CN115368863A - Heat-resistant high-resilience asparagus polyurea pouring sealant and preparation method thereof - Google Patents
Heat-resistant high-resilience asparagus polyurea pouring sealant and preparation method thereof Download PDFInfo
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- CN115368863A CN115368863A CN202211172180.2A CN202211172180A CN115368863A CN 115368863 A CN115368863 A CN 115368863A CN 202211172180 A CN202211172180 A CN 202211172180A CN 115368863 A CN115368863 A CN 115368863A
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- pouring sealant
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- resilience
- heat
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- 239000000565 sealant Substances 0.000 title claims abstract description 97
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 229920002396 Polyurea Polymers 0.000 title claims abstract description 26
- 235000005340 Asparagus officinalis Nutrition 0.000 title abstract description 4
- 244000003416 Asparagus officinalis Species 0.000 title abstract 2
- 150000002148 esters Chemical class 0.000 claims abstract description 50
- 229920005989 resin Polymers 0.000 claims abstract description 47
- 239000011347 resin Substances 0.000 claims abstract description 47
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 46
- 239000000945 filler Substances 0.000 claims abstract description 42
- 238000003756 stirring Methods 0.000 claims abstract description 42
- 229920000805 Polyaspartic acid Polymers 0.000 claims abstract description 33
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 33
- 108010064470 polyaspartate Proteins 0.000 claims abstract description 33
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 27
- 229920000642 polymer Polymers 0.000 claims abstract description 25
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 23
- -1 aspartyl Chemical group 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 150000003335 secondary amines Chemical class 0.000 claims description 50
- 229920000608 Polyaspartic Polymers 0.000 claims description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 11
- LVASCWIMLIKXLA-CABCVRRESA-N 7-bromo-6-chloro-3-[3-[(2r,3s)-3-hydroxypiperidin-2-yl]-2-oxopropyl]quinazolin-4-one Chemical compound O[C@H]1CCCN[C@@H]1CC(=O)CN1C(=O)C2=CC(Cl)=C(Br)C=C2N=C1 LVASCWIMLIKXLA-CABCVRRESA-N 0.000 claims description 9
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 239000010703 silicon Substances 0.000 claims description 9
- 239000011668 ascorbic acid Substances 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- 241000276489 Merlangius merlangus Species 0.000 claims description 4
- 239000004148 curcumin Substances 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 4
- 239000002270 dispersing agent Substances 0.000 claims description 2
- YZZTZUHVGICSCS-UHFFFAOYSA-N n-butan-2-yl-4-[[4-(butan-2-ylamino)phenyl]methyl]aniline Chemical compound C1=CC(NC(C)CC)=CC=C1CC1=CC=C(NC(C)CC)C=C1 YZZTZUHVGICSCS-UHFFFAOYSA-N 0.000 claims description 2
- 125000000467 secondary amino group Chemical class [H]N([*:1])[*:2] 0.000 abstract description 5
- 230000009467 reduction Effects 0.000 abstract description 4
- 239000000084 colloidal system Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 14
- 229920002635 polyurethane Polymers 0.000 description 10
- 239000004814 polyurethane Substances 0.000 description 10
- 238000004382 potting Methods 0.000 description 10
- 230000001070 adhesive effect Effects 0.000 description 9
- 239000000853 adhesive Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 229920003225 polyurethane elastomer Polymers 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000003292 glue Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 239000000377 silicon dioxide Substances 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- 239000012948 isocyanate Substances 0.000 description 5
- 238000005086 pumping Methods 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- KXDHJXZQYSOELW-UHFFFAOYSA-M Carbamate Chemical compound NC([O-])=O KXDHJXZQYSOELW-UHFFFAOYSA-M 0.000 description 4
- 239000004202 carbamide Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 150000002513 isocyanates Chemical class 0.000 description 4
- 229910002012 Aerosil® Inorganic materials 0.000 description 3
- 125000003277 amino group Chemical group 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- 238000005266 casting Methods 0.000 description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 3
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 3
- 241000234427 Asparagus Species 0.000 description 2
- 108010011485 Aspartame Proteins 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- 239000000605 aspartame Substances 0.000 description 2
- IAOZJIPTCAWIRG-QWRGUYRKSA-N aspartame Chemical compound OC(=O)C[C@H](N)C(=O)N[C@H](C(=O)OC)CC1=CC=CC=C1 IAOZJIPTCAWIRG-QWRGUYRKSA-N 0.000 description 2
