CN114854354A - Low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant and preparation method thereof - Google Patents
Low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant and preparation method thereof Download PDFInfo
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 239000003063 flame retardant Substances 0.000 title claims abstract description 49
- 239000004814 polyurethane Substances 0.000 title claims abstract description 47
- 229920002635 polyurethane Polymers 0.000 title claims abstract description 41
- 239000000565 sealant Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 61
- 229920001730 Moisture cure polyurethane Polymers 0.000 claims abstract description 30
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000007822 coupling agent Substances 0.000 claims abstract description 24
- 229920002545 silicone oil Polymers 0.000 claims abstract description 21
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 16
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 16
- 239000003054 catalyst Substances 0.000 claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 239000002270 dispersing agent Substances 0.000 claims abstract description 16
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- 229920005862 polyol Polymers 0.000 claims abstract description 16
- 150000003077 polyols Chemical class 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 16
- 239000000853 adhesive Substances 0.000 claims abstract description 15
- 230000001070 adhesive effect Effects 0.000 claims abstract description 15
- 238000004382 potting Methods 0.000 claims abstract description 15
- 239000004925 Acrylic resin Substances 0.000 claims abstract description 14
- 229920000178 Acrylic resin Polymers 0.000 claims abstract description 14
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 14
- 238000006011 modification reaction Methods 0.000 claims abstract description 14
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 13
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229920001451 polypropylene glycol Polymers 0.000 claims description 33
- 239000000839 emulsion Substances 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 25
- -1 polyoxypropylene Polymers 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 19
- 239000002131 composite material Substances 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 18
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 12
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 12
- 239000004094 surface-active agent Substances 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 9
- RBNPOMFGQQGHHO-UHFFFAOYSA-N glyceric acid Chemical compound OCC(O)C(O)=O RBNPOMFGQQGHHO-UHFFFAOYSA-N 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 6
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 6
- 239000002041 carbon nanotube Substances 0.000 claims description 6
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 6
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 6
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 claims description 6
- 229920005749 polyurethane resin Polymers 0.000 claims description 6
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 6
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 claims description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 6
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 5
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 3
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 3
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 3
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 229920000142 Sodium polycarboxylate Polymers 0.000 claims description 3
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 claims description 3
- 239000006230 acetylene black Substances 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- 229920013822 aminosilicone Polymers 0.000 claims description 3
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 3
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 3
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 3
- 150000002009 diols Chemical class 0.000 claims description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 3
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 3
- 239000000194 fatty acid Substances 0.000 claims description 3
- 229930195729 fatty acid Natural products 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 3
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000003273 ketjen black Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 3
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 3
- GTRSAMFYSUBAGN-UHFFFAOYSA-N tris(2-chloropropyl) phosphate Chemical group CC(Cl)COP(=O)(OCC(C)Cl)OCC(C)Cl GTRSAMFYSUBAGN-UHFFFAOYSA-N 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 7
- 230000017525 heat dissipation Effects 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
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- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
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- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
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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
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
-
- 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
- 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
-
- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention belongs to the technical field of electronic pouring sealants, and discloses a low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant and a preparation method thereof, wherein the low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant comprises, by mass, 30-50 parts of polyether polyol, 20-30 parts of modified polyurethane prepolymer, 15-20 parts of heat-conducting powder, 10-20 parts of modified graphene oxide, 5-10 parts of vinyl silicone oil, 3-5 parts of a flame retardant, 3-5 parts of a catalyst, 2-4 parts of a defoaming agent, 2-4 parts of a dispersing agent, 1-2 parts of a coupling agent, and 1-2 parts of a curing agent. According to the invention, the acrylic resin is firstly utilized to modify polyurethane to obtain an acrylic modified polyurethane prepolymer, and then the amino-terminated silicone oil, the coupling agent and the toluene are utilized to carry out modification reaction on the graphene oxide, so that the finally prepared electronic potting adhesive has good flame retardance, water resistance and electrical properties, high temperature resistance, low viscosity, excellent heat conductivity and good heat dissipation effect.
Description
Technical Field
The invention belongs to the technical field of electronic pouring sealants, and particularly relates to a low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant and a preparation method thereof.
