CN111057490A - Preparation method of high-adhesion polyacrylate-based pouring sealant - Google Patents
Preparation method of high-adhesion polyacrylate-based pouring sealant 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
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/062—Copolymers with monomers not covered by C09J133/06
- C09J133/068—Copolymers with monomers not covered by C09J133/06 containing glycidyl groups
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08L2203/00—Applications
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- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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Abstract
The invention relates to a preparation method of a high-adhesion polyacrylate-based pouring sealant, belonging to the technical field of adhesive materials. The polyacrylate is a polymer which is prepared by taking an acrylate monomer containing a hydrogen ester group as a main material and copolymerizing the acrylate monomer with an unsaturated olefin monomer, the polyacrylate has wide material source, simple preparation process, quick drying and forming, good transparency, good bonding performance on various materials, excellent weather resistance, water resistance and chemical resistance, particularly excellent bonding performance on hydrophobic surface materials, excellent aging resistance of the polyacrylate, convenient use and good durability of a bonded joint, the polyacrylate can be used for bonding materials such as metal, plastics and the like, the bonding performance is excellent, and the pouring sealant prepared by taking the polyacrylate as a raw material can effectively improve the bonding capability on metal plates and plastic plates.
Description
Technical Field
The invention relates to a preparation method of a high-adhesion polyacrylate-based pouring sealant, belonging to the technical field of adhesive materials.
Background
In the world, science and technology are changing day by day, and human society has also entered the era of electronic information. With the improvement of electronic technical requirements in the market and the intensive research of people, electronic components and logic circuits tend to be more compact and miniaturized, and therefore, higher requirements are put on the stability of electric appliances. In the electronic industry, packaging is one of the necessary processes for electronic components, and packaging is an operation process for reasonably arranging, assembling, bonding, connecting, isolating from the environment, protecting and the like each component constituting an electronic device or an integrated circuit according to the specified requirements. The electronic element is encapsulated by encapsulation so as to effectively prevent the invasion of moisture, dust and harmful gas to the electronic element, slow down vibration, prevent external force damage and stabilize element parameters, and minimize the external adverse effect. However, the increase in power of electronic devices and the densification and miniaturization of electronic components and logic circuits also make heat dissipation of electronic components difficult, and electronic potting adhesives are required to have good heat conduction and insulation properties. If the heat can not be conducted in time, local heat concentration is easy to form, and then components and assemblies can be damaged, so that the normal operation of the system is influenced. With the continuous maturity of the process, the heat conduction electronic potting plays an increasingly important role in the protection of equipment, especially in the protection of high-voltage high-power components and assemblies. The application of the heat conduction material can effectively diffuse the heat generated by the circuit, prevent the heat of the circuit from concentrating and the temperature from rising, and further prolong the service life of the electronic device. With the application and development of the electric circuit integration technology, the heat dissipation of the device is more and more difficult, the heat dissipation of the electronic device is particularly important, and the heat conduction material becomes an essential auxiliary material for the application of the electronic device.
With the progress of science and technology, highly integrated electronic circuits are rapidly developed, wherein micro-transformers play a very important role, and in the application of micro-transformers, the bonding and fixing process is a difficult problem which is needed to be solved urgently. At present, most micro transformers are fixed on a circuit board through reflow soldering equipment, and a heating circuit is arranged in the equipment, so that air or nitrogen can be heated to a high enough temperature and then blown to the circuit board with a mounted element, and solder on two sides of the element is melted and bonded with a main board. The process is easy to control the temperature, can avoid oxidation in the welding process, improves the welding wetting force, accelerates the wetting speed, reduces the generation of tin balls, avoids bridging and obtains better welding quality. If the process is adopted, the miniature transformer needs to be filled with a heat-resistant bonding pouring sealant so as to achieve the effect of fixing protection. The transformer is widely applied in daily production life, the transformer cannot be used in daily life and production without time and place, and in the use process of the transformer, the potting adhesive in the transformer is large in using amount and plays a great role in the use performance of the transformer, so that the quality of the potting adhesive in the transformer greatly determines the quality of the transformer. At the end of the 30's of the 20 th century, Haider, Inc. of Corning glass, USA, Panode, Inc. of general electric company, made a lot of fundamental work around the hydrolytic condensation reaction of various silane monomers and heat-resistant silicone resins. Heidel successfully synthesized the first organic product, a silicone insulating varnish for electrical insulation. The silicone resin has excellent heat resistance, dielectric property and weather resistance, lower thermal expansion coefficient and light weight, and is very suitable for shallow potting of small transformers. The pouring sealant for the small-sized transformer is prepared by adopting bisphenol A epoxy resin, polyether polyol, aluminum hydroxide, dimethyl tetrahydrophthalic anhydride, polyester resin and the like by LuoLiang et al, has high-temperature vulcanization speed and high bonding performance, but has poor high-temperature resistance, and is suitable for a reflow soldering process.
