical alumina powder C with a median particle size of 5 micrometers, wherein the weight ratio of the spherical silica powder to the spherical alumina powder A to the spherical alumina powder B to the spherical alumina powder C is 15:30:40: 15.
The preparation of this example comprises the following steps:
(1) the spherical silica fine powder, the spherical alumina powder a, the spherical alumina powder B, and the spherical alumina powder C were put into a three-dimensional motion mixer, and mixed for 15 minutes at spindle speeds of 5, 10, and 20r/min, respectively, to obtain the inorganic powder used in this example.
(2) 10kg of JF-158 high-purity bisphenol A epoxy resin, 0.64kg of butanediol diglycidyl ether and 0.8kg of iron oxide red are put into a defoaming kettle equipped with a spiral-ribbon stirrer, the stirring is started, the temperature is raised to 100-145 ℃, 70kg of inorganic powder obtained in the step (1) in the embodiment is added in batches, and the powder is added each time until the viscosity of the sizing material is basically stable, and then the next batch of powder is added until the powder is completely added.
(3) Controlling the temperature of the material at 145-150 ℃, reducing the pressure to 0.1-0.2 kPa, and keeping the material until no bubbles are discharged.
(4) And reducing the temperature to 110-115 ℃ to remove the vacuum, adding 3.6kg of 3,4' -diaminobenzophenone curing agent, continuously reducing the pressure to 0.1-0.2 kPa, stirring for 15min, discharging, and immediately using for encapsulating treatment of electronic and electrical equipment.
The performance of the sizing material before curing and the performance test data after curing for 12h at 110 ℃, 2h at 150 ℃ and 5h at 180 ℃ in sequence are shown in Table 1.
Example 2
In the embodiment, 100 parts of liquid epoxy resin, 7.5 parts of toughening agent, 40 parts of curing agent, 800 parts of inorganic powder and 0 part of pigment;
the inorganic powder comprises a mixture of spherical silica powder with a median particle size of 30 micrometers, spherical alumina powder A with a median particle size of 20 micrometers, spherical alumina powder B with a median particle size of 10 micrometers and spherical alumina powder C with a median particle size of 5 micrometers, wherein the weight ratio of the spherical silica powder to the spherical alumina powder A to the spherical alumina powder B to the spherical alumina powder C is 10:30:30: 30.
The preparation of this example comprises the following steps:
(1) the spherical silica fine powder, the spherical alumina powder a, the spherical alumina powder B, and the spherical alumina powder C were put into a three-dimensional motion mixer, and mixed for 15 minutes at spindle speeds of 5, 10, and 20r/min, respectively, to obtain the inorganic powder used in this example.
(2) Adding 90 parts by weight of 4,4 '-diaminodiphenyl sulfone into a reaction kettle, heating to 180-185 ℃, keeping the temperature until the materials are molten, starting stirring, adding 10 parts by weight of 3,4' -diaminodiphenyl ether, stirring for 15min, cooling, discharging the materials into an iron pan when the temperature is reduced to 150 ℃, cooling to room temperature, crushing by using a crusher, sieving by using a 50-mesh standard sieve, and then filling into a plastic bag for later use as a curing agent used in the embodiment.
(3) 10kg of DER354 bisphenol F epoxy resin and 0.75kg of propylene glycol diglycidyl ether are put into a defoaming kettle equipped with a helical ribbon type stirrer, the stirring is started, the temperature is raised to 100-145 ℃, 80kg of inorganic powder is added in batches, and the next batch of powder is added after the powder is added each time until the viscosity of the sizing material is basically stable, until the powder is completely added.
(4) Controlling the temperature of the material at 145-150 ℃, reducing the pressure to 0.1-0.2 kPa, and keeping the material until no bubbles are discharged.
(5) And (3) reducing the temperature to 105-110 ℃, removing the vacuum, adding 4.0kg of the curing agent obtained in the step (2) of the embodiment, continuously reducing the pressure to 0.1-0.2 kPa, stirring for 15min, discharging, and immediately using for encapsulating treatment of electronic and electrical equipment.
The performance of the sizing material before curing and the performance test data after curing for 12h at 110 ℃, 2h at 150 ℃ and 5h at 180 ℃ in sequence are shown in Table 1.