Background
At present, with the development of science and technology, more and more electronic products are updated and upgraded, the power consumption of equipment is continuously increased, and the heat productivity is rapidly increased. The bottleneck of future high-frequency high-power electronic products is a large amount of heat generated by the electronic products, and if the heat cannot be dissipated in time, the service life of the electronic products is shortened, the use power consumption of the electronic products is increased, more importantly, the running speed of the products is reduced, and the product quality is influenced.
Pouring sealant is widely used in electronic packaging, and is usually used in the core portion of electronic products, which is also the portion mainly generating heat. However, the existing electronic potting adhesive has complex synthesis process, poor high temperature resistance and unsatisfactory heat dissipation effect. Therefore, a new low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant and a preparation method thereof are needed to be designed.
Through the above analysis, the problems and defects of the prior art are as follows: the existing electronic potting adhesive has the disadvantages of complex synthesis process, poor high temperature resistance and unsatisfactory heat dissipation effect.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant and a preparation method thereof.
The low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant is prepared from, by mass, 30-50 parts of polyether polyol, 20-30 parts of modified polyurethane prepolymer, 15-20 parts of heat-conducting powder, 10-20 parts of modified graphene oxide, 5-10 parts of vinyl silicone oil, 3-5 parts of flame retardant, 3-5 parts of catalyst, 2-4 parts of defoaming agent, 2-4 parts of dispersing agent, 1-2 parts of coupling agent and 1-2 parts of curing agent.
Further, the polyether polyol is one or two of polyoxypropylene diol and polyoxypropylene triol;
the heat conducting powder is selected from one or more of carbon nano tubes, aluminum oxide, nano aluminum nitride, carbon black, acetylene black, ketjen black, nano silver wires, copper nano powder, gold nano powder and nano magnesium oxide powder, and preferably any one or more of carbon nano tubes, aluminum oxide and nano silver wires.
Further, the flame retardant is tris (2-chloropropyl) phosphate; the catalyst is any one or more of stannous octoate, dibutyltin dilaurate and triethylenediamine, and preferably dibutyltin dilaurate;
the defoaming agent is selected from any one or more of emulsified silicone oil, higher alcohol fatty acid ester compound, polyoxyethylene polyoxypropylene pentaerythritol ether, polyoxyethylene polyoxypropylene amine ether, polyoxypropylene glycerol ether, polyoxypropylene polyoxyethylene glycerol ether and polydimethylsiloxane, and is preferably polyoxypropylene glycerol ether;
the dispersing agent is selected from any one or more of a surfactant, a sodium polycarboxylate salt, sodium dodecyl benzene sulfonate and polyvinyl alcohol, and the surfactant is preferably OP-10;
the coupling agent is selected from any one or more of vinyl silane coupling agent, amino silane coupling agent and epoxy silane coupling agent; preferably a vinyl silane coupling agent comprising vinyl triethoxysilane, vinyl trimethoxysilane, preferably vinyl trimethoxysilane;
the curing agent is selected from any one or more of toluene diisocyanate, isophorone diisocyanate, diphenylmethane diisocyanate and hexamethylene diisocyanate, and toluene diisocyanate is preferred.
Another object of the present invention is to provide a method for preparing a low-viscosity flame-retardant heat-conductive solvent-free polyurethane electronic potting adhesive for implementing the low-viscosity flame-retardant heat-conductive solvent-free polyurethane electronic potting adhesive, wherein the method for preparing the low-viscosity flame-retardant heat-conductive solvent-free polyurethane electronic potting adhesive comprises the following steps:
step one, preparing a modified polyurethane prepolymer: preparing polyurethane-acrylate composite emulsion by using polyurethane and acrylic resin emulsion; dehydrating polypropylene glycol, and then adding the dehydrated polypropylene glycol into the polyurethane-acrylate composite emulsion to perform a heating reaction to obtain an acrylic acid modified polyurethane prepolymer;
step two, preparing modified graphene oxide: dispersing graphene oxide in water, adding amino-terminated silicone oil, a coupling agent and toluene, mixing, performing modification reaction to obtain a modified graphene oxide solution, performing centrifugal washing, and performing ultrasonic dispersion to obtain a modified graphene oxide dispersion solution;
step three, preparing the electronic pouring sealant: after the raw materials are respectively weighed, the modified polyurethane prepolymer, the heat conducting powder, the modified graphene oxide, the catalyst and the coupling agent are uniformly mixed, polyether polyol, vinyl silicone oil, a flame retardant, a defoaming agent, a dispersing agent and a curing agent are added, and the electronic potting adhesive is obtained through curing and forming.
