CN113943546A - Two-component silicone pouring sealant for electrical components and preparation method thereof - Google Patents
Two-component silicone pouring sealant for electrical components and preparation method thereof Download PDFInfo
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- CN113943546A CN113943546A CN202111261079.XA CN202111261079A CN113943546A CN 113943546 A CN113943546 A CN 113943546A CN 202111261079 A CN202111261079 A CN 202111261079A CN 113943546 A CN113943546 A CN 113943546A
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- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 41
- 239000000565 sealant Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 22
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 20
- 239000003063 flame retardant Substances 0.000 claims abstract description 18
- 239000004970 Chain extender Substances 0.000 claims abstract description 17
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000007822 coupling agent Substances 0.000 claims abstract description 14
- 239000002270 dispersing agent Substances 0.000 claims abstract description 13
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims abstract description 12
- 239000003054 catalyst Substances 0.000 claims abstract description 12
- 239000012975 dibutyltin dilaurate Substances 0.000 claims abstract description 12
- 239000000945 filler Substances 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 12
- 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 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000654 additive Substances 0.000 claims abstract description 5
- 230000000996 additive effect Effects 0.000 claims abstract description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 19
- 239000000853 adhesive Substances 0.000 claims description 17
- 230000001070 adhesive effect Effects 0.000 claims description 17
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 13
- 229910021485 fumed silica Inorganic materials 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 239000004408 titanium dioxide Substances 0.000 claims description 10
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical group [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 9
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 claims description 9
- 238000004382 potting Methods 0.000 claims description 9
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 claims description 9
- IBOFVQJTBBUKMU-UHFFFAOYSA-N 4,4'-methylene-bis-(2-chloroaniline) Chemical compound C1=C(Cl)C(N)=CC=C1CC1=CC=C(N)C(Cl)=C1 IBOFVQJTBBUKMU-UHFFFAOYSA-N 0.000 claims description 7
- 241001112258 Moca Species 0.000 claims description 6
- 239000003292 glue Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000006229 carbon black Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000000498 cooling water Substances 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 5
- 239000011229 interlayer Substances 0.000 claims description 5
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 4
- 150000001412 amines Chemical group 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 229920002545 silicone oil Polymers 0.000 claims description 4
- 239000005995 Aluminium silicate Substances 0.000 claims description 2
- DTCPBBPYYOBKGN-UHFFFAOYSA-N N,N-dihydroxy-2,3-di(propan-2-yl)aniline Chemical compound ON(C1=C(C(=CC=C1)C(C)C)C(C)C)O DTCPBBPYYOBKGN-UHFFFAOYSA-N 0.000 claims description 2
- 239000004952 Polyamide Substances 0.000 claims description 2
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical group [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 claims description 2
- 235000012211 aluminium silicate Nutrition 0.000 claims description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 2
- 229920002647 polyamide Polymers 0.000 claims description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 230000003993 interaction Effects 0.000 abstract 1
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 9
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 9
- 238000012360 testing method Methods 0.000 description 8
- 238000004132 cross linking Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000010998 test method Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 230000002265 prevention Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000007790 scraping Methods 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- XSAOTYCWGCRGCP-UHFFFAOYSA-K aluminum;diethylphosphinate Chemical compound [Al+3].CCP([O-])(=O)CC.CCP([O-])(=O)CC.CCP([O-])(=O)CC XSAOTYCWGCRGCP-UHFFFAOYSA-K 0.000 description 2
- ZQKXQUJXLSSJCH-UHFFFAOYSA-N melamine cyanurate Chemical compound NC1=NC(N)=NC(N)=N1.O=C1NC(=O)NC(=O)N1 ZQKXQUJXLSSJCH-UHFFFAOYSA-N 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006757 chemical reactions by type Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- PKTOVQRKCNPVKY-UHFFFAOYSA-N dimethoxy(methyl)silicon Chemical compound CO[Si](C)OC PKTOVQRKCNPVKY-UHFFFAOYSA-N 0.000 description 1
- WHGNXNCOTZPEEK-UHFFFAOYSA-N dimethoxy-methyl-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](C)(OC)CCCOCC1CO1 WHGNXNCOTZPEEK-UHFFFAOYSA-N 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- 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
-
- 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
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to a two-component silicone pouring sealant for electrical components, which comprises a component A and a component B, wherein the component A comprises the following components in parts by weight: 800-930 parts of hydroxyl-terminated polydimethylsiloxane, 15-25 parts of white slurry, 5-10 parts of filler, 1-2 parts of chain extender, 0.5-1 part of coupling agent, 1-2 parts of dibutyltin dilaurate catalyst, 30-40 parts of flame retardant and 50-100 parts of heat conducting agent; the component B comprises: 400-450 parts of additive, 150-250 parts of powdery filler, 10-20 parts of black paste, 5-10 parts of dispersing agent, 3-6 parts of water, 20-40 parts of coupling agent, 100-150 parts of ethyl orthosilicate and 150-250 parts of n-heptane; the component A comprises: and the component B is (2-2.2): 1. the invention can improve the mixing degree of the raw materials and realize the interaction of the raw materials, thereby ensuring the preparation and the use of the pouring sealant.