At present, the heat-conducting pouring sealant used in China mainly comprises three types of epoxy resin, polyurethane and organic silicon, wherein the former two types of heat-conducting pouring sealants have the advantages of better adhesive property to a base material, but have the defect of low use temperature, and if the heat-conducting pouring sealant is used in a high-power supply, a relay and a sensor or an electronic appliance needing high-temperature use, the pouring sealant can be pulverized and lose elasticity for a long time. The organic silicon heat-conducting pouring sealant has the advantages of high temperature resistance, small linear expansion coefficient and the like, can be used at a high temperature of 230 ℃ for a long time, but has poor bonding capability to a base material and almost no bonding capability. The organosilicon pouring sealant on the market at present has poor adhesive capacity, and has almost no adhesive capacity particularly for aluminum and PC boards.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the problems that the organic silicon pouring sealant on the market has poor bonding capability and almost has no bonding capability to aluminum and PC plates, the preparation method of the high-bonding polyacrylate-based pouring sealant is provided.
In order to solve the technical problems, the invention adopts the following technical scheme:
(1) adding carbon five petroleum resin into cyclohexane, and stirring at the normal temperature at the rotating speed of 240-280 r/min for 20-30 min to obtain a carbon five petroleum resin solution;
(2) adding polyacrylate powder, epoxy resin, polysulfone resin and polyethylene glycol into N, N-dimethylformamide, and stirring at the normal temperature at the rotating speed of 280-300 r/min for 30-40 min to obtain a polymer solution;
(3) placing aluminum nitride, zinc oxide and silicon nitride in a stirrer, and stirring and mixing at the normal temperature at the rotating speed of 180-200 r/min for 10-20 min to obtain a powder filler;
(4) adding the carbon five petroleum resin solution and the powder filler into the polymer solution, stirring at the rotating speed of 600-800 r/min for 30-40 min at normal temperature, then placing in an ultrasonic dispersion machine, and performing ultrasonic dispersion for 20-30 min at normal temperature to obtain the high-adhesion polyacrylate-based pouring sealant.
The weight parts of the polyacrylate powder, the epoxy resin, the polysulfone resin, the carbon penta-petroleum resin, the aluminum nitride, the zinc oxide, the silicon nitride, the polyethylene glycol, the cyclohexane and the N, N-dimethylformamide are 60-80 parts of the polyacrylate powder, 30-40 parts of the epoxy resin, 18-24 parts of the polysulfone resin, 12-16 parts of the carbon penta-petroleum resin, 18-24 parts of the aluminum nitride, 6-8 parts of the zinc oxide, 6-8 parts of the silicon nitride, 3-4 parts of the polyethylene glycol, 30-40 parts of the cyclohexane and 120-160 parts of the N, N-dimethylformamide.
And (4) the power of ultrasonic dispersion in the step (4) is 400-500W.
The concrete preparation steps of the polyacrylate powder in the step (2) are as follows:
(1) adding butyl acrylate, methyl methacrylate, hydroxypropyl methacrylate and glycidyl methacrylate into acrylic acid, and stirring at the rotating speed of 160-180 r/min for 2-4 min at normal temperature to obtain a mixed monomer;
(2) adding sodium dodecyl benzene sulfonate and sodium carbonate into deionized water, stirring for 10-12 min at a rotating speed of 180-200 r/min under a water bath condition of 70-80 ℃, and preserving heat to obtain a surfactant solution;
(3) adding 1/10 mixed monomer and 1/3 sodium persulfate into a surfactant solution, and stirring and reacting for 10-12 min at a rotating speed of 200-240 r/min under a water bath condition of 70-80 ℃ to obtain seed emulsion;
(4) slowly adding the residual 9/10 mixed monomer into the seed emulsion, adding the residual 2/3 sodium persulfate, and reacting for 1-2 hours at the rotating speed of 240-280 r/min under the water bath condition of 80-90 ℃ to obtain mixed emulsion;
(5) cooling the mixed emulsion to room temperature, and adjusting the pH value to 7 to obtain polyacrylate emulsion;
(6) standing the polyacrylate emulsion for 1-2 hours at normal temperature, drying in an oven at 80-100 ℃ for 20-24 hours, and cooling at normal temperature to obtain polyacrylate powder.
The weight parts of the acrylic acid, the butyl acrylate, the methyl methacrylate, the hydroxypropyl methacrylate, the glycidyl methacrylate, the sodium persulfate, the sodium dodecyl benzene sulfonate, the sodium carbonate and the deionized water are 30-40 parts of acrylic acid, 20-30 parts of butyl acrylate, 18-24 parts of methyl methacrylate, 6-8 parts of hydroxypropyl methacrylate, 8-12 parts of glycidyl methacrylate, 0.3-0.6 part of sodium persulfate, 0.2-0.4 part of sodium dodecyl benzene sulfonate, 4-6 parts of sodium carbonate and 100-120 parts of deionized water.
And (4) adding the mixed monomer at a rate of 30-40 mL/min.
And (5) adopting ammonia water with the mass fraction of 1% for pH adjustment.
The specific preparation steps of the aluminum nitride in the step (3) are as follows:
(1) adding potassium chloride, calcium chloride and ammonium chloride into aluminum powder, placing the aluminum powder into a ball mill, introducing argon at the speed of 80-100 mL/min for protection, and ball-milling at the rotating speed of 200-250 r/min for 20-24 h at normal temperature to obtain precursor powder;
(2) placing the precursor powder in a tubular atmosphere furnace, introducing nitrogen at the speed of 100-120 mL/min for protection, calcining at the temperature of 1000-1200 ℃ for 2-4 h, and cooling to room temperature along with the furnace to obtain massive aluminum nitride;
(3) and (3) placing the blocky aluminum nitride in a ball mill, and stirring at the normal temperature at the rotating speed of 300-340 r/min for 20-24 h to obtain the aluminum nitride powder.