Further, the preparation method of the modified polyurethane prepolymer in the first step comprises the following steps:
(1) according to the following steps of 1: 1, respectively weighing polyurethane and acrylic resin emulsion in a mass part ratio, placing the polyurethane and the acrylic resin emulsion in a stirring device, and fully and uniformly mixing the polyurethane and the acrylic resin emulsion under the stirring condition;
(2) adding a surfactant in the stirring process of a stirring device, and fully and uniformly mixing to obtain polyurethane-acrylate composite emulsion; wherein the surfactant is preferably OP-10;
(3) taking polypropylene glycol and carrying out vacuum-pumping dehydration to obtain dehydrated polypropylene glycol; under the protection of nitrogen, cooling dehydrated polypropylene glycol, and adding the dehydrated polypropylene glycol into the polyurethane-acrylate composite emulsion;
(4) controlling the addition amount of the polyurethane-acrylate composite emulsion to be 15-30% of the mass fraction of the dehydrated polypropylene glycol, stirring to mix uniformly, and heating to react to obtain the acrylic modified polyurethane prepolymer.
Further, the temperature-rising reaction in the step (4) includes:
and (3) placing the mixed solution of the polyurethane-acrylate composite emulsion and the dehydrated polypropylene glycol into a reaction device, heating to 85-95 ℃, and reacting for 2-4 hours to obtain the acrylic modified polyurethane prepolymer.
Further, the preparation method of the modified graphene oxide in the second step includes:
(1) dispersing graphene oxide in water to prepare a graphene oxide solution;
(2) adding amino silicone oil, a coupling agent and toluene into the graphene oxide solution, uniformly mixing, and then carrying out modification reaction to obtain a modified graphene oxide solution;
(3) and (3) carrying out centrifugal washing on the modified graphene oxide solution, and then ultrasonically dispersing in water to prepare the modified graphene oxide dispersion liquid.
Further, the modification reaction conditions in the step (2) are as follows: carrying out modification reaction for 8-14 h at the temperature of 70-150 ℃;
the ultrasonic dispersion time in the step (3) is 1-3 hours, and the concentration of the modified graphene oxide solution is 2-12 g/mL.
Further, the preparation method of the electronic pouring sealant in the third step comprises the following steps:
(1) respectively weighing polyether polyol, a modified polyurethane prepolymer, heat-conducting powder, modified graphene oxide, vinyl silicone oil, a flame retardant, a catalyst, a defoaming agent, a dispersing agent, a coupling agent and a curing agent;
(2) respectively and uniformly mixing the modified polyurethane prepolymer, the heat conducting powder and the modified graphene oxide, vacuumizing, dehydrating, cooling, adding a catalyst and a coupling agent, and fully stirring to obtain a first mixture;
(3) and preheating the first mixture, adding polyether polyol, vinyl silicone oil and a flame retardant, uniformly mixing, adding a defoaming agent and a dispersing agent, stirring, adding a curing agent, stirring while performing vacuum defoaming, and performing curing molding to obtain the low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic potting adhesive.
Further, the conditions for curing and molding in the step (3) include: setting the curing temperature to be 80-140 ℃ and the curing time to be 6-24 h;
wherein the curing temperature is preferably 100 ℃, and the curing time is preferably 12 h.
In combination with the technical solutions and the technical problems to be solved, please analyze the advantages and positive effects of the technical solutions to be protected in the present invention from the following aspects:
first, aiming at the technical problems existing in the prior art and the difficulty in solving the problems, the technical problems to be solved by the technical scheme of the present invention are closely combined with results, data and the like in the research and development process, and some creative technical effects are brought after the problems are solved. The specific description is as follows:
according to the preparation method of the low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant provided by the invention, firstly, polyurethane is modified by using acrylic resin to obtain an acrylic modified polyurethane prepolymer, and then, the graphene oxide is subjected to modification reaction by using amino-terminated silicone oil, a coupling agent and toluene, so that the finally prepared electronic pouring sealant has good flame retardance, water resistance and electrical performance, does not need to perform surface treatment on electronic components, is simpler in process treatment, and is easy to realize automatic production.