Description
Technical Field
The invention belongs to the field of adhesives, and particularly relates to a two-component silicone pouring sealant for electrical components and a preparation method thereof.
Background
Along with the rapid development of electronic technology, electronic components are developed towards higher power, higher performance and miniaturization and densification, and meanwhile, along with the continuous widening of the field, the use environment of the electronic components is also more and more harsh. The pouring sealant is also called electronic glue and is used for bonding, sealing, encapsulating and coating protection of electronic components. The pouring sealant is used for sealing the electrical appliance element, and can play roles of moisture prevention, dust prevention, insulation, shock prevention and the like after curing.
Currently, silicone potting adhesives on the market are in many reaction types such as dealcoholization type, ketoxime type, deacidification type and the like, and basically adopt a form of two-component use. The reaction activity of two components in the existing two-component silicone pouring sealant is generally poor, so that the cross-linking density is low, the curing strength and hardness are poor, and the performance of the two-component silicone pouring sealant is influenced finally.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the two-component silicone pouring sealant for the electrical element and the preparation method thereof, which can improve the reaction activity, increase the cross-linking density, improve the pouring strength of the pouring sealant, improve the curing strength and hardness and enhance the thermal conductivity, thereby ensuring the preparation and the use of the pouring sealant.
The first purpose of the invention is to provide a two-component silicone pouring sealant for electrical components, which comprises a component A and a component B, wherein the component A and the component B are respectively prepared by weight parts,
the component A comprises: 800-930 parts of hydroxyl-terminated polydimethylsiloxane, 15-25 parts of white slurry, 5-10 parts of filler, 1-2 parts of chain extender, 0.5-1 part of coupling agent, 1-2 parts of dibutyltin dilaurate catalyst, 30-40 parts of flame retardant and 50-100 parts of heat conducting agent;
the component B comprises: 400-450 parts of additive, 150-250 parts of powdery filler, 10-20 parts of black paste, 5-10 parts of dispersing agent, 3-6 parts of water, 20-40 parts of coupling agent, 100-150 parts of ethyl orthosilicate and 150-250 parts of n-heptane;
the component A comprises: and the component B is (2-2.2): 1.
further, in the component A, the viscosity of the hydroxyl-terminated polydimethylsiloxane at 25 ℃ is one or two of 3000cps and 20000 cps.
Further, in the component A, the filler is one or more of fumed silica, polyamide wax and kaolin, the chain extender is a liquid amine chain extender, the liquid amine chain extender is one or more of liquid MOCA (3,3 '-dichloro-4, 4' -diaminodiphenylmethane), ethylenediamine and N, N-dihydroxy (diisopropyl) aniline, the flame retardant is a nitrogen-phosphorus halogen-free flame retardant, and the heat conducting agent is aluminum hydroxide.
Further, in the component A, the white slurry is a ground mixture of DOP (dioctyl phthalate) and titanium dioxide; in the component B, the black paste is a ground mixture of DOP, carbon black and a dispersant, and the dispersant is one or more of BYK161, BYK163 and BYK 972.
