CN117683508A - Double-component polyurethane heat-conducting pouring sealant adhesive and preparation method thereof - Google Patents
Double-component polyurethane heat-conducting pouring sealant adhesive and preparation method thereof Download PDFInfo
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- CN117683508A CN117683508A CN202311830435.4A CN202311830435A CN117683508A CN 117683508 A CN117683508 A CN 117683508A CN 202311830435 A CN202311830435 A CN 202311830435A CN 117683508 A CN117683508 A CN 117683508A
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- 239000000853 adhesive Substances 0.000 title claims abstract description 43
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 43
- 229920002635 polyurethane Polymers 0.000 title claims abstract description 34
- 239000004814 polyurethane Substances 0.000 title claims abstract description 34
- 239000000565 sealant Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 229920001730 Moisture cure polyurethane Polymers 0.000 claims abstract description 62
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 42
- 229920000570 polyether Polymers 0.000 claims abstract description 42
- 229920005862 polyol Polymers 0.000 claims abstract description 27
- 150000003077 polyols Chemical class 0.000 claims abstract description 27
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- 239000004519 grease Substances 0.000 claims abstract description 9
- 229920005906 polyester polyol Polymers 0.000 claims abstract description 9
- 239000002131 composite material Substances 0.000 claims abstract description 8
- 239000000945 filler Substances 0.000 claims abstract description 8
- 239000004014 plasticizer Substances 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 20
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 claims description 17
- 238000001816 cooling Methods 0.000 claims description 16
- 125000005442 diisocyanate group Chemical group 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims description 11
- 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 10
- 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 10
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 10
- 238000004382 potting Methods 0.000 claims description 10
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 8
- 229920000642 polymer Polymers 0.000 claims description 8
- 230000004224 protection Effects 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 229920001451 polypropylene glycol Polymers 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 claims description 4
- -1 polyoxypropylene Polymers 0.000 claims description 4
- 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 4
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 2
- 229920013701 VORANOL™ Polymers 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052797 bismuth Inorganic materials 0.000 claims description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 2
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 238000007789 sealing Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 230000007774 longterm Effects 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 10
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 230000032683 aging Effects 0.000 description 6
- 230000018044 dehydration Effects 0.000 description 4
- 238000006297 dehydration reaction Methods 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 230000006750 UV protection Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000002209 hydrophobic effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000000084 colloidal system Substances 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
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- Sealing Material Composition (AREA)
- Polyurethanes Or Polyureas (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention belongs to the technical field of adhesives, and relates to a double-component polyurethane heat-conducting pouring sealant adhesive and a preparation method thereof, wherein the double-component polyurethane heat-conducting pouring sealant adhesive comprises the following components in parts by weight: 21-25 parts of low-viscosity polyurethane prepolymer A; 60-74 parts of low-viscosity polyurethane prepolymer B; 9-11 parts of non-reactive plasticizer; and the component B comprises the following components: 9-12 parts of natural grease polyol; 9-12 parts of non-polyester polyol; 19-23 parts of polyether polyol; 50-61 parts of composite filler; 1-3 parts of an anti-settling agent; 0.05-0.5 part of catalyst; the volume ratio of the component A to the component B is 1:1. The bi-component polyurethane heat-conducting pouring sealant adhesive is solvent-free, is suitable for pouring and bonding of electrical components, has excellent mechanical properties, and can keep good bonding and sealing effects after long-term use.
Description
Technical Field
The invention belongs to the technical field of adhesives, and particularly relates to a double-component polyurethane heat-conducting pouring sealant adhesive and a preparation method thereof.
Background
The polyurethane pouring sealant has relatively excellent low temperature resistance, is slightly soft in material, has relatively good cohesiveness to common pouring materials, has binding force between epoxy resin and organic silicon, and has relatively good waterproof, moistureproof and insulating properties.