Secondly, considering the technical scheme as a whole or from the perspective of products, the technical effect and advantages of the technical scheme to be protected by the invention are specifically described as follows:
the preparation method of the low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant provided by the invention is simple and feasible, and the prepared electronic pouring sealant is high-temperature resistant, low in viscosity, excellent in heat-conducting property and good in heat dissipation effect.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments of the present invention will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart of a method for preparing a low-viscosity flame-retardant heat-conductive solvent-free polyurethane electronic pouring sealant according to an embodiment of the present invention;
fig. 2 is a flowchart of a method for preparing modified graphene oxide according to an embodiment of the present invention;
fig. 3 is a flowchart of a method for preparing an electronic potting adhesive according to an embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Aiming at the problems in the prior art, the invention provides a low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant and a preparation method thereof, and the invention is described in detail below with reference to the accompanying drawings.
First, an embodiment is explained. This section is an explanatory embodiment expanding on the claims so as to fully understand how the present invention is embodied by those skilled in the art.
The low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant provided by the embodiment of the invention comprises, by mass, 30-50 parts of polyether polyol, 20-30 parts of modified polyurethane prepolymer, 15-20 parts of heat-conducting powder, 10-20 parts of modified graphene oxide, 5-10 parts of vinyl silicone oil, 3-5 parts of flame retardant, 3-5 parts of catalyst, 2-4 parts of defoaming agent, 2-4 parts of dispersing agent, 1-2 parts of coupling agent and 1-2 parts of curing agent.
The polyether polyol provided by the embodiment of the invention is one or two of polyoxypropylene diol and polyoxypropylene triol; the heat conducting powder is selected from one or more of carbon nano tube, aluminum oxide, nano aluminum nitride, carbon black, acetylene black, ketjen black, nano silver wire, copper nano powder, gold nano powder and nano magnesium oxide powder, and preferably any one or more of carbon nano tube, aluminum oxide and nano silver wire.
The flame retardant provided by the embodiment of the invention is tris (2-chloropropyl) phosphate; the catalyst is any one or more of stannous octoate, dibutyltin dilaurate and triethylenediamine, and preferably dibutyltin dilaurate;
the defoaming agent is selected from one or more of emulsified silicone oil, higher alcohol fatty acid ester compound, polyoxyethylene polyoxypropylene pentaerythritol ether, polyoxyethylene polyoxypropylene amine ether, polyoxypropylene glycerol ether, polyoxypropylene polyoxyethylene glycerol ether and polydimethylsiloxane, and is preferably polyoxypropylene glycerol ether;
the dispersing agent is selected from any one or more of a surfactant, a sodium polycarboxylate salt, sodium dodecyl benzene sulfonate and polyvinyl alcohol, and the surfactant is preferably OP-10;
the coupling agent is selected from any one or more of vinyl silane coupling agent, amino silane coupling agent and epoxy silane coupling agent; preferably a vinyl silane coupling agent comprising vinyl triethoxysilane, vinyl trimethoxysilane, preferably vinyl trimethoxysilane;
the curing agent is selected from any one or more of toluene diisocyanate, isophorone diisocyanate, diphenylmethane diisocyanate and hexamethylene diisocyanate, and toluene diisocyanate is preferred.
As shown in fig. 1, the preparation method of the low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant provided by the embodiment of the invention comprises the following steps:
s101, preparing a modified polyurethane prepolymer: preparing polyurethane-acrylate composite emulsion by using polyurethane and acrylic resin emulsion; dehydrating polypropylene glycol, and then adding the dehydrated polypropylene glycol into the polyurethane-acrylate composite emulsion to perform a heating reaction to obtain an acrylic acid modified polyurethane prepolymer;
s102, preparing modified graphene oxide: dispersing graphene oxide in water, adding amino-terminated silicone oil, a coupling agent and toluene, mixing, performing modification reaction to obtain a modified graphene oxide solution, performing centrifugal washing, and performing ultrasonic dispersion to obtain a modified graphene oxide dispersion solution;
s103, preparing the electronic pouring sealant: after the raw materials are respectively weighed, the modified polyurethane prepolymer, the heat conducting powder, the modified graphene oxide, the catalyst and the coupling agent are uniformly mixed, polyether polyol, vinyl silicone oil, a flame retardant, a defoaming agent, a dispersing agent and a curing agent are added, and the electronic potting adhesive is obtained through curing and forming.