The aluminum powder, the ammonium chloride, the potassium chloride and the calcium chloride are 40-50 parts by weight of aluminum powder, 60-80 parts by weight of ammonium chloride, 0.2-0.4 part by weight of potassium chloride and 0.3-0.6 part by weight of calcium chloride.
Compared with other methods, the method has the beneficial technical effects that:
(1) the high-adhesion polyacrylate-based pouring sealant is prepared by taking polyacrylate as a raw material, wherein polyacrylate is a polymer which is prepared by taking an acrylate monomer containing a hydrogen ester group as a main material and copolymerizing the acrylate monomer with an unsaturated olefin monomer, the polyacrylate has wide material source, simple preparation process, quick drying and forming, good transparency, good adhesion performance to various materials, excellent weather resistance, water resistance and chemical resistance, particularly excellent adhesion performance to hydrophobic surface materials, excellent aging resistance of polyacrylate, convenient use and good durability of an adhesion joint, polyacrylate can be used for adhesion of materials such as metal and plastic, and the adhesion performance is excellent, and the pouring sealant prepared by taking polyacrylate as the raw material can effectively improve the adhesion capacity to metal plates and plastic plates;
(2) the invention prepares the high-adhesion polyacrylate-based pouring sealant by adding the epoxy resin and the polysulfone resin, wherein the molecular chain of the polysulfone resin is a linear macromolecular compound which is formed by connecting an isopropylene group, an ether bond and a sulfone group, and the isopropylene group, the ether bond and the sulfone group have different influences on the performance of the polysulfone: the ether bond can increase the flexibility of a molecular chain more than an isopropylidene group, the thermal stability can be improved, phenyl groups at two ends of the ether bond can rotate around the inside of the ether bond, the toughness of the polymer is increased, oxygen atoms on the diphenylene sulfone group are symmetrical, the polarity is smaller, sulfur atoms on a main chain are in the highest oxidation state, in addition, the sulfone group and two adjacent benzene rings form a high-conjugated diphenylsulfone structure, the sulfone group has the tendency of attracting electrons from the adjacent benzene rings, so that the number of the electrons of the benzene rings is insufficient, the high-resonance structure of the diphenylene sulfone group also provides thermal stability, the high-resonance structure also enables the diphenylene sulfone group to have high-strength chemical bonds, the stability of the substance in an oxidation environment enables the substance to have the strong tendency of resisting the loss of electrons and changing into an oxide, the whole diphenylene sulfone group has the inherent oxidation resistance, and therefore, a large amount of accompanying heat or ionizing radiation can be dissipated, the polyphenylene sulfone group endows the whole polymer molecule with inherent characteristics of thermal stability, oxidation resistance, rigidity and the like, the polysulfone resin is added to effectively improve the thermal stability of the pouring sealant, the epoxy resin is a polymer resin with outstanding performance, and the polyphenylene sulfone group has the main characteristics of strong adhesive force, good electrical insulation, easy obtainment and suitability for mass use, polar groups such as light groups, epoxy groups and the like in the structure of the epoxy resin can generate secondary valence bonds and hydrogen bonds with a plurality of polar surfaces, has extremely strong adhesive capacity, and the epoxy groups and the light groups can react with functional groups of other compounds to form a cross-linked network structure, thereby obtaining higher mechanical strength, and the adhesive capacity of the pouring sealant can be effectively improved by adding the epoxy resin.
Detailed Description
Respectively weighing 30-40 parts of acrylic acid, 20-30 parts of butyl acrylate, 18-24 parts of methyl methacrylate, 6-8 parts of hydroxypropyl methacrylate, 8-12 parts of glycidyl methacrylate, 0.3-0.6 part of sodium persulfate, 0.2-0.4 part of sodium dodecyl benzene sulfonate, 4-6 parts of sodium carbonate and 100-120 parts of deionized water according to parts by weight, adding butyl acrylate, methyl methacrylate, hydroxypropyl methacrylate and glycidyl methacrylate into acrylic acid, stirring at the rotating speed of 160-180 r/min for 2-4 min at normal temperature to obtain a mixed monomer, adding sodium dodecyl benzene sulfonate and sodium carbonate into deionized water, stirring at the rotating speed of 180-200 r/min under the water bath condition of 70-80 ℃ for 10-12 min, preserving heat to obtain a surfactant solution, adding 1/10 mixed monomer and 1/3 parts of sodium persulfate into the surfactant solution, stirring and reacting for 10-12 min at a rotating speed of 200-240 r/min under a water bath condition of 70-80 ℃ to obtain seed emulsion, slowly adding the rest 9/10 mixed monomer into the seed emulsion at a dropping speed of 30-40 mL/min, adding the rest 2/3 sodium persulfate, reacting for 1-2 h at a rotating speed of 240-280 r/min under a water bath condition of 80-90 ℃ to obtain mixed emulsion, cooling the mixed emulsion to room temperature, dropping ammonia water with a mass fraction of 1% to adjust the pH value to 7 to obtain polyacrylate emulsion, standing the polyacrylate emulsion at normal temperature for 1-2 h, drying in an oven at 80-100 ℃ for 20-24 h, and cooling at normal temperature to obtain polyacrylate powder; respectively weighing 40-50 parts of aluminum powder, 60-80 parts of ammonium chloride, 0.2-0.4 part of potassium chloride and 0.3-0.6 part of calcium chloride according to parts by weight, adding the potassium chloride, the calcium chloride and the ammonium chloride into the aluminum powder, placing the aluminum powder