Further, in the component A, the coupling agent is one or more of silane coupling agents KH-792 (gamma-aminoethyl aminopropyl trimethoxysilane), KH-103 (gamma-diethylene triaminopropyl methyldimethoxysilane) and KH-550 (gamma-aminopropyl triethoxysilane); in the component B, the coupling agent is one or more of silane coupling agents KH-560 (3-glycidoxypropyltrimethoxysilane), KH-561 (3-glycidoxypropyltriethoxysilane) and KH-562 (3-glycidoxypropylmethyldimethoxysilane).
Further, in the component B, the additive is one or more of methyl silicone oil, hydroxyl silicone oil and vinyl silicone oil, and the powdery filler is one or two of titanium dioxide and fumed silica.
The second purpose of the invention is to provide a preparation method of the two-component silicone pouring sealant for the electrical components, which comprises the following steps:
preparation of the component A:
adding hydroxyl-terminated polydimethylsiloxane and white slurry into a reaction kettle for preparing the adhesive, adjusting the rotating speed, dispersing at a high speed, and dehydrating in vacuum at 90-110 ℃ for 2-3 h; stopping heating, discharging hot water in the interlayer, starting circulating cooling water, adjusting the rotating speed, dispersing at a high speed, cooling to 30-40 ℃, and additionally adding a filler, a chain extender, a coupling agent, a dibutyltin dilaurate catalyst, a flame retardant and a heat conducting agent to obtain a component A;
preparation of the component B:
adding the reaction raw materials of the component B into a reaction kettle for preparing the glue, adjusting the rotating speed to scrape the edges, dispersing at a high speed, and stirring in vacuum for 1-2 hours to obtain the component B;
the preparation method of the two-component silicone pouring sealant comprises the following steps:
and mixing the component A and the component B according to the mass ratio, and uniformly stirring to obtain the two-component silicone pouring sealant.
Compared with the prior art, the invention has the following beneficial effects:
(1) the water in the component B can be used as a cocatalyst to hydrolyze ethyl orthosilicate into orthosilicate anhydride, so that the reaction activity of the orthosilicate anhydride and the hydroxyl-terminated polydimethylsiloxane is higher under the action of a dibutyltin dilaurate catalyst in the mixing process of the component A and the component B, the crosslinking density can be increased, and the curing strength and hardness are improved;
(2) the two-component silicone pouring sealant provided by the invention is medium-hardness condensed type pouring silicone rubber, and has good leveling property and excellent process operability; the flexibility and the impact resistance are good; excellent heat resistance, moisture resistance and cold resistance; the adhesive has excellent adhesion to PC shells, LED lamp tubes, PCB boards and the like without using other primers; has excellent moisture-proof and waterproof effects;
(3) according to the component B provided by the invention, water and n-heptane are used as solvents, and the combination of water-based solvents and oil-based solvents can reduce the viscosity of the component B, so that the raw materials can be fully mixed, and the preparation and use of the pouring sealant can be ensured; the heat is released in the mixing and curing process, so that n-heptane can be volatilized, and alkyl impurities cannot be introduced;
(4) in the component A provided by the invention, a silane coupling agent KH-792 of diamine functional group silanes can be used, and the crosslinking speed between raw materials is controlled; the component B can use a coupling agent KH-560 containing an epoxy group to control the curing hardness of the product; under the combined action of the two coupling agents, the adhesive force of the product can be greatly improved, so that the sealing performance of the product is improved;
(5) the component A provided by the invention uses white paste, the component B uses black paste, the component A and the component B can present gray after being mixed, and the uniform degree of mixing of the component A and the component B can be judged according to whether the gray is uniform, so that the preparation and the use of the pouring sealant are ensured;
(6) the component A provided by the invention can use aluminum hydroxide, and can be used as a flame retardant to improve the flame retardant property of the product together with a halogen-free flame retardant; but also can be used as a heat-conducting agent to improve the heat-conducting property of the product.
Detailed Description
The principles and features of this invention are described in conjunction with the following examples, which are intended to illustrate the invention, but not to limit the scope of the invention, in which the amounts are in parts by weight.