The preparation method of the modified polyurethane prepolymer in the step S101 provided by the embodiment of the present invention includes:
(1) according to the following steps of 1: 1, respectively weighing polyurethane and acrylic resin emulsion in a mass part ratio, placing the polyurethane and the acrylic resin emulsion in a stirring device, and fully and uniformly mixing the polyurethane and the acrylic resin emulsion under the stirring condition;
(2) adding a surfactant in the stirring process of a stirring device, and fully and uniformly mixing to obtain polyurethane-acrylate composite emulsion; wherein the surfactant is preferably OP-10;
(3) taking polypropylene glycol and carrying out vacuum-pumping dehydration to obtain dehydrated polypropylene glycol; under the protection of nitrogen, cooling dehydrated polypropylene glycol, and adding the dehydrated polypropylene glycol into the polyurethane-acrylate composite emulsion;
(4) controlling the addition amount of the polyurethane-acrylate composite emulsion to be 15-30% of the mass fraction of the dehydrated polypropylene glycol, stirring to mix uniformly, and heating to react to obtain the acrylic modified polyurethane prepolymer.
The temperature rise reaction in the step (4) provided by the embodiment of the invention comprises the following steps: and (3) placing the mixed solution of the polyurethane-acrylate composite emulsion and the dehydrated polypropylene glycol into a reaction device, heating to 85-95 ℃, and reacting for 2-4 hours to obtain the acrylic modified polyurethane prepolymer.
As shown in fig. 2, the preparation method of the modified graphene oxide in step S102 provided by the embodiment of the present invention includes:
s201, dispersing graphene oxide in water to prepare a graphene oxide solution;
s202, adding amino silicone oil, a coupling agent and toluene into the graphene oxide solution, uniformly mixing, and then carrying out modification reaction to obtain a modified graphene oxide solution;
s203, carrying out centrifugal washing on the modified graphene oxide solution, and then ultrasonically dispersing in water to prepare the modified graphene oxide dispersion liquid.
The modification reaction conditions in step S202 provided in the embodiment of the present invention are: carrying out modification reaction for 8-14 h at the temperature of 70-150 ℃; the ultrasonic dispersion time in the step S203 is 1-3 h, and the concentration of the modified graphene oxide solution is 2-12 g/mL.
As shown in fig. 3, the method for preparing the electronic potting adhesive of step S103 according to the embodiment of the present invention includes:
s301, respectively weighing polyether polyol, a modified polyurethane prepolymer, heat-conducting powder, modified graphene oxide, vinyl silicone oil, a flame retardant, a catalyst, a defoaming agent, a dispersing agent, a coupling agent and a curing agent;
s302, respectively and uniformly mixing the modified polyurethane prepolymer, the heat conducting powder and the modified graphene oxide, vacuumizing, dehydrating, cooling, adding a catalyst and a coupling agent, and fully stirring to obtain a first mixture;
s303, preheating the first mixture, adding polyether polyol, vinyl silicone oil and a flame retardant, uniformly mixing, adding a defoaming agent and a dispersing agent, stirring, adding a curing agent, stirring while performing vacuum defoaming, and performing curing molding to obtain the low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic potting adhesive.
The conditions for curing and forming in step S303 provided in the embodiment of the present invention include: setting the curing temperature to be 80-140 ℃ and the curing time to be 6-24 h; wherein the curing temperature is preferably 100 ℃ and the curing time is preferably 12 h.
And II, application embodiment. In order to prove the creativity and the technical value of the technical scheme of the invention, the part is an application example of the technical scheme of the claims to a specific product or related technology.
The electronic pouring sealant prepared by the preparation method of the low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant provided by the embodiment of the invention has the advantages of high temperature resistance, low viscosity, excellent heat-conducting property, good heat dissipation effect, good flame retardance, water resistance and electrical property, no need of surface treatment on electronic components, simpler process treatment and easiness in realization of automatic production.
The above description is only for the purpose of illustrating the embodiments of the present invention, and the scope of the present invention should not be limited thereto, and any modifications, equivalents and improvements made by those skilled in the art within the technical scope of the present invention as disclosed in the present invention should be covered by the scope of the present invention.