in a ball mill, introducing argon at a rate of 80-100 mL/min for protection, carrying out ball milling at a rotating speed of 200-250 r/min for 20-24 h at normal temperature to obtain precursor powder, placing the precursor powder in a tubular atmosphere furnace, introducing nitrogen at a rate of 100-120 mL/min for protection, carrying out heat preservation and calcination at a temperature of 1000-1200 ℃ for 2-4 h, cooling the furnace to room temperature to obtain blocky aluminum nitride, placing the blocky aluminum nitride in the ball mill, and stirring at the rotating speed of 300-340 r/min for 20-24 h at normal temperature to obtain aluminum nitride powder; then, respectively weighing 60-80 parts by weight of polyacrylate powder, 30-40 parts by weight of epoxy resin, 18-24 parts by weight of polysulfone resin, 12-16 parts by weight of carbon-penta petroleum resin, 18-24 parts by weight of aluminum nitride, 6-8 parts by weight of zinc oxide, 6-8 parts by weight of silicon nitride, 3-4 parts by weight of polyethylene glycol, 30-40 parts by weight of cyclohexane and 120-160 parts by weight of N, N-dimethylformamide, adding the carbon-penta petroleum resin into the cyclohexane, stirring at the normal temperature at the rotating speed of 240-280 r/min for 20-30 min to obtain a carbon-penta petroleum resin solution, adding the polyacrylate powder, the epoxy resin, the polysulfone resin and the polyethylene glycol into the N, N-dimethylformamide, stirring at the normal temperature at the rotating speed of 280-300 r/min for 30-40 min to obtain a polymer solution, placing the aluminum nitride, the zinc oxide and the silicon nitride into a stirrer, stirring and mixing at the normal temperature at the rotating speed of 180-200 r, and (3) obtaining a powder filler, adding the carbon five petroleum resin solution and the powder filler into the polymer solution, stirring at the normal temperature at the rotating speed of 600-800 r/min for 30-40 min, then placing in an ultrasonic dispersion machine, and ultrasonically dispersing at the normal temperature at the power of 400-500W for 20-30 min to obtain the high-adhesion polyacrylate-based pouring sealant.
Example 1
Respectively weighing 30 parts of acrylic acid, 20 parts of butyl acrylate, 18 parts of methyl methacrylate, 6 parts of hydroxypropyl methacrylate, 8 parts of glycidyl methacrylate, 0.3 part of sodium persulfate, 0.2 part of sodium dodecyl benzene sulfonate, 4 parts of sodium carbonate and 100 parts of deionized water according to parts by weight, adding the butyl acrylate, the methyl methacrylate, the hydroxypropyl methacrylate and the glycidyl methacrylate into the acrylic acid, stirring for 2min at the rotating speed of 160r/min at normal temperature to obtain a mixed monomer, adding the sodium dodecyl benzene sulfonate and the sodium carbonate into the deionized water, stirring for 10min at the rotating speed of 180r/min under the water bath condition of 70 ℃, preserving heat to obtain a surfactant solution, adding the 1/10 mixed monomer and the 1/3 sodium persulfate into the surfactant solution, stirring and reacting for 10min at the rotating speed of 200r/min under the water bath condition of 70 ℃, obtaining seed emulsion, slowly adding the residual 9/10 mixed monomer into the seed emulsion at the dropping rate of 30mL/min, adding the residual 2/3 sodium persulfate, reacting for 1h at the rotating speed of 240r/min under the water bath condition of 80 ℃ to obtain mixed emulsion, cooling the mixed emulsion to room temperature, dropping ammonia water with the mass fraction of 1% to adjust the pH value to 7 to obtain polyacrylate emulsion, standing the polyacrylate emulsion for 1h at normal temperature, drying for 20h in an oven at 80 ℃, and cooling at normal temperature to obtain polyacrylate powder; respectively weighing 40 parts of aluminum powder, 60 parts of ammonium chloride, 0.2 part of potassium chloride and 0.3 part of calcium chloride according to parts by weight, adding the potassium chloride, the calcium chloride and the ammonium chloride into the aluminum powder, placing the aluminum powder in a ball mill, introducing argon at the speed of 80mL/min for protection, ball-milling at the normal temperature at the rotating speed of 200r/min for 20h to obtain precursor powder, placing the precursor powder in a tubular atmosphere furnace, introducing nitrogen at the speed of 100mL/min for protection, carrying out heat preservation and calcination at the temperature of 1000 ℃ for 2h, cooling to the room temperature along with the furnace to obtain blocky aluminum nitride, placing the blocky aluminum nitride in the ball mill, and stirring at the normal temperature at the rotating speed of 300r/min for 20h to obtain aluminum nitride powder; respectively weighing 60 parts of polyacrylate powder, 30 parts of epoxy resin, 18 parts of polysulfone resin, 12 parts of carbon-five petroleum resin, 18 parts of aluminum nitride, 6 parts of zinc oxide, 6 parts of silicon nitride, 3 parts of polyethylene glycol, 30 parts of cyclohexane and 120 parts of N, N-dimethylformamide, adding the carbon-five petroleum resin into the cyclohexane, stirring at 240r/min for 20min at normal temperature to obtain a carbon-five petroleum resin solution, adding the polyacrylate powder, the epoxy resin, the polysulfone resin and the polyethylene glycol into the N, N-dimethylformamide, stirring at 280r/min at normal temperature for 30min to obtain a polymer solution, placing the aluminum nitride, the zinc oxide and the silicon nitride into a stirrer, stirring and mixing at 180r/min at normal temperature for 10min to obtain a powder filler, adding the carbon-five petroleum resin solution and the powder filler into the polymer solution, stirring the mixture for 30min at the normal temperature at the rotating speed of 600r/min, then placing the mixture in an ultrasonic dispersion machine, and ultrasonically dispersing the mixture for 20min at the normal temperature at the power of 400W to obtain the high-adhesion polyacrylate-based pouring sealant.