- 229960003438 aspartame Drugs 0.000 description 2
- 235000010357 aspartame Nutrition 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 125000001951 carbamoylamino group Chemical group C(N)(=O)N* 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005538 encapsulation Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 239000011863 silicon-based powder Substances 0.000 description 2
- 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 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000007551 Shore hardness test Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229960004717 insulin aspart Drugs 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- APUGANPCBWRHBD-UHFFFAOYSA-N n,n'-di(butan-2-yl)-1,1-diphenylmethanediamine Chemical compound C=1C=CC=CC=1C(NC(C)CC)(NC(C)CC)C1=CC=CC=C1 APUGANPCBWRHBD-UHFFFAOYSA-N 0.000 description 1
- VOMXSOIBEJBQNF-UTTRGDHVSA-N novorapid Chemical compound C([C@H](NC(=O)[C@H](CC(C)C)NC(=O)[C@H](CO)NC(=O)[C@H](CS)NC(=O)[C@H]([C@@H](C)CC)NC(=O)[C@H](CO)NC(=O)[C@H]([C@@H](C)O)NC(=O)[C@H](CS)NC(=O)[C@H](CS)NC(=O)[C@H](CCC(N)=O)NC(=O)[C@H](CCC(O)=O)NC(=O)[C@H](C(C)C)NC(=O)[C@@H](NC(=O)CN)[C@@H](C)CC)C(=O)N[C@@H](CCC(N)=O)C(=O)N[C@@H](CC(C)C)C(=O)N[C@@H](CCC(O)=O)C(=O)N[C@@H](CC(N)=O)C(=O)N[C@@H](CC=1C=CC(O)=CC=1)C(=O)N[C@@H](CS)C(=O)N[C@@H](CC(N)=O)C(O)=O)C1=CC=C(O)C=C1.C([C@@H](C(=O)N[C@@H](CC(C)C)C(=O)N[C@H](C(=O)N[C@@H](CCC(O)=O)C(=O)N[C@@H](C)C(=O)N[C@@H](CC(C)C)C(=O)N[C@@H](CC=1C=CC(O)=CC=1)C(=O)N[C@@H](CC(C)C)C(=O)N[C@@H](C(C)C)C(=O)N[C@@H](CS)C(=O)NCC(=O)N[C@@H](CCC(O)=O)C(=O)N[C@@H](CCCNC(N)=N)C(=O)NCC(=O)N[C@@H](CC=1C=CC=CC=1)C(=O)N[C@@H](CC=1C=CC=CC=1)C(=O)N[C@@H](CC=1C=CC(O)=CC=1)C(=O)N[C@@H]([C@@H](C)O)C(=O)N[C@@H](CC(O)=O)C(=O)N[C@@H](CCCCN)C(=O)N[C@@H]([C@@H](C)O)C(O)=O)C(C)C)NC(=O)[C@H](CO)NC(=O)CNC(=O)[C@H](CS)NC(=O)[C@H](CC(C)C)NC(=O)[C@H](CC=1NC=NC=1)NC(=O)[C@H](CCC(N)=O)NC(=O)[C@H](CC(N)=O)NC(=O)[C@@H](NC(=O)[C@@H](N)CC=1C=CC=CC=1)C(C)C)C1=CN=CN1 VOMXSOIBEJBQNF-UTTRGDHVSA-N 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920005906 polyester polyol Polymers 0.000 description 1
- 239000011527 polyurethane coating Substances 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000004634 thermosetting polymer Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-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
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/02—Polyureas
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3225—Polyamines
- C08G18/325—Polyamines containing secondary or tertiary amino groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
- C08G18/4081—Mixtures of compounds of group C08G18/64 with other macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/64—Macromolecular compounds not provided for by groups C08G18/42 - C08G18/63
- C08G18/6415—Macromolecular compounds not provided for by groups C08G18/42 - C08G18/63 having nitrogen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6633—Compounds of group C08G18/42
- C08G18/6637—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6648—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3225 or C08G18/3271 and/or polyamines of C08G18/38
- C08G18/6651—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3225 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3225 or polyamines of C08G18/38
-
- 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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- 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)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Sealing Material Composition (AREA)
Abstract
The application relates to the technical field of pouring sealant, and particularly discloses heat-resistant high-resilience aspartyl polyurea pouring sealant and a preparation method thereof. A heat-resistant high-resilience asparagus polyurea pouring sealant consists of a component A and a component B; the component A comprises the following raw materials: polyaspartic acid ester resin, secondary amine, filler, silane coupling agent, anti-settling agent, leveling agent and defoaming agent; the component B comprises the following raw materials: HDI polymer, prepolymer P and defoaming agent. The preparation method comprises the following steps: preparation of the component A: mixing the polyaspartic acid ester resin and the secondary amine, stirring under the protection of nitrogen, adding other components, and stirring and mixing; then vacuumizing and defoaming to obtain a component A; preparation of the component B: mixing the components, and then stirring and dispersing under a vacuum condition to obtain a component B. The preparation method of the application improves the technical problems of softening of colloid, reduction of elasticity and reduction of mechanical property when the pouring sealant is used in a high-temperature environment.