Example 1
A two-component silicone pouring sealant for electrical components comprises a component A and a component B, which are calculated according to parts by weight,
the component A comprises: 600 parts of hydroxyl-terminated polydimethylsiloxane (viscosity of 3000cps at 25 ℃), 200 parts of hydroxyl-terminated polydimethylsiloxane (viscosity of 20000cps at 25 ℃), 15 parts of white slurry, 5 parts of fumed silica, 1 part of chain extender liquid MOCA, 0.5 part of silane coupling agent KH-792, 1 part of dibutyltin dilaurate catalyst, 30 parts of halogen-free flame retardant Kelain Exolit OP 1230 (aluminum diethylphosphinate), 50 parts of aluminum hydroxide;
the component B comprises: 400 parts of methyl silicone oil, 120 parts of titanium dioxide, 30 parts of fumed silica, 10 parts of black paste, 5 parts of dispersant BYK161, 3 parts of water, 20 parts of silane coupling agent KH-560, 100 parts of tetraethoxysilane and 150 parts of n-heptane;
wherein the white paste is a ground mixture of DOP and titanium dioxide, and the black paste is a ground mixture of DOP, carbon black and a dispersing agent;
the component A comprises: the component B is 2: 1.
the preparation method of the two-component silicone pouring sealant comprises the following steps:
preparation of component A:
adding hydroxyl-terminated polydimethylsiloxane and white slurry into a reaction kettle for preparing the adhesive, adjusting the rotating speed, dispersing at a high speed, and dehydrating in vacuum at 90 ℃ for 2 hours; stopping heating, discharging hot water in the interlayer, starting circulating cooling water, adjusting the rotating speed, dispersing at a high speed, cooling to 30 ℃, and additionally adding fumed silica, chain extender liquid MOCA, silane coupling agent KH-792, dibutyltin dilaurate catalyst, halogen-free flame retardant Kelain Exolit OP 1230 and aluminum hydroxide to obtain a component A;
preparation of the component B:
adding the reaction raw materials of the component B into a reaction kettle for preparing the glue, adjusting the rotating speed, scraping, dispersing at a high speed, and stirring in vacuum for 1h to obtain the component B;
preparing the two-component silicone pouring sealant:
mixing the component A and the component B according to the proportion of 2: 1, and uniformly stirring to obtain the double-component silicone pouring sealant.
Example 2
A two-component silicone pouring sealant for electrical components comprises a component A and a component B, which are calculated according to parts by weight,
the component A comprises: 650 parts of hydroxyl-terminated polydimethylsiloxane (viscosity of 3000cps at 25 ℃), 280 parts of hydroxyl-terminated polydimethylsiloxane (viscosity of 20000cps at 25 ℃), 25 parts of white slurry, 10 parts of fumed silica, 2 parts of chain extender ethylenediamine, 1 part of silane coupling agent KH-792, 2 parts of dibutyltin dilaurate catalyst, 40 parts of halogen-free flame retardant melamine cyanurate and 100 parts of aluminum hydroxide;
the component B comprises: 450 parts of methyl silicone oil, 180 parts of titanium dioxide, 70 parts of fumed silica, 20 parts of black paste, 10 parts of a dispersing agent BYK972, 6 parts of water, 40 parts of a silane coupling agent KH-560, 150 parts of tetraethoxysilane and 250 parts of n-heptane;
wherein the white paste is a ground mixture of DOP and titanium dioxide, and the black paste is a ground mixture of DOP, carbon black and a dispersing agent;
the component A comprises: component B is 2.2: 1.
the preparation method of the two-component silicone pouring sealant comprises the following steps:
preparation of component A:
adding hydroxyl-terminated polydimethylsiloxane and white slurry into a reaction kettle for preparing the adhesive, adjusting the rotating speed, dispersing at a high speed, and dehydrating in vacuum at 110 ℃ for 3 hours; stopping heating, discharging hot water in the interlayer, starting circulating cooling water, adjusting the rotating speed, dispersing at a high speed, cooling to 40 ℃, and additionally adding fumed silica, chain extender ethylenediamine, silane coupling agent KH-792, dibutyltin dilaurate catalyst, halogen-free flame retardant melamine cyanurate and aluminum hydroxide to obtain a component A;
preparation of the component B:
adding the reaction raw materials of the component B into a reaction kettle for preparing the glue, adjusting the rotating speed, scraping, dispersing at a high speed, and stirring in vacuum for 2 hours to obtain the component B;
preparing the two-component silicone pouring sealant:
mixing the component A and the component B according to the proportion of 2.2: 1, and uniformly stirring to obtain the double-component silicone pouring sealant.