Claims (10)
1. The low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant is characterized by comprising, by mass, 30-50 parts of polyether polyol, 20-30 parts of modified polyurethane prepolymer, 15-20 parts of heat-conducting powder, 10-20 parts of modified graphene oxide, 5-10 parts of vinyl silicone oil, 3-5 parts of flame retardant, 3-5 parts of catalyst, 2-4 parts of defoaming agent, 2-4 parts of dispersing agent, 1-2 parts of coupling agent and 1-2 parts of curing agent.
2. The low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant as claimed in claim 1, wherein the polyether polyol is one or both of polyoxypropylene diol and polyoxypropylene triol;
the heat conducting powder is selected from one or more of carbon nano tubes, aluminum oxide, nano aluminum nitride, carbon black, acetylene black, ketjen black, nano silver wires, copper nano powder, gold nano powder and nano magnesium oxide powder, and preferably any one or more of carbon nano tubes, aluminum oxide and nano silver wires.
3. The low-viscosity flame-retardant thermally-conductive solvent-free polyurethane electronic potting adhesive of claim 1, wherein the flame retardant is tris (2-chloropropyl) phosphate; the catalyst is any one or more of stannous octoate, dibutyltin dilaurate and triethylenediamine, and preferably dibutyltin dilaurate;
the defoaming agent is selected from any one or more of emulsified silicone oil, higher alcohol fatty acid ester compound, polyoxyethylene polyoxypropylene pentaerythritol ether, polyoxyethylene polyoxypropylene amine ether, polyoxypropylene glycerol ether, polyoxypropylene polyoxyethylene glycerol ether and polydimethylsiloxane, and is preferably polyoxypropylene glycerol ether;
the dispersing agent is selected from any one or more of a surfactant, a sodium polycarboxylate salt, sodium dodecyl benzene sulfonate and polyvinyl alcohol, and the surfactant is preferably OP-10;
the coupling agent is selected from any one or more of vinyl silane coupling agent, amino silane coupling agent and epoxy silane coupling agent; preferably a vinyl silane coupling agent comprising vinyl triethoxysilane, vinyl trimethoxysilane, preferably vinyl trimethoxysilane;
the curing agent is selected from any one or more of toluene diisocyanate, isophorone diisocyanate, diphenylmethane diisocyanate and hexamethylene diisocyanate, and toluene diisocyanate is preferred.
4. A preparation method of the low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant for implementing the low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant as claimed in any one of claims 1 to 3, wherein the preparation method of the low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant comprises the following steps:
step one, preparing a modified polyurethane prepolymer: preparing polyurethane-acrylate composite emulsion by using polyurethane and acrylic resin emulsion; dehydrating polypropylene glycol, and then adding the dehydrated polypropylene glycol into the polyurethane-acrylate composite emulsion to perform a heating reaction to obtain an acrylic acid modified polyurethane prepolymer;
step two, preparing modified graphene oxide: dispersing graphene oxide in water, adding amino-terminated silicone oil, a coupling agent and toluene, mixing, performing modification reaction to obtain a modified graphene oxide solution, performing centrifugal washing, and performing ultrasonic dispersion to obtain a modified graphene oxide dispersion solution;
step three, preparing the electronic pouring sealant: after the raw materials are respectively weighed, the modified polyurethane prepolymer, the heat conducting powder, the modified graphene oxide, the catalyst and the coupling agent are uniformly mixed, polyether polyol, vinyl silicone oil, a flame retardant, a defoaming agent, a dispersing agent and a curing agent are added, and the electronic potting adhesive is obtained through curing and forming.
5. The preparation method of the low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant as claimed in claim 4, wherein the preparation method of the modified polyurethane prepolymer in the first step comprises the following steps:
(1) according to the following steps of 1: 1, respectively weighing polyurethane and acrylic resin emulsion in a mass part ratio, placing the polyurethane and the acrylic resin emulsion in a stirring device, and fully and uniformly mixing the polyurethane and the acrylic resin emulsion under the stirring condition;
(2) adding a surfactant in the stirring process of a stirring device, and fully and uniformly mixing to obtain polyurethane-acrylate composite emulsion; wherein the surfactant is preferably OP-10;
(3) taking polypropylene glycol and carrying out vacuum-pumping dehydration to obtain dehydrated polypropylene glycol; under the protection of nitrogen, cooling dehydrated polypropylene glycol, and adding the dehydrated polypropylene glycol into the polyurethane-acrylate composite emulsion;
(4) controlling the addition amount of the polyurethane-acrylate composite emulsion to be 15-30% of the mass fraction of the dehydrated polypropylene glycol, stirring to mix uniformly, and heating to react to obtain the acrylic modified polyurethane prepolymer.