Example 2
Respectively weighing 35 parts of acrylic acid, 25 parts of butyl acrylate, 21 parts of methyl methacrylate, 7 parts of hydroxypropyl methacrylate, 10 parts of glycidyl methacrylate, 0.5 part of sodium persulfate, 0.3 part of sodium dodecyl benzene sulfonate, 5 parts of sodium carbonate and 110 parts of deionized water according to parts by weight, adding the butyl acrylate, the methyl methacrylate, the hydroxypropyl methacrylate and the glycidyl methacrylate into the acrylic acid, stirring for 3min at the rotating speed of 170r/min at normal temperature to obtain a mixed monomer, adding the sodium dodecyl benzene sulfonate and the sodium carbonate into the deionized water, stirring for 11min at the rotating speed of 190r/min under the water bath condition of 75 ℃, preserving heat to obtain a surfactant solution, adding the 1/10 mixed monomer and the 1/3 sodium persulfate into the surfactant solution, stirring and reacting for 11min at the rotating speed of 220r/min under the water bath condition of 75 ℃, obtaining seed emulsion, slowly adding the residual 9/10 mixed monomer into the seed emulsion at the dropping rate of 35mL/min, adding the residual 2/3 sodium persulfate, reacting for 1.5h at the rotating speed of 260r/min under the condition of water bath at the temperature of 85 ℃ to obtain mixed emulsion, cooling the mixed emulsion to room temperature, dropping ammonia water with the mass fraction of 1% to adjust the pH value to 7 to obtain polyacrylate emulsion, standing the polyacrylate emulsion for 1.5h at the room temperature, drying the polyacrylate emulsion in a drying oven at the temperature of 90 ℃ for 22h, and cooling at the normal temperature to obtain polyacrylate powder; respectively weighing 45 parts of aluminum powder, 70 parts of ammonium chloride, 0.3 part of potassium chloride and 0.5 part of calcium chloride according to parts by weight, adding the potassium chloride, the calcium chloride and the ammonium chloride into the aluminum powder, placing the aluminum powder in a ball mill, introducing argon at the speed of 90mL/min for protection, ball-milling the aluminum powder at the normal temperature at the rotating speed of 225r/min for 22h to obtain precursor powder, placing the precursor powder in a tubular atmosphere furnace, introducing nitrogen at the speed of 110mL/min for protection, carrying out heat preservation and calcination at the temperature of 1100 ℃ for 3h, cooling the furnace to the room temperature to obtain blocky aluminum nitride, placing the blocky aluminum nitride in the ball mill, and stirring the blocky aluminum nitride at the normal temperature at the rotating speed of 320r/min for 22h to obtain aluminum; respectively weighing 70 parts of polyacrylate powder, 35 parts of epoxy resin, 21 parts of polysulfone resin, 14 parts of carbon-five petroleum resin, 21 parts of aluminum nitride, 7 parts of zinc oxide, 7 parts of silicon nitride, 3.5 parts of polyethylene glycol, 35 parts of cyclohexane and 140 parts of N, N-dimethylformamide according to parts by weight, adding the carbon-five petroleum resin into the cyclohexane, stirring at the rotating speed of 260r/min for 25min at normal temperature to obtain a carbon-five petroleum resin solution, adding the polyacrylate powder, the epoxy resin, the polysulfone resin and the polyethylene glycol into the N, N-dimethylformamide, stirring at the rotating speed of 290r/min at normal temperature for 35min to obtain a polymer solution, placing the aluminum nitride, the zinc oxide and the silicon nitride into a stirrer, stirring and mixing at the rotating speed of 190r/min at normal temperature for 15min to obtain a powder filler, adding the carbon-five petroleum resin solution and the powder filler into the polymer solution, stirring at the normal temperature at the rotating speed of 700r/min for 35min, then placing in an ultrasonic dispersion machine, and ultrasonically dispersing at the normal temperature at the power of 450W for 25min to obtain the high-adhesion polyacrylate-based pouring sealant.