Example 3
A two-component silicone pouring sealant for electrical components comprises a component A and a component B, which are calculated according to parts by weight,
the component A comprises: 610 parts of hydroxyl-terminated polydimethylsiloxane (viscosity of 3000cps at 25 ℃), 240 parts of hydroxyl-terminated polydimethylsiloxane (viscosity of 20000cps at 25 ℃), 17 parts of white slurry, 10 parts of fumed silica, 1 part of chain extender liquid MOCA, 1 part of silane coupling agent KH-792, 1 part of dibutyltin dilaurate catalyst, 35 parts of halogen-free flame retardant Kelain Exolit OP 1230 (aluminum diethylphosphinate), 80 parts of aluminum hydroxide;
the component B comprises: 420 parts of methyl silicone oil, 200 parts of titanium dioxide, 15 parts of fumed silica, 10 parts of black paste, 10 parts of a dispersing agent BYK161, 5 parts of water, 30 parts of a silane coupling agent KH-560, 110 parts of tetraethoxysilane and 200 parts of n-heptane;
wherein the white paste is a ground mixture of DOP and titanium dioxide, and the black paste is a ground mixture of DOP, carbon black and a dispersing agent;
the component A comprises: the component B is 2: 1.
the preparation method of the two-component silicone pouring sealant comprises the following steps:
preparation of component A:
adding hydroxyl-terminated polydimethylsiloxane and white slurry into a reaction kettle for preparing the adhesive, adjusting the rotating speed, dispersing at a high speed, and dehydrating in vacuum at 100 ℃ for 2 hours; stopping heating, discharging hot water in the interlayer, starting circulating cooling water, adjusting the rotating speed, dispersing at a high speed, cooling to 40 ℃, and additionally adding fumed silica, chain extender liquid MOCA, silane coupling agent KH-792, dibutyltin dilaurate catalyst, halogen-free flame retardant Kelain Exolit OP 1230 and aluminum hydroxide to obtain a component A;
preparation of the component B:
adding the reaction raw materials of the component B into a reaction kettle for preparing the glue, adjusting the rotating speed, scraping, dispersing at a high speed, and stirring in vacuum for 1h to obtain the component B;
preparing the two-component silicone pouring sealant:
mixing the component A and the component B according to the proportion of 2: 1, and uniformly stirring to obtain the double-component silicone pouring sealant.
Comparative example
Referring to example 1, the difference from example 1 is that the B component does not include water and n-heptane.
Description of the test methods:
(1) the operation time testing method comprises the following steps: testing the operating time according to GB/T13477.5;
(2) the initial fixation time test method comprises the following steps: testing initial fixation time according to Q/HSM 34-2008;
(3) the hardness test method comprises the following steps: testing the hardness according to GB/T531-2008;
(4) tensile strength test method: testing the tensile strength according to GB/T-528;
(5) the temperature resistance test method comprises the following steps: pouring the two-component silicone pouring sealant to the head of the heating pipe, standing and curing for 24 hours, and testing the temperature resistance of the two-component silicone pouring sealant at 200 ℃.
The test data of each example and comparative example are shown in table 1.