However, there are problems in that the high temperature resistance is poor and foaming is easy, and vacuum defoaming is necessary; after solidification, the surface of the colloid is not smooth, the toughness is poor, the aging resistance, shock resistance and ultraviolet rays are very weak, and the colloid is easy to change color.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a double-component polyurethane heat-conducting pouring sealant adhesive and a preparation method thereof, and the specific technical scheme is as follows:
the invention provides a two-component polyurethane heat-conducting pouring sealant adhesive, which comprises the following components in parts by weight:
and (3) a component A: 21-25 parts of low-viscosity polyurethane prepolymer A; 60-74 parts of low-viscosity polyurethane prepolymer B; 9-11 parts of non-reactive plasticizer;
the polyurethane prepolymer A is an NCO-terminated polymer, and the molar ratio of isocyanate groups to hydroxyl groups is 1.5-2.2:1, a step of; the polyurethane prepolymer B is an NCO-terminated polymer, and the molar ratio of isocyanate groups to hydroxyl groups is 2.5-3.0:1, the viscosity is 800-1600 mPa.s;
and the component B comprises the following components: 9-12 parts of natural grease polyol; 9-12 parts of non-polyester polyol; 19-23 parts of polyether polyol; 50-61 parts of composite filler; 1-3 parts of an anti-settling agent; 0.05-0.5 part of catalyst;
the volume ratio of the component A to the component B is 1:1.
The bi-component polyurethane heat conduction potting adhesive disclosed by the invention has the advantages that the formula is optimized, the low-viscosity system ensures the flowing property and the leveling property, and the bi-component polyurethane heat conduction potting adhesive is suitable for potting of complex structures; on the premise of ensuring mechanical properties by adopting the low-viscosity and low-NCO polyurethane prepolymer A, multi-branched chain extension is obtained, so that the product has lower viscosity; the polyurethane prepolymer B with low viscosity and higher NCO is adopted, so that the product has better flexibility, tensile property and lower viscosity on the premise of ensuring mechanical property; adopting a non-reactive plasticizer to prevent NCO in the prepolymer from reacting, so that the material is solidified and loses efficacy; the natural grease polyol and the prepolymer are combined, so that the product can be endowed with good hydrophobic performance, and the phenomenon of bubbles is avoided; meanwhile, under the synergistic effect of the natural grease polyol and other components, the ultraviolet resistance, weather resistance and chemical resistance are greatly improved; the pouring sealant adhesive can be applied to the pouring of electronic components with high heat.
Further, the low-viscosity polyurethane prepolymer A is a polymer containing NCO ends prepared by the reaction of the following raw materials in percentage by weight: 50-70% of polyether triol and 30-50% of diisocyanate.
Further, the low-viscosity polyurethane prepolymer B is a polymer containing NCO ends prepared by the reaction of the following raw materials in percentage by weight: 35-60% of polyether triol and 40-65% of diisocyanate.
Further, the raw material polyether triol of the low-viscosity polyurethane prepolymer A has an average molecular weight of 2000-5000; the diisocyanate is at least one of toluene diisocyanate, diphenylmethane diisocyanate and diphenylmethane diisocyanate.
The beneficial effects of adopting the further technical scheme are that: the main chain of the polyether triol contains ether bond (-R-O-R-), and the terminal group or the side group contains three hydroxyl groups (-OH), so that the three-dimensional crosslinking reaction is satisfied, and the excellent water resistance, impact resistance and low-temperature property are provided
Further, the raw material polyether triol of the low-viscosity polyurethane prepolymer B has an average molecular weight of 6000-12000; the diisocyanate is at least one of toluene diisocyanate, diphenylmethane diisocyanate and hexamethylene diisocyanate.
The beneficial effects of adopting the further technical scheme are that: the adopted polyether triol main chain contains ether bond (-R-O-R-), and the terminal group or the side group contains three hydroxyl groups (-OH), so that the high molecular weight of 6000-12000 can further improve the excellent low-temperature flexibility, hydrolysis resistance stability and low viscosity characteristic.
Further, the natural oil polyol is basf 750, and the viscosity is 5000-7000mpa.s.
Further, the polyether polyol is the Dow polyether VORANOL 3003LM with the viscosity 604mPa.S.
Further, the hydroxyl value of the non-polyester polyol is 200-300mg KOH/g, and the non-polyester polyol is one of polyoxypropylene dihydric alcohol, polyoxypropylene trihydric alcohol and polypropylene dihydric alcohol.