Example 3
Respectively weighing 40 parts of acrylic acid, 30 parts of butyl acrylate, 24 parts of methyl methacrylate, 8 parts of hydroxypropyl methacrylate, 12 parts of glycidyl methacrylate, 0.6 part of sodium persulfate, 0.4 part of sodium dodecyl benzene sulfonate, 6 parts of sodium carbonate and 120 parts of deionized water according to parts by weight, adding the butyl acrylate, the methyl methacrylate, the hydroxypropyl methacrylate and the glycidyl methacrylate into the acrylic acid, stirring for 4min at the rotating speed of 180r/min at normal temperature to obtain a mixed monomer, adding the sodium dodecyl benzene sulfonate and the sodium carbonate into the deionized water, stirring for 12min at the rotating speed of 200r/min under the water bath condition of 80 ℃, preserving heat to obtain a surfactant solution, adding the 1/10 mixed monomer and the 1/3 sodium persulfate into the surfactant solution, stirring and reacting for 12min at the rotating speed of 240r/min under the water bath condition of 80 ℃, obtaining seed emulsion, slowly adding the residual 9/10 mixed monomer into the seed emulsion at a dropping rate of 40mL/min, adding the residual 2/3 sodium persulfate, reacting for 2h at a rotating speed of 280r/min under a water bath condition of 90 ℃ to obtain mixed emulsion, cooling the mixed emulsion to room temperature, dropping ammonia water with the mass fraction of 1% to adjust the pH value to 7 to obtain polyacrylate emulsion, standing the polyacrylate emulsion for 2h at normal temperature, drying for 24h in a drying oven at 100 ℃, and cooling at normal temperature to obtain polyacrylate powder; respectively weighing 50 parts of aluminum powder, 80 parts of ammonium chloride, 0.4 part of potassium chloride and 0.6 part of calcium chloride according to parts by weight, adding the potassium chloride, the calcium chloride and the ammonium chloride into the aluminum powder, placing the aluminum powder in a ball mill, introducing argon at the speed of 100mL/min for protection, ball-milling at the rotating speed of 250r/min for 24 hours at normal temperature to obtain precursor powder, placing the precursor powder in a tubular atmosphere furnace, introducing nitrogen at the speed of 120mL/min for protection, carrying out heat preservation and calcination at the temperature of 1200 ℃ for 4 hours, cooling to room temperature along with the furnace to obtain blocky aluminum nitride, placing the blocky aluminum nitride in the ball mill, and stirring at the rotating speed of 340r/min for 24 hours at normal temperature to obtain aluminum nitride powder; respectively weighing 80 parts of polyacrylate powder, 40 parts of epoxy resin, 24 parts of polysulfone resin, 16 parts of carbon-five petroleum resin, 24 parts of aluminum nitride, 8 parts of zinc oxide, 8 parts of silicon nitride, 4 parts of polyethylene glycol, 40 parts of cyclohexane and 160 parts of N, N-dimethylformamide, adding the carbon-five petroleum resin into the cyclohexane, stirring at the rotating speed of 280r/min for 30min at normal temperature to obtain a carbon-five petroleum resin solution, adding the polyacrylate powder, the epoxy resin, the polysulfone resin and the polyethylene glycol into the N, N-dimethylformamide, stirring at the rotating speed of 300r/min at normal temperature for 40min to obtain a polymer solution, placing the aluminum nitride, the zinc oxide and the silicon nitride into a stirrer, stirring and mixing at the rotating speed of 200r/min at normal temperature for 20min to obtain a powder filler, adding the carbon-five petroleum resin solution and the powder filler into the polymer solution, stirring at the normal temperature at the rotating speed of 800r/min for 40min, then placing in an ultrasonic dispersion machine, and ultrasonically dispersing at the normal temperature at the power of 500W for 30min to obtain the high-adhesion polyacrylate-based pouring sealant.
The performance of the high-adhesion polyacrylate-based pouring sealant prepared by the invention and the commercially available pouring sealant is tested, and the specific detection results are shown in the following table 1.
The test method comprises the following steps:
the gel time and the heat distortion temperature were measured in the following methods for examples 1 to 3 and comparative examples, and transformers of the same type were each potted and the potting effect was observed, and the results are shown in table 1.
Method for determining gel time: the measurement was carried out using an HG-1A gel time measuring instrument. 100g of the high-bonding polyacrylate based pouring sealant is uniformly placed in a central circular groove of a stainless steel plate heated to 150 ℃, a stopwatch is started, and a small stainless steel spoon is used for stirring clockwise until the pouring sealant is not filamentized, namely the gel time is measured.
Measurement of Heat distortion temperature: respectively making the high-bonding polyacrylate-based pouring sealant into a rod-shaped structure of 120mm multiplied by 15mm multiplied by 10mm, soaking the rod-shaped pouring sealant in water with the constant temperature rise of 2 ℃/min after solidification, and applying force to the rod-shaped pouring sealant to enable the maximum bending stress of the rod-shaped pouring sealant to reach 18.5kg/cm2And when the bending deformation of the middle point of the rod-shaped pouring sealant reaches 0.21mm, recording the temperature of water at the moment, namely the thermal deformation temperature.
The encapsulation effect is as follows:
excellent: the encapsulation has no bubbles visible to naked eyes, and is dense.
And (4) qualification: small bubbles exist, and the whole use is not greatly influenced.
Unqualified: more air bubbles exist, and the filling effect is poor.
TABLE 1 characterization of the Properties of the high-adhesion polyacrylate-based pouring sealant
As shown in Table 1, the high-adhesion polyacrylate-based pouring sealant prepared by the invention has the advantages of short gel time, high thermal deformation temperature, good high temperature resistance and good pouring effect.