Example 3
In the embodiment, the epoxy resin composition comprises 100 parts of liquid epoxy resin, 9 parts of a toughening agent, 42 parts of a curing agent, 920 parts of inorganic powder and 0 part of a pigment;
the inorganic powder comprises a mixture of spherical silica powder with a median particle size of 35 microns, spherical alumina powder A with a median particle size of 25 microns, spherical alumina powder B with a median particle size of 15 microns and spherical alumina powder C with a median particle size of 3 microns, wherein the weight ratio of the spherical silica powder to the spherical alumina powder A to the spherical alumina powder B to the spherical alumina powder C is 10:40:40: 10.
The preparation of this example comprises the following steps:
(1) the spherical silica fine powder, the spherical alumina powder a, the spherical alumina powder B, and the spherical alumina powder C were put into a three-dimensional motion mixer, and mixed for 15 minutes at spindle speeds of 5, 10, and 20r/min, respectively, to obtain the inorganic powder used in this example.
(2) The curing agent used in this example was the same as that obtained in step (2) of example 2.
(3) Putting 10kg of high-purity bisphenol F epoxy resin and 0.9kg of diethylene glycol diglycidyl ether into a deaeration kettle equipped with a spiral stirrer, stirring and heating to 100-145 ℃, adding 92kg of inorganic powder in batches, and adding the next batch of powder after the powder is added each time until the viscosity of the rubber material is basically stable until the powder is completely added.
(4) Controlling the temperature of the material at 145-150 ℃, reducing the pressure to 0.1-0.2 kPa, and keeping the material until no bubbles are discharged.
(5) And reducing the temperature to 105-110 ℃, removing the vacuum, adding 4.2kg of curing agent, continuously reducing the pressure to 0.1-0.2 kPa, stirring for 15min, discharging, and immediately using for encapsulating treatment of the electronic and electrical equipment.
The performance of the sizing material before curing and the performance test data after curing for 12h at 110 ℃, 2h at 150 ℃ and 5h at 180 ℃ in sequence are shown in Table 1.
Example 4
In the embodiment, 100 parts of liquid epoxy resin, 12 parts of toughening agent, 50 parts of curing agent, 1100 parts of inorganic powder and 15 parts of pigment are adopted;
the inorganic powder comprises a mixture of spherical silica powder with a median particle size of 35 microns, spherical alumina powder A with a median particle size of 30 microns, spherical alumina powder B with a median particle size of 15 microns and spherical alumina powder C with a median particle size of 5 microns, wherein the weight ratio of the spherical silica powder to the spherical alumina powder A to the spherical alumina powder B to the spherical alumina powder C is 20:40:30: 10.
The preparation of this example comprises the following steps:
(1) the spherical silica fine powder, the spherical alumina powder a, the spherical alumina powder B, and the spherical alumina powder C were put into a three-dimensional motion mixer, and mixed for 15 minutes at spindle speeds of 5, 10, and 20r/min, respectively, to obtain the inorganic powder used in this example.
(2) Adding 80 parts by weight of 4,4 '-diaminodiphenyl sulfone into a reaction kettle, heating to 180-185 ℃, keeping the temperature until the materials are molten, starting stirring, adding 20 parts by weight of 3,4' -diaminodiphenyl ketone, stirring for 15min, cooling, discharging the materials into an iron disc when the temperature is reduced to 150 ℃, cooling to room temperature, crushing by using a crusher, sieving by using a 50-mesh standard sieve, and filling into a plastic bag for later use as a curing agent used in the embodiment.
(3) Putting 10kg of high-purity bisphenol F epoxy resin, 1.2kg of butanediol diglycidyl ether and 1.5kg of carbon black into a defoaming kettle equipped with a spiral-belt stirrer, stirring and heating to 100-145 ℃, adding 110kg of inorganic powder in batches, and adding the next batch of powder after the powder is added each time until the viscosity of the sizing material is basically stable until the powder is completely added.
(4) Controlling the temperature of the material at 145-150 ℃, reducing the pressure to 0.1-0.2 kPa, and keeping the material until no bubbles are discharged.
(5) And reducing the temperature to 105-110 ℃, removing the vacuum, adding 5.0kg of curing agent, continuously reducing the pressure to 0.1-0.2 kPa, stirring for 15min, discharging, and immediately using for encapsulating treatment of the electronic and electrical equipment.
The performance of the sizing material before curing and the performance test data after curing for 12h at 110 ℃, 2h at 150 ℃ and 5h at 180 ℃ in sequence are shown in Table 1.