Further, the non-reactive plasticizer includes at least one of other non-reactive phosphates such as propylene carbonate, triethyl phosphate, etc., preferably propylene carbonate.
Further, the catalyst is one or a combination of two or more of dibutyl tin dilaurate, organic bismuth and organic zinc.
Further, the anti-settling agent is at least one of GARAMITE-1958, RHEYBYK-R605 and BYK-R607
Further, the composite filler is a compound of aluminum hydroxide and aluminum oxide.
Further, in the composite filler, the alumina accounts for 33 percent, and the maximum particle size of the composite filler is smaller than 170 mu m.
The second purpose of the invention is to provide a preparation method of the bi-component polyurethane heat-conducting pouring sealant adhesive, which comprises the following steps:
d1, preparing polyurethane prepolymer A: according to weight percentage, putting polyether triol into a flask, heating to 100-110 ℃, vacuumizing to remove water, cooling to 45-55 ℃, adding diisocyanate, reacting under the protection of nitrogen, heating to 80-85 ℃ and continuously heating for 2-3h until NCO value is unchanged, and cooling to room temperature to obtain polyurethane prepolymer A;
d2, preparing polyurethane prepolymer B: according to weight percentage, putting polyether triol into a flask, heating to 100-110 ℃, vacuumizing to remove water, cooling to 45-55 ℃, adding diisocyanate, reacting under the protection of nitrogen, heating to 80-85 ℃ and continuously heating for 2-3h until NCO value is unchanged, and cooling to room temperature to obtain polyurethane prepolymer B;
d3, 21-25 parts of low-viscosity polyurethane prepolymer A; 60-74 parts of low-viscosity polyurethane prepolymer B; 9-11 parts of non-reactive plasticizer are put into a stirring kettle, and are vacuumized and stirred for 1-2 hours, the mixing temperature is less than or equal to 50 ℃, and the vacuum degree is minus 0.08 to minus 0.09MPa, so that a component A is obtained;
d4, 9-12 parts of natural grease polyol; 9-12 parts of a non-polyester polyol; 19-23 parts of polyether polyol; 50-61 parts of composite filler; 1-3 parts of an anti-settling agent; and (3) adding 0.05-0.5 part of catalyst into a stirring kettle, vacuumizing and stirring for 1-2 hours, wherein the mixing temperature is less than or equal to 60 ℃, and the vacuum degree is minus 0.08-minus 0.09MPa, so as to obtain the component B.
Compared with the prior art, the invention has the beneficial effects that:
the double-component polyurethane heat-conducting potting adhesive prepared by the invention comprises A, B components, wherein the overall viscosity of the component A is less than 2500 cps at 25 ℃, the overall viscosity of the component B is less than 1500cps at 25 ℃, and the low-viscosity system ensures the flowing property and leveling property, so that the double-component polyurethane heat-conducting potting adhesive is suitable for potting complex structures; the natural grease polyol and the prepolymer are combined, so that the product can be endowed with good hydrophobic performance, and the phenomenon of bubbles is avoided; meanwhile, under the synergistic effect of the natural grease polyol and other components, the ultraviolet resistance, weather resistance and chemical resistance are greatly improved; the pouring sealant adhesive is solvent-free, and can be applied to the pouring of electronic components with high heat.
Detailed Description
The principles and features of the present invention are described below in connection with examples, which are set forth only to illustrate the present invention and not to limit the scope of the invention.