Description
Technical Field
The application relates to the technical field of pouring sealant, in particular to heat-resistant high-resilience aspartyl polyurea pouring sealant and a preparation method thereof.
Background
The pouring sealant is mainly used for bonding electronic components in electronic instruments and equipment, and is also called as electronic glue. The encapsulation is mainly to mechanically or manually fill liquid polymer into devices with electronic components and circuits, and cure the liquid polymer into a thermosetting polymer insulating material with excellent performance under normal temperature or heating condition. The function of the device is to strengthen the integrity of the electronic device and improve the resistance of the electronic device to external impact and vibration. And the insulation between internal elements and circuits of the electronic device is improved, thereby being beneficial to the miniaturization and the light weight of the electronic device. Meanwhile, internal elements and circuits of the electronic device are prevented from being directly exposed, and the waterproof and damp-proof performance of the electronic device is improved. The pouring sealant is widely used in the field of electronic and electric appliances, mainly plays a role in sealing and protecting electronic components, and is required to have good fluidity, good mechanical property, adhesive property, waterproof property, flame retardant property and electrical insulation property after being cured, and simultaneously can not corrode components of an electronic circuit board.
The types of pouring sealants are very many, and are divided into material types, and at present, most common pouring sealants mainly comprise epoxy resin pouring sealant, organic silicon resin pouring sealant and polyurethane pouring sealant, and the three pouring sealants can be divided into hundreds of different products. Generally, the organic silicon pouring sealant is an electronic pouring sealant prepared from silicon rubber, and has the advantages of low hardness, poor mechanical properties, low surface energy and poor adhesion with a base material of common organic silicon pouring sealants, and can be used for repairing encapsulated electronic devices after electronic components are poured. The epoxy pouring sealant has excellent dielectric property and higher hardness, can obtain certain toughness through modification, has good bonding property on hard base materials such as metal and the like, has good corrosion resistance and smaller curing shrinkage and linear expansion coefficient, but cannot be repaired after electronic components are poured, and has relatively higher price. The polyurethane pouring sealant has good bonding performance to rubber, metal and plastic, and the cured product has moderate strength, good elasticity and water resistance; meanwhile, the polyurethane pouring sealant overcomes the defects of brittleness of the epoxy pouring sealant and poor adhesion of the organic silicon pouring sealant, and is slightly low in cost. But the polyurethane has larger elastic internal heat generation ratio and poorer high-temperature resistance.
Although the comprehensive performance of the polyurethane elastomer is good, the service temperature of the polyurethane elastomer is not more than 80 ℃, and the short-term service temperature of the polyurethane elastomer is not more than 120 ℃, so that the application of the polyurethane elastomer is greatly limited. The polyurethane elastomer has poor heat-resistant deformation performance, the appearance size of the polyurethane elastomer is changed under the condition of high use temperature, and physical and mechanical indexes such as hardness, tensile strength, modulus and the like of the polyurethane elastomer are changed to lose application price, so that the polyurethane elastomer loses use value under the conditions of high frequency and high temperature, and the middle-high temperature encapsulation application of the polyurethane is limited.