Example 5
In the embodiment, the epoxy resin is 100 parts, the toughening agent is 5 parts, the curing agent is 50 parts, the inorganic powder is 750 parts, and the pigment is 3 parts;
the inorganic powder comprises a mixture of spherical silica powder with a median particle size of 25 micrometers, spherical alumina powder A with a median particle size of 20 micrometers, spherical alumina powder B with a median particle size of 10 micrometers and spherical alumina powder C with a median particle size of 2 micrometers, wherein the weight ratio of the spherical silica powder to the spherical alumina powder A to the spherical alumina powder B to the spherical alumina powder C is 5:20:60: 15.
The preparation of this example comprises the following steps:
(1) the spherical silica fine powder, the spherical alumina powder a, the spherical alumina powder B, and the spherical alumina powder C were put into a three-dimensional motion mixer, and mixed for 15 minutes at spindle speeds of 5, 10, and 20r/min, respectively, to obtain the inorganic powder used in this example.
(2) Adding 90 parts by weight of 3,3 '-diaminodiphenyl sulfone into a reaction kettle, heating to 180-185 ℃, keeping the temperature until the materials are molten, starting stirring, adding 10 parts by weight of p, p' -diaminotriphenyl diether, stirring for 15min, cooling, discharging the materials into an iron plate when the temperature is reduced to 150 ℃, cooling to room temperature, crushing by using a crusher, sieving by using a 50-mesh standard sieve, and filling into a plastic bag for later use as a curing agent used in the embodiment.
(3) 10kg of CY 179 low-viscosity alicyclic epoxy resin, 0.5kg of diethylene glycol diglycidyl ether and 0.3kg of phthalocyanine blue are put into a defoaming kettle equipped with a spiral stirrer, stirring is started, the temperature is raised to 100-145 ℃, 75kg of inorganic powder is added in batches, and the powder is added each time until the viscosity of the sizing material is basically stable, and then the next batch of powder is added until the powder is completely added.
(4) Controlling the temperature of the material at 145-150 ℃, reducing the pressure to 0.1-0.2 kPa, and keeping the material until no bubbles are discharged.
(5) And reducing the temperature to 105-110 ℃, removing the vacuum, adding 5.0kg of curing agent, continuously reducing the pressure to 0.1-0.2 kPa, stirring for 15min, discharging, and immediately using for encapsulating treatment of the electronic and electrical equipment.
The performance of the sizing material before curing and the performance test data after curing for 12h at 110 ℃, 2h at 150 ℃ and 5h at 180 ℃ in sequence are shown in Table 1.
Example 6
In the embodiment, 100 parts of liquid epoxy resin, 6.8 parts of toughening agent, 30 parts of curing agent, 950 parts of inorganic powder and 0 part of pigment are adopted;
the inorganic powder comprises a mixture of spherical silica powder with a median particle size of 25 micrometers, spherical alumina powder A with a median particle size of 15 micrometers, spherical alumina powder B with a median particle size of 5 micrometers and spherical alumina powder C with a median particle size of 1 micrometer, wherein the weight ratio of the spherical silica powder to the spherical alumina powder A to the spherical alumina powder B to the spherical alumina powder C is 20:35:35: 10.
The preparation of this example comprises the following steps:
(1) the spherical silica fine powder, the spherical alumina powder a, the spherical alumina powder B, and the spherical alumina powder C were put into a three-dimensional motion mixer, and mixed for 15 minutes at spindle speeds of 5, 10, and 20r/min, respectively, to obtain the inorganic powder used in this example.
(2) The curing agent used in this example was the same as that obtained in step (2) of example 4.
(3) Putting 7kg of high-purity bisphenol A epoxy resin, 3kg of high-purity bisphenol F epoxy resin and 0.68kg of ethylene glycol diglycidyl ether into a defoaming kettle equipped with a spiral-ribbon stirrer, stirring and heating to 100-145 ℃, adding 95kg of inorganic powder in batches, and adding the next batch of powder after the powder is added each time until the viscosity of the sizing material is basically stable until the powder is completely added.
(4) Controlling the temperature of the material at 145-150 ℃, reducing the pressure to 0.1-0.2 kPa, and keeping the material until no bubbles are discharged.
(5) And reducing the temperature to 105-110 ℃, removing the vacuum, adding 3.0kg of curing agent, continuously reducing the pressure to 0.1-0.2 kPa, stirring for 15min, discharging, and immediately using for encapsulating treatment of the electronic and electrical equipment.
The performance of the sizing material before curing and the performance test data after curing for 12h at 110 ℃, 2h at 150 ℃ and 5h at 180 ℃ in sequence are shown in Table 1.
The testing method of the main performance of the rubber compound obtained in each example is as follows:
the viscosity of the compound before curing was measured with a rotational viscometer.