Example 1:
the preparation of the bi-component polyurethane heat-conducting pouring sealant adhesive comprises the following steps:
d1, preparing polyurethane prepolymer A: sequentially adding 100g of polyether triol into a dried 2L four-mouth bottle, heating to 100 ℃ for vacuum dehydration for 2 hours, cooling to 50 ℃, adding 74g of diphenylmethane diisocyanate, heating to 85 ℃ for heat preservation reaction for 2.5 hours under the protection of nitrogen, cooling to room temperature when the NCO value is unchanged during the reaction, discharging to obtain polyurethane prepolymer A, and placing the polyurethane prepolymer A in a dried nitrogen closed container for later use;
d2, preparing a low-viscosity polyurethane prepolymer B: sequentially adding 100g of polyether triol into a dried 2L four-mouth bottle, heating to 100 ℃ for vacuum dehydration for 2 hours, cooling to 50 ℃, adding 122g of diphenylmethane diisocyanate, heating to 85 ℃ for heat preservation reaction for 2.5 hours under the protection of nitrogen, cooling to room temperature when the NCO value is unchanged during the reaction, discharging to obtain a polyurethane prepolymer B, and placing the polyurethane prepolymer B in a dried nitrogen closed container for later use;
d3, mixing 23g of polyurethane prepolymer A and 67g of low-viscosity polyurethane prepolymer B;10g of propylene carbonate is put into a stirring kettle, and is vacuumized and stirred for 1.5 hours, the mixing temperature is less than or equal to 50 ℃, and the vacuum degree is minus 0.08MPa, so that a well mixed component A is obtained;
d4, 10.5g basf 750;10.5g polyether 3003LM;21.1g of polyether polyol; 36.85g aluminum hydroxide with 18.15g alumina; 2.8g of anti-settling agent GARAMITE-1958;0.09g of dibutyl tin dilaurate is put into a stirring kettle, vacuumized and stirred for 1.5 hours, the mixing temperature is less than or equal to 60 ℃, and the vacuum degree is-0.08 MPa, so that the component B is obtained.
Example 2
The preparation of the bi-component polyurethane heat-conducting pouring sealant adhesive comprises the following steps:
d1, D2 prepolymer is prepared as in example 1, and is not described here again;
d3, 21g of polyurethane prepolymer A and 60g of low-viscosity polyurethane prepolymer B;11g of propylene carbonate is put into a stirring kettle, and is vacuumized and stirred for 1.5 hours, the mixing temperature is less than or equal to 50 ℃, and the vacuum degree is minus 0.08MPa, so that a well mixed component A is obtained;
d4, 12g of Basoff 750;12g of polyether 3003LM;23g of polyether polyol; 36.85g aluminum hydroxide with 18.15g alumina; 2.8g of anti-settling agent GARAMITE-1958;0.09g of dibutyl tin dilaurate is put into a stirring kettle, vacuumized and stirred for 1.5 hours, the mixing temperature is less than or equal to 60 ℃, and the vacuum degree is-0.08 MPa, so that the component B is obtained.
Example 3
The preparation of the bi-component polyurethane heat-conducting pouring sealant adhesive comprises the following steps:
d1, D2 prepolymer is prepared as in example 1, and is not described here again;
d3, mixing 25g of polyurethane prepolymer A and 74g of low-viscosity polyurethane prepolymer B;9g of propylene carbonate is put into a stirring kettle, and is vacuumized and stirred for 1.5 hours, the mixing temperature is less than or equal to 50 ℃, and the vacuum degree is minus 0.08MPa, so that a well mixed component A is obtained;
d4, 9g of basf 750;9g of polyether 3003LM;19g of polyether polyol; 40.87g aluminum hydroxide with 20.13g alumina; 2.8g of anti-settling agent GARAMITE-1958;0.09g of dibutyl tin dilaurate is put into a stirring kettle, vacuumized and stirred for 1.5 hours, the mixing temperature is less than or equal to 60 ℃, and the vacuum degree is-0.08 MPa, so that the component B is obtained.
Comparative example 1:
the preparation of the bi-component polyurethane heat-conducting pouring sealant adhesive comprises the following steps:
d1, D2 prepolymer is prepared as in example 1, and is not described here again;
d3, 20g of polyurethane prepolymer A and 59g of low-viscosity polyurethane prepolymer B;12g of propylene carbonate is put into a stirring kettle, and is vacuumized and stirred for 1.5 hours, the mixing temperature is less than or equal to 50 ℃, and the vacuum degree is minus 0.08MPa, so that a well mixed component A is obtained;
d4, 13g of basf 750;13g of polyether 3003LM;24g of polyether polyol; 32.83g aluminum hydroxide with 16.17g alumina; 2.8g of anti-settling agent GARAMITE-1958;0.09g of dibutyl tin dilaurate is put into a stirring kettle, vacuumized and stirred for 1.5 hours, the mixing temperature is less than or equal to 60 ℃, and the vacuum degree is minus 0.089MPa, so that the component B is obtained.