Therefore, it is important to develop a pouring sealant that can be used under high-frequency and high-temperature conditions to solve the problem of poor high-temperature resistance of the pouring sealant.
Disclosure of Invention
In order to solve the technical problems of softening of colloid, reduction of elasticity and reduction of mechanical properties caused by the use of the pouring sealant in a high-frequency high-temperature environment, the application provides the asparagus polyurea pouring sealant which is good in processing property, high in strength, good in temperature resistance and high in resilience elasticity.
In a first aspect, the application provides a heat-resistant high-resilience aspartyl polyurea pouring sealant, which adopts the following technical scheme: a heat-resistant high-resilience asparaguese polyurea pouring sealant comprises a component A and a component B;
the component A comprises the following raw materials in parts by weight:
polyaspartic acid ester resin: 30-55 parts of
Secondary amine: 10-40 parts of
Filling: 26 to 35 portions of
Silane coupling agent: 2-5 parts of
Anti-settling agent: 1 to 3 portions of
Leveling agent: 0 to 0.8 portion
Defoaming agent: 0.2-1.2 parts;
the component B comprises the following raw materials in parts by weight:
HDI polymer: 20 to 79.8 portions of
Prepolymer P:20 to 79.8 portions of
Defoaming agent: 0.1-0.3 portion.
By adopting the technical scheme, the aliphatic isocyanate, the polyaspartic ester resin and the secondary amine are adopted, and other components are added to prepare the bicomponent aspartic polyurea pouring sealant, wherein the polyaspartic ester resin contains the aliphatic resin with the active secondary amino group, and the secondary amine has good temperature resistance; the hydrogen atom on each amino group in the secondary amine is replaced by a sec-butyl group, and the combination of the active hydrogen atom in the polyaspartic acid ester resin and the sec-butyl group in the secondary amine in a limited space generates a plurality of unique performance amino groups to form urea bonds which affect a hard segment, and the urea bonds can play a role in improving the temperature resistance, so that the heat resistance of the pouring sealant is effectively improved; the butyl in the secondary amine plays a role of an internal plasticizer, so that the prepared pouring sealant has high strength and high resilience;
the HDI polymer and the prepolymer P form a component B, wherein the prepolymer P is prepared by reacting hydroxyl-containing polymers such as polyester polyol and the like with isocyanate, so that the prepolymer P contains more polar groups such as aliphatic groups, amine aliphatic groups and the like, and the cohesive strength is high, so that the pouring sealant has higher strength and temperature resistance;
in addition, secondary amine reacts with isocyanate in the prepolymer P to generate carbamido, compared with carbamate in polyurethane filling glue, the strength of the carbamido is higher than that of the carbamate, and the breaking elongation of polyaspartic acid polyurea is high, so that the pouring sealant prepared by the application has higher strength, stronger tensile strength, good temperature resistance and high resilience elasticity, and has strong applicability and good application effect.
Preferably, the polyaspartic acid ester resin is one or a combination of N, N '- (methylenebis-4, 1-cyclohexanediyl) tetraaspartic acid tetraethyl ester, N' - (methylenebis-4, 1-cyclohexanediyl) tetraaspartic acid tetrabutyl ester, F421, F524 and F520.
By adopting the technical scheme, the polyaspartic acid adopted by the application has an active secondary amino group, and active hydrogen in the active secondary amino group can react with a secondary butyl group in secondary amine, so that the high temperature resistance and the high resilience of the pouring sealant are effectively improved.
Preferably, the polyaspartic ester resin has a viscosity of less than 1500cps; the secondary amine has a viscosity of less than 200cps.
By adopting the technical scheme, the viscosity of the polyaspartic ester resin is less than 1500cps, the polyaspartic ester resin with the viscosity is compounded with the secondary amine with the viscosity of less than 200cps, the single component has low viscosity due to low monomer viscosity, and more fillers can be added at the same mixed viscosity, so that the cost can be reduced, the performance is not influenced, and the preparation cost is effectively reduced;
after the component A and the component B are mixed, the mixture has lower mixed viscosity, so that the viscosity of the pouring sealant is lower, the fluidity is better, the dispersion of a system is facilitated, the addition amount of the filler can be better increased, the preparation cost of the pouring sealant is reduced, and the tensile strength, the elongation at break and the tearing strength of the prepared pouring sealant are better.