TABLE 1 data of test experiments for examples and comparative examples
Compared with the comparative example, the two-component silicone pouring sealant obtained in the embodiment of the invention has longer operation time and shorter initial curing time, has higher hardness and relatively higher strength after being completely cured, and can ensure the temperature resistance; the preparation method of the invention can improve the reaction activity, increase the cross-linking density, improve the encapsulation strength of the pouring sealant, and improve the curing strength and hardness, thereby ensuring the preparation and use of the pouring sealant.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A two-component silicone pouring sealant for electrical components comprises a component A and a component B, and is characterized in that the two-component silicone pouring sealant comprises the following components in parts by weight,
the component A comprises: 800-930 parts of hydroxyl-terminated polydimethylsiloxane, 15-25 parts of white slurry, 5-10 parts of filler, 1-2 parts of chain extender, 0.5-1 part of coupling agent, 1-2 parts of dibutyltin dilaurate catalyst, 30-40 parts of flame retardant and 50-100 parts of heat conducting agent;
the component B comprises: 400-450 parts of additive, 150-250 parts of powdery filler, 10-20 parts of black paste, 5-10 parts of dispersing agent, 3-6 parts of water, 20-40 parts of coupling agent, 100-150 parts of ethyl orthosilicate and 150-250 parts of n-heptane;
the component A comprises: and the component B is (2-2.2): 1.
2. the two-component silicone potting adhesive for electrical components of claim 1, wherein in the component A, the hydroxyl-terminated polydimethylsiloxane has one or two of a viscosity of 3000cps and a viscosity of 20000cps at 25 ℃.
3. The two-component silicone potting adhesive for electrical components of claim 1, wherein in the component A, the white paste is a ground mixture of DOP and titanium dioxide; in the component B, the black paste is a ground mixture of DOP, carbon black and a dispersant, and the dispersant is one or more of BYK161, BYK163 and BYK 972.
4. The two-component silicone potting adhesive for electrical components of claim 1, wherein in the component A, the filler is one or more of fumed silica, polyamide wax and kaolin.
5. The two-component silicone potting adhesive for electrical components of claim 1, wherein in the component A, the chain extender is a liquid amine chain extender, and the liquid amine chain extender is one or more of liquid MOCA, ethylenediamine and N, N-dihydroxy (diisopropyl) aniline.
6. The two-component silicone potting adhesive for electrical components of claim 1, wherein in the component a, the coupling agent is one or more of silane coupling agents KH-792, KH-103 and KH-550; in the component B, the coupling agent is one or more of silane coupling agents KH-560, KH-561 and KH-562.
7. The two-component silicone potting adhesive for electrical components of claim 1, wherein in the component A, the flame retardant is nitrogen-phosphorus halogen-free flame retardant, and the heat conducting agent is aluminum hydroxide.
8. The two-component silicone potting adhesive for electrical components of claim 1, wherein in the component B, the additive is one or more of methyl silicone oil, hydroxy silicone oil and vinyl silicone oil.
9. The two-component silicone potting adhesive for electrical components of claim 1, wherein in the component B, the powdery filler is one or two of titanium dioxide and fumed silica.
10. A method for preparing the two-component silicone pouring sealant for electrical components according to any one of claims 1 to 9,
preparation of the component A:
adding hydroxyl-terminated polydimethylsiloxane and white slurry into a reaction kettle for preparing the adhesive, adjusting the rotating speed, dispersing at a high speed, and dehydrating in vacuum at 90-110 ℃ for 2-3 h; stopping heating, discharging hot water in the interlayer, starting circulating cooling water, adjusting the rotating speed, dispersing at a high speed, cooling to 30-40 ℃, and additionally adding a filler, a chain extender, a coupling agent, a dibutyltin dilaurate catalyst, a flame retardant and a heat conducting agent to obtain a component A;
preparation of the component B:
adding the reaction raw materials of the component B into a reaction kettle for preparing the glue, adjusting the rotating speed to scrape the edges, dispersing at a high speed, and stirring in vacuum for 1-2 hours to obtain the component B;
the preparation method of the two-component silicone pouring sealant comprises the following steps:
and mixing the component A and the component B according to the mass ratio, and uniformly stirring to obtain the two-component silicone pouring sealant.
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| CN115386293A (en) * | 2022-09-22 | 2022-11-25 | 杭州赛维动力科技有限公司 | Sprayable silicone adhesive for power equipment and preparation method thereof |
| CN115894937A (en) * | 2022-11-23 | 2023-04-04 | 新纳奇材料科技江苏有限公司 | High-strength silicone resin and preparation method thereof |
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