Comparative example 2:
the preparation of the bi-component polyurethane heat-conducting pouring sealant adhesive comprises the following steps:
d1, D2 prepolymer is prepared as in example 1, and is not described here again;
d3, mixing 26g of polyurethane prepolymer A and 75g of low-viscosity polyurethane prepolymer B;8g of propylene carbonate is put into a stirring kettle, and is vacuumized and stirred for 1.5 hours, the mixing temperature is less than or equal to 50 ℃, and the vacuum degree is minus 0.08MPa, so that a well mixed component A is obtained;
d4, 8g of basf 750;8g of polyether 3003LM;18g of polyether polyol; 41.54g aluminum hydroxide with 20.46g alumina; 2.8g of anti-settling agent GARAMITE-1958;0.09g of dibutyl tin dilaurate is put into a stirring kettle, vacuumized and stirred for 1.5 hours, the mixing temperature is less than or equal to 60 ℃, and the vacuum degree is-0.08 MPa, so that the component B is obtained.
Comparative example 3:
the preparation of the bi-component polyurethane heat-conducting pouring sealant adhesive comprises the following steps:
d1, D2 prepolymer is prepared as in example 1, and is not described here again;
d3, preparing 23g of polyurethane prepolymer A and 67g of low-viscosity polyurethane prepolymer B;10g of propylene carbonate is put into a stirring kettle, and is vacuumized and stirred for 1.5 hours, the mixing temperature is less than or equal to 50 ℃, and the vacuum degree is minus 0.08MPa, so that a well mixed component A is obtained;
d4, 10.5g polyether 403;10.5g polyether 3003LM;21.1g of polyether polyol; 36.85g aluminum hydroxide with 18.15g alumina; 2.8g of anti-settling agent GARAMITE-1958;0.09g of dibutyl tin dilaurate is put into a stirring kettle, vacuumized and stirred for 1.5 hours, the mixing temperature is less than or equal to 60 ℃, and the vacuum degree is-0.08 MPa, so that the component B is obtained.
Comparative example 4:
the preparation of the bi-component polyurethane heat-conducting pouring sealant adhesive comprises the following steps:
d1, preparing polyurethane prepolymer A: sequentially adding 100g of PPG-3000 into a dry 2L four-mouth bottle, heating to 100 ℃ for vacuum dehydration for 2 hours, cooling to 50 ℃, adding 74g of diphenylmethane diisocyanate, heating to 85 ℃ for reaction for 2.5 hours under the protection of nitrogen, cooling to room temperature when the NCO value is unchanged, discharging to obtain polyurethane prepolymer A, and placing the polyurethane prepolymer A in a dry nitrogen closed container for later use;
d2 polyurethane prepolymer B: as in embodiment 1, the description thereof is omitted here;
d3, mixing 23g of polyurethane prepolymer A and 67g of low-viscosity polyurethane prepolymer B;10g of propylene carbonate is put into a stirring kettle, and is vacuumized and stirred for 1.5 hours, the mixing temperature is less than or equal to 50 ℃, and the vacuum degree is minus 0.08MPa, so that a well mixed component A is obtained;
d4, 10.5g basf 750;10.5g polyether 3003LM;21.1g of polyether polyol; 36.85g aluminum hydroxide with 18.15g alumina; 2.8g of anti-settling agent GARAMITE-1958;0.09g of dibutyl tin dilaurate is put into a stirring kettle, vacuumized and stirred for 1.5 hours, the mixing temperature is less than or equal to 60 ℃, and the vacuum degree is-0.08 MPa, so that the component B is obtained.