6. The method for preparing the low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant as claimed in claim 5, wherein the temperature-raising reaction in the step (4) comprises:
and (3) placing the mixed solution of the polyurethane-acrylate composite emulsion and the dehydrated polypropylene glycol into a reaction device, heating to 85-95 ℃, and reacting for 2-4 hours to obtain the acrylic modified polyurethane prepolymer.
7. The preparation method of the low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant as claimed in claim 4, wherein the preparation method of the modified graphene oxide in the second step comprises:
(1) dispersing graphene oxide in water to prepare a graphene oxide solution;
(2) adding amino silicone oil, a coupling agent and toluene into the graphene oxide solution, uniformly mixing, and then carrying out modification reaction to obtain a modified graphene oxide solution;
(3) and (3) carrying out centrifugal washing on the modified graphene oxide solution, and then ultrasonically dispersing in water to prepare the modified graphene oxide dispersion liquid.
8. The method for preparing the low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant as claimed in claim 7, wherein the modification reaction conditions in the step (2) are as follows: carrying out modification reaction for 8-14 h at the temperature of 70-150 ℃;
the ultrasonic dispersion time in the step (3) is 1-3 hours, and the concentration of the modified graphene oxide solution is 2-12 g/mL.
9. The method for preparing the low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant as claimed in claim 4, wherein the method for preparing the electronic pouring sealant in the third step comprises:
(1) respectively weighing polyether polyol, a modified polyurethane prepolymer, heat-conducting powder, modified graphene oxide, vinyl silicone oil, a flame retardant, a catalyst, a defoaming agent, a dispersing agent, a coupling agent and a curing agent;
(2) respectively and uniformly mixing the modified polyurethane prepolymer, the heat conducting powder and the modified graphene oxide, vacuumizing, dehydrating, cooling, adding a catalyst and a coupling agent, and fully stirring to obtain a first mixture;
(3) and preheating the first mixture, adding polyether polyol, vinyl silicone oil and a flame retardant, uniformly mixing, adding a defoaming agent and a dispersing agent, stirring, adding a curing agent, stirring while performing vacuum defoaming, and performing curing molding to obtain the low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic potting adhesive.
10. The method for preparing the low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant as claimed in claim 9, wherein the curing and molding conditions in the step (3) comprise: setting the curing temperature to be 80-140 ℃ and the curing time to be 6-24 h;
wherein the curing temperature is preferably 100 ℃, and the curing time is preferably 12 h.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115584129A (en) * | 2022-09-21 | 2023-01-10 | 深圳市欧普特工业材料有限公司 | Heat-conducting silica gel sheet and preparation method thereof |
| CN116041983A (en) * | 2022-12-06 | 2023-05-02 | 锐腾新材料制造(苏州)有限公司 | Surface treatment method of powder for polyurethane heat-conducting pouring sealant |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113088235A (en) * | 2021-03-09 | 2021-07-09 | 北京旭碳新材料科技有限公司 | Graphene heat dissipation pouring sealant composition, and pouring sealant and heat dissipation module prepared from composition |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113088235A (en) * | 2021-03-09 | 2021-07-09 | 北京旭碳新材料科技有限公司 | Graphene heat dissipation pouring sealant composition, and pouring sealant and heat dissipation module prepared from composition |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115584129A (en) * | 2022-09-21 | 2023-01-10 | 深圳市欧普特工业材料有限公司 | Heat-conducting silica gel sheet and preparation method thereof |
| CN115584129B (en) * | 2022-09-21 | 2024-01-30 | 深圳市欧普特工业材料有限公司 | Heat-conducting silica gel sheet and preparation method thereof |
| CN116041983A (en) * | 2022-12-06 | 2023-05-02 | 锐腾新材料制造(苏州)有限公司 | Surface treatment method of powder for polyurethane heat-conducting pouring sealant |
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