Measuring the thermal conductivity coefficient of the cured product at 105 ℃ by a steady-state heat flow method according to GB/T29313-2012; measuring the linear expansion coefficient by a German NETZSCH DIL402C linear expansion instrument, wherein the heating rate is 2 ℃/min; measuring the thermal deformation temperature according to a GB/T1634.2-2004A method, horizontally placing the sample, and increasing the temperature at a rate of 2 ℃/min; the impact strength is measured according to GB/T1043.1-2008 by adopting a simply supported beam method, and the sample has no gap; the bending strength is measured according to GB/T9341-2000, and the test speed is 2 mm/min; measuring tensile strength according to GB/T1040.2-2006, adopting 1A type dumbbell type sample, and its tensile speed is 1 mm/min; measuring the electrical strength under power frequency by a continuous pressure increasing method according to GB/T1408.1-2006, wherein the thickness of the sample is 1.0 mm; measuring the density at 23 + -2 deg.C by a dipping method according to GB/T1033.1-2008A method; the cold and hot impact test refers to GB/T15023-. The insert consists of an M12 hexagonal flat-headed steel screw and a steel hexagonal nut which is fully engaged and tightened on the bottom of the screw. The procedure for the cold-hot impact test was: and (3) putting a group of 5 bolt and nut insert samples into a 180 ℃ blast oven, keeping the samples for 1h, taking out the samples, immediately putting the samples into a mixture of anti-freezing solution and dry ice, wherein the volume of the mixture is not less than 10L, the temperature of the mixture is constant between-35 ℃ and-40 ℃, keeping the mixture for 10min, taking out the anti-freezing solution on the surface of the sample, wiping the sample, and observing whether the sample cracks, wherein the test period is the same. The above operation was repeated until cracking occurred in 2 out of 5 specimens.
The results of the tests on the main properties of the compounds obtained in the above examples are shown in Table 1.
Table 1 results of testing the main properties of the compounds obtained in the examples
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (7)
1. The cracking-resistant epoxy pouring sealant with improved heat-conducting property is characterized by comprising the following components in parts by weight: 100 parts of liquid epoxy resin, 5-12 parts of toughening agent, 30-50 parts of curing agent, 700-1100 parts of inorganic powder and 0-15 parts of pigment;
the inorganic powder comprises spherical silica powder with a median particle size of 25-35 mu m, spherical alumina powder A with a median particle size of more than 15 and less than or equal to 30 mu m, spherical alumina powder B with a median particle size of more than 5 and less than or equal to 15 mu m and spherical alumina powder C with a median particle size of more than 1 and less than or equal to 5 mu m, wherein the weight ratio of the spherical silica powder to the spherical alumina powder A to the spherical alumina powder B to the spherical alumina powder C is (5-20): 20-40): 30-60): 10-30.
2. The crack-resistant epoxy potting adhesive with improved thermal conductivity of claim 1, wherein the curing agent is an aromatic amine having a benzophenone, diphenyl ether or diphenyl sulfone structure attached thereto.
3. The crack-resistant epoxy potting adhesive with improved thermal conductivity of claim 2, wherein the curing agent is at least one of 4, 4' -diaminobenzophenone, 3,4' -diaminobenzophenone, 4' -diaminodiphenyl ether, 3,4' -diaminodiphenyl ether, 4' -diaminodiphenyl sulfone, 3 ' -diaminodiphenyl sulfone and p, p ' -diaminotriphenyl diether.
4. The crack-resistant epoxy potting adhesive with improved thermal conductivity of claim 1, wherein the liquid epoxy resin is at least one of bisphenol a epoxy resin, bisphenol F epoxy resin and cycloaliphatic epoxy resin.
5. The crack-resistant epoxy potting adhesive with improved thermal conductivity of claim 1, wherein the toughening agent is an aliphatic glycidyl ether containing two or more epoxy groups.
6. The crack-resistant epoxy potting adhesive with improved thermal conductivity of claim 5, wherein the toughening agent is at least one of hexanediol diglycidyl ether, butanediol diglycidyl ether, propylene glycol diglycidyl ether, ethylene glycol diglycidyl ether, diethylene glycol diglycidyl ether, neopentyl glycol diglycidyl ether, glycerol triglycidyl ether, trimethylolpropane triglycidyl ether.
7. The crack-resistant epoxy potting adhesive with improved thermal conductivity of claim 1, wherein the colorant is at least one of red iron oxide, carbon black, phthalocyanine blue, graphite, scarlet powder, green iron oxide, and blue iron oxide.
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