Comparative example 5:
the preparation of the bi-component polyurethane heat-conducting pouring sealant adhesive comprises the following steps:
d1, preparing polyurethane prepolymer A: as in embodiment 1, the description thereof is omitted here;
d2, preparing polyurethane prepolymer B: sequentially adding 100g of PPG-7000 into a dried 2L four-mouth bottle, heating to 100 ℃ for vacuum dehydration for 2 hours, cooling to 50 ℃, adding 74g of diphenylmethane diisocyanate, heating to 85 ℃ for reaction for 2.5 hours under the protection of nitrogen, cooling to room temperature when the NCO value is unchanged, discharging to prepare polyurethane prepolymer B, and placing the polyurethane prepolymer B in a dried nitrogen closed container for later use;
d3, preparing 23g of polyurethane prepolymer A and 67g of low-viscosity polyurethane prepolymer B;10g of propylene carbonate is put into a stirring kettle, and is vacuumized and stirred for 1.5 hours, the mixing temperature is less than or equal to 50 ℃, and the vacuum degree is minus 0.08MPa, so that a well mixed component A is obtained;
d4, 10.5g basf 750;10.5g polyether 3003LM;21.1g of polyether polyol; 36.85g aluminum hydroxide with 18.15g alumina; 2.8g of anti-settling agent GARAMITE-1958;0.09g of dibutyl tin dilaurate is put into a stirring kettle, vacuumized and stirred for 1.5 hours, the mixing temperature is less than or equal to 60 ℃, and the vacuum degree is-0.08 MPa, so that the component B is obtained.
Testing
The following performance tests were performed on the adhesives prepared in examples and comparative examples, and the results obtained are shown in table 1:
1. mechanical testing
Measuring the tensile shear strength of GB/T7124-2008 adhesive;
measurement of the elongation at break of GB/T2567-2008 adhesive.
2. Burn-in test
Aging box temperature, humidity conditions: 85 ℃ and 85%;
aging time: 1000h.
3. Ultraviolet aging test
An ultraviolet aging test box;
aging for 100h;
sample testing standard GB 13022-1991;
measurement of GB/T7124-2008 adhesive tensile shear Strength.
4. Cold and hot impact resistance test
High and low temperature impact 1000 cycles, -30-60 ℃;
measurement of GB/T7124-2008 adhesive tensile shear Strength.
5. Peel test: GB/T2792-2014.
Table 1 comparison of test data for examples and comparative examples
As can be seen from the test results in Table 1, the two-component polyurethane adhesive in the embodiment of the invention has excellent mechanical properties and can maintain good bonding and sealing effects in the long-term use process; greatly improves the ultraviolet resistance, weather resistance and chemical resistance; the combination of the natural oil polyol and the prepolymer can also endow the product with good hydrophobic performance, thereby avoiding the phenomenon of air bubbles.
Another: the viscosity of the prepared bi-component polyurethane heat conduction potting adhesive comprises A, B components by adopting a Brookfield viscometer with a #14 rotor, wherein the overall viscosity of the component A is less than 3500cps at 25 ℃, and the overall viscosity of the component B is less than 1500cps at 25 ℃; the low-viscosity system ensures the flowing property and leveling property, and is suitable for filling and sealing a complex structure; the pouring sealant adhesive can be applied to the pouring of electronic components with high heat.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (10)
1. The double-component polyurethane heat-conducting pouring sealant adhesive is characterized by comprising the following components in parts by weight:
and (3) a component A: 21-25 parts of low-viscosity polyurethane prepolymer A; 60-74 parts of low-viscosity polyurethane prepolymer B; 9-11 parts of non-reactive plasticizer;
the polyurethane prepolymer A is an NCO-terminated polymer, and the molar ratio of isocyanate groups to hydroxyl groups is 1.5-2.2:1, a step of; the polyurethane prepolymer B is an NCO-terminated polymer, and the molar ratio of isocyanate groups to hydroxyl groups is 2.5-3.0:1, the viscosity is 800-1600 mPa.s;
and the component B comprises the following components: 9-12 parts of natural grease polyol; 9-12 parts of non-polyester polyol; 19-23 parts of polyether polyol; 50-61 parts of composite filler; 1-3 parts of an anti-settling agent; 0.05-0.5 part of catalyst;
the volume ratio of the component A to the component B is 1:1.
2. The two-part polyurethane heat conducting potting adhesive of claim 1, wherein the low viscosity polyurethane prepolymer a is a polymer containing terminal NCO produced by the reaction of the following raw materials in weight percent: 50-70% of polyether triol and 30-50% of diisocyanate.