Claims (9)
1. A preparation method of a high-adhesion polyacrylate-based pouring sealant is characterized by comprising the following specific preparation steps:
(1) adding carbon five petroleum resin into cyclohexane, and stirring at the normal temperature at the rotating speed of 240-280 r/min for 20-30 min to obtain a carbon five petroleum resin solution;
(2) adding polyacrylate powder, epoxy resin, polysulfone resin and polyethylene glycol into N, N-dimethylformamide, and stirring at the normal temperature at the rotating speed of 280-300 r/min for 30-40 min to obtain a polymer solution;
(3) placing aluminum nitride, zinc oxide and silicon nitride in a stirrer, and stirring and mixing at the normal temperature at the rotating speed of 180-200 r/min for 10-20 min to obtain a powder filler;
(4) adding the carbon five petroleum resin solution and the powder filler into the polymer solution, stirring at the rotating speed of 600-800 r/min for 30-40 min at normal temperature, then placing in an ultrasonic dispersion machine, and performing ultrasonic dispersion for 20-30 min at normal temperature to obtain the high-adhesion polyacrylate-based pouring sealant.
2. The method for preparing a high adhesion polyacrylate based potting adhesive according to claim 1, wherein the weight parts of polyacrylate powder, epoxy resin, polysulfone resin, carbon penta petroleum resin, aluminum nitride, zinc oxide, silicon nitride, polyethylene glycol, cyclohexane and N, N-dimethylformamide are 60-80 parts of polyacrylate powder, 30-40 parts of epoxy resin, 18-24 parts of polysulfone resin, 12-16 parts of carbon penta petroleum resin, 18-24 parts of aluminum nitride, 6-8 parts of zinc oxide, 6-8 parts of silicon nitride, 3-4 parts of polyethylene glycol, 30-40 parts of cyclohexane and 120-160 parts of N, N-dimethylformamide.
3. The method for preparing the high-adhesion polyacrylate-based pouring sealant according to claim 1, wherein the power of the ultrasonic dispersion in the step (4) is 400-500W.
4. The method for preparing the high-adhesion polyacrylate-based pouring sealant according to claim 1, wherein the concrete preparation steps of the polyacrylate powder in the step (2) are as follows:
(1) adding butyl acrylate, methyl methacrylate, hydroxypropyl methacrylate and glycidyl methacrylate into acrylic acid, and stirring at the rotating speed of 160-180 r/min for 2-4 min at normal temperature to obtain a mixed monomer;
(2) adding sodium dodecyl benzene sulfonate and sodium carbonate into deionized water, stirring for 10-12 min at a rotating speed of 180-200 r/min under a water bath condition of 70-80 ℃, and preserving heat to obtain a surfactant solution;
(3) adding 1/10 mixed monomer and 1/3 sodium persulfate into a surfactant solution, and stirring and reacting for 10-12 min at a rotating speed of 200-240 r/min under a water bath condition of 70-80 ℃ to obtain seed emulsion;
(4) slowly adding the residual 9/10 mixed monomer into the seed emulsion, adding the residual 2/3 sodium persulfate, and reacting for 1-2 hours at the rotating speed of 240-280 r/min under the water bath condition of 80-90 ℃ to obtain mixed emulsion;
(5) cooling the mixed emulsion to room temperature, and adjusting the pH value to 7 to obtain polyacrylate emulsion;
(6) standing the polyacrylate emulsion for 1-2 hours at normal temperature, drying in an oven at 80-100 ℃ for 20-24 hours, and cooling at normal temperature to obtain polyacrylate powder.
5. The method for preparing the high-adhesion polyacrylate-based pouring sealant according to claim 4, wherein the weight parts of the acrylic acid, the butyl acrylate, the methyl methacrylate, the hydroxypropyl methacrylate, the glycidyl methacrylate, the sodium persulfate, the sodium dodecyl benzene sulfonate, the sodium carbonate and the deionized water are 30-40 parts of acrylic acid, 20-30 parts of butyl acrylate, 18-24 parts of methyl methacrylate, 6-8 parts of hydroxypropyl methacrylate, 8-12 parts of glycidyl methacrylate, 0.3-0.6 part of sodium persulfate, 0.2-0.4 part of sodium dodecyl benzene sulfonate, 4-6 parts of sodium carbonate and 100-120 parts of deionized water.
6. The method for preparing the high-adhesion polyacrylate-based pouring sealant according to claim 4, wherein the adding rate of the mixed monomer in the step (4) is 30-40 mL/min.
7. The method for preparing high adhesion polyacrylate based pouring sealant according to claim 4, wherein the pH adjustment in step (5) is 1% by weight of ammonia water.
8. The preparation method of the high-adhesion polyacrylate-based pouring sealant as claimed in claim 1, wherein the specific preparation steps of the aluminum nitride in the step (3) are as follows:
(1) adding potassium chloride, calcium chloride and ammonium chloride into aluminum powder, placing the aluminum powder into a ball mill, introducing argon at the speed of 80-100 mL/min for protection, and ball-milling at the rotating speed of 200-250 r/min for 20-24 h at normal temperature to obtain precursor powder;
(2) placing the precursor powder in a tubular atmosphere furnace, introducing nitrogen at the speed of 100-120 mL/min for protection, calcining at the temperature of 1000-1200 ℃ for 2-4 h, and cooling to room temperature along with the furnace to obtain massive aluminum nitride;
(3) and (3) placing the blocky aluminum nitride in a ball mill, and stirring at the normal temperature at the rotating speed of 300-340 r/min for 20-24 h to obtain the aluminum nitride powder.