3. The two-part polyurethane heat conducting potting adhesive of claim 1, wherein the low viscosity polyurethane prepolymer B is a polymer containing terminal NCO produced by the reaction of the following raw materials in weight percent: 35-60% of polyether triol and 40-65% of diisocyanate.
4. The two-component polyurethane heat-conducting pouring sealant adhesive according to claim 2, wherein the raw material polyether triol of the low-viscosity polyurethane prepolymer A has an average molecular weight of 2000-5000; the diisocyanate is at least one of toluene diisocyanate, diphenylmethane diisocyanate and diphenylmethane diisocyanate.
5. The two-component polyurethane heat-conducting pouring sealant adhesive according to claim 3, wherein the raw material polyether triol of the low-viscosity polyurethane prepolymer B has an average molecular weight of 6000-12000; the diisocyanate is at least one of toluene diisocyanate, diphenylmethane diisocyanate and hexamethylene diisocyanate.
6. The two-component polyurethane heat-conducting pouring sealant adhesive according to claim 1, wherein the natural oil polyol is basf 750 and has a viscosity of 5000-7000mpa.s; the polyether polyol is the Dow polyether VORANOL 3003LM with the viscosity 604mPa.S.
7. The two-component polyurethane heat-conducting pouring sealant adhesive according to claim 1, wherein the hydroxyl value of the non-polyester polyol is 200-300mg KOH/g, and the non-polyester polyol is one of polyoxypropylene glycol, polyoxypropylene triol and polypropylene glycol.
8. The two-part polyurethane heat conducting potting adhesive of claim 1, wherein the non-reactive plasticizer comprises propylene carbonate, triethyl phosphate.
9. The two-component polyurethane heat-conducting pouring sealant adhesive according to claim 1, wherein the catalyst is one or a combination of two or more of dibutyl tin dilaurate, organic bismuth and organic zinc.
10. A method for preparing the two-component polyurethane heat-conducting pouring sealant adhesive as claimed in any one of claims 1 to 9, which comprises the following steps:
d1, preparing polyurethane prepolymer A: according to weight percentage, putting polyether triol into a flask, heating to 100-110 ℃, vacuumizing to remove water, cooling to 45-55 ℃, adding diisocyanate, reacting under the protection of nitrogen, heating to 80-85 ℃ and continuously heating for 2-3h until NCO value is unchanged, and cooling to room temperature to obtain polyurethane prepolymer A;
d2, preparing polyurethane prepolymer B: according to weight percentage, putting polyether triol into a flask, heating to 100-110 ℃, vacuumizing to remove water, cooling to 45-55 ℃, adding diisocyanate, reacting under the protection of nitrogen, heating to 80-85 ℃ and continuously heating for 2-3h until NCO value is unchanged, and cooling to room temperature to obtain polyurethane prepolymer B;
d3, 21-25 parts of low-viscosity polyurethane prepolymer A; 60-74 parts of low-viscosity polyurethane prepolymer B; 9-11 parts of non-reactive plasticizer are put into a stirring kettle, and are vacuumized and stirred for 1-2 hours, the mixing temperature is less than or equal to 50 ℃, and the vacuum degree is minus 0.08 to minus 0.09MPa, so that a component A is obtained;
d4, 9-12 parts of natural grease polyol; 9-12 parts of a non-polyester polyol; 19-23 parts of polyether polyol; 50-61 parts of composite filler; 1-3 parts of an anti-settling agent; and (3) adding 0.05-0.5 part of catalyst into a stirring kettle, vacuumizing and stirring for 1-2 hours, wherein the mixing temperature is less than or equal to 60 ℃, and the vacuum degree is minus 0.08-minus 0.09MPa, so as to obtain the component B.
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| CN202311830435.4A CN117683508A (en) | 2023-12-28 | 2023-12-28 | Double-component polyurethane heat-conducting pouring sealant adhesive and preparation method thereof |
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| CN202311830435.4A CN117683508A (en) | 2023-12-28 | 2023-12-28 | Double-component polyurethane heat-conducting pouring sealant adhesive and preparation method thereof |
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