9. The method for preparing the high-adhesion polyacrylate-based pouring sealant according to claim 8, wherein the aluminum powder, the ammonium chloride, the potassium chloride and the calcium chloride are 40-50 parts by weight, 60-80 parts by weight, 0.2-0.4 part by weight and 0.3-0.6 part by weight.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113725202A (en) * | 2021-08-18 | 2021-11-30 | 东莞中之科技股份有限公司 | Flip-chip exempts from bonding wire to dazzle various luminous LED lamp pearl packaging structure able to programme |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880375A (en) * | 2009-05-06 | 2010-11-10 | 合肥三晶电子有限公司 | Special curing agent for high-thermal-conductivity epoxy resin potting material, and potting material prepared from the same |
| CN102796346A (en) * | 2011-06-01 | 2012-11-28 | 深圳光启高等理工研究院 | Modified epoxy resin and method for preparing base material based on modified epoxy resin |
| CN102942889A (en) * | 2012-11-29 | 2013-02-27 | 宜兴市江南药用化工厂 | Low-halogen epoxy potting adhesive, and preparation method and application thereof |
| CN103012690A (en) * | 2012-12-12 | 2013-04-03 | 广州市高士实业有限公司 | Acrylic resin/organosilicon hybrid composite electronic potting adhesive and preparation method thereof |
| CN103059515A (en) * | 2012-12-20 | 2013-04-24 | 桂林电器科学研究院 | Vinyl ester resin modified epoxy pouring sealant and preparation method thereof |
| CN103937432A (en) * | 2014-02-14 | 2014-07-23 | 上海禧合应用材料有限公司 | Sealant |
| CN104356985A (en) * | 2014-10-15 | 2015-02-18 | 安徽蓝翔电器成套设备有限公司 | Transformer potting glue and preparation method and application thereof |
| CN104479607A (en) * | 2014-12-31 | 2015-04-01 | 烟台泰盛精化科技有限公司 | Low-stress transparent epoxy resin adhesive capable of curing fast at room temperature |
| CN107986246A (en) * | 2016-10-26 | 2018-05-04 | 河北正雍新材料科技有限公司 | A kind of method that aluminium powder nitriding prepares spherical aluminum nitride powder |
| CN109153902A (en) * | 2016-05-26 | 2019-01-04 | 泽菲罗斯有限公司 | Solid polymer binder composition and its product and method with operation at high temperature |
-
2019
- 2019-12-10 CN CN201911253988.1A patent/CN111057490A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880375A (en) * | 2009-05-06 | 2010-11-10 | 合肥三晶电子有限公司 | Special curing agent for high-thermal-conductivity epoxy resin potting material, and potting material prepared from the same |
| CN102796346A (en) * | 2011-06-01 | 2012-11-28 | 深圳光启高等理工研究院 | Modified epoxy resin and method for preparing base material based on modified epoxy resin |
| CN102942889A (en) * | 2012-11-29 | 2013-02-27 | 宜兴市江南药用化工厂 | Low-halogen epoxy potting adhesive, and preparation method and application thereof |
| CN103012690A (en) * | 2012-12-12 | 2013-04-03 | 广州市高士实业有限公司 | Acrylic resin/organosilicon hybrid composite electronic potting adhesive and preparation method thereof |
| CN103059515A (en) * | 2012-12-20 | 2013-04-24 | 桂林电器科学研究院 | Vinyl ester resin modified epoxy pouring sealant and preparation method thereof |
| CN103937432A (en) * | 2014-02-14 | 2014-07-23 | 上海禧合应用材料有限公司 | Sealant |
| CN104356985A (en) * | 2014-10-15 | 2015-02-18 | 安徽蓝翔电器成套设备有限公司 | Transformer potting glue and preparation method and application thereof |
| CN104479607A (en) * | 2014-12-31 | 2015-04-01 | 烟台泰盛精化科技有限公司 | Low-stress transparent epoxy resin adhesive capable of curing fast at room temperature |
| CN109153902A (en) * | 2016-05-26 | 2019-01-04 | 泽菲罗斯有限公司 | Solid polymer binder composition and its product and method with operation at high temperature |
| CN107986246A (en) * | 2016-10-26 | 2018-05-04 | 河北正雍新材料科技有限公司 | A kind of method that aluminium powder nitriding prepares spherical aluminum nitride powder |
Non-Patent Citations (1)
| Title |
|---|
| 韩长日 等 主编: "《胶粘剂生产工艺与技术》", 31 January 2018, 北京：科学技术文献出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113725202A (en) * | 2021-08-18 | 2021-11-30 | 东莞中之科技股份有限公司 | Flip-chip exempts from bonding wire to dazzle various luminous LED lamp pearl packaging structure able to programme |
| CN113725202B (en) * | 2021-08-18 | 2023-11-14 | 东莞中之科技股份有限公司 | Flip bonding wire-free programmable colorful luminous LED lamp bead packaging method |
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