Preferably, the secondary amine is one or a combination of 4,4 '-methylenebis [ N-sec-butylanilino ], 4' bis-sec-butylaminodiphenylmethane, wanalink 6200, E100 and E300.
By adopting the technical scheme, secondary amine and polyaspartic ester resin are compounded for use, the secondary amine selected by the application can play a role in improving temperature resistance and high strength and still keeping elasticity and strength at high temperature, and the secondary amine adopted by the application has very high reaction activity with medium isocyanate of prepolymer P; when the WANALINK A6200 is selected, the addition amount of the secondary amine can be increased, so that the operable time is long, the addition amount of the secondary amine has influence on the operable time, and the curing speed can be adjusted by adjusting the dosage ratio of the resin, wherein the curing speed is E100> E300>6200.
Preferably, the leveling agent is one or a combination of byketol-specific and BYK-354.
By adopting the technical scheme, generally, the leveling agent is foam-stabilized most of the time, the self-defoaming performance of the pouring sealant at the later stage is influenced, the defect that the pouring sealant has bubbles is caused, and the bubble-stabilizing agent conflicts with the defoaming agent; the leveling agent adopted by the application can provide rapid leveling property and good substrate wettability, and has the characteristics of good leveling property and unstable foam.
Preferably, the filler is 1250-mesh silicon micropowder, 800-mesh silicon micropowder, 1250-mesh heavy calcium carbonate and 800-mesh heavy calcium carbonate or a combination of more than one of the two.
By adopting the technical scheme, the silicon powder and the coarse whiting can increase the amount of the pouring sealant, and tests show that the silicon powder and the coarse whiting with 1250-mesh and 800-mesh numbers have better dispersion performance, can be uniformly dispersed in a system and are not easy to settle, and are favorable for reducing the viscosity of the pouring sealant; in addition, the filler selected by the application also has the effect of improving the electrical property of the pouring sealant, and the cost for preparing the pouring sealant can be reduced.
Preferably, the defoaming agent is one or a combination of BYK535 and GA 1890.
Preferably, the silane coupling agent is one of KH550, KH560, OFS-6040 and CG-1601.
By adopting the technical scheme, the silane coupling agent can improve the compatibility of the filler and the polyaspartic ester resin, can also improve the dispersion effect of the filler in the polyaspartic ester resin, and is easy to uniformly and stably disperse the filler in a pouring sealant system; in addition, the silane coupling agent adopted by the application can also effectively improve the adhesive force of the pouring sealant, so that the pouring sealant can be more stably fixed on the surface of the base material.
Preferably, the HDI polymer is at least one of HT-100 and E402-100, and the prepolymer P is GB605A-100.
Preferably, the NCO content of the HT-100 is 23% and the NCO content of the E402-100 is 9%; the NCO content of GB605A-100 is 6 percent respectively.
By adopting the technical scheme, the HDI polymer under the NCO content can provide rigidity and temperature resistance of the pouring sealant, the strength of the pouring sealant at high temperature is guaranteed, the prepolymer P with the NCO content provides flexibility and elasticity of the pouring sealant, meanwhile, E402-100 and the prepolymer P can provide resilience performance of the pouring sealant together, the E402-100 has good elasticity but is easy to crack at high temperature, the prepolymer P has poor elasticity but cannot crack at high temperature, and the two complementary synergistic effects effectively improve the elasticity and the difficulty in cracking of the pouring sealant at high temperature.
In a second aspect, the application provides a preparation method of the heat-resistant high-resilience aspartic polyurea pouring sealant, which adopts the following technical scheme:
a preparation method of a heat-resistant high-resilience aspartyl polyurea pouring sealant comprises the following steps:
preparation of the component A: mixing polyaspartic acid ester resin and secondary amine, stirring for 8-12 minutes at a stirring speed of 200-500rpm under the protection of nitrogen, then adding a filler, a silane coupling agent, an anti-settling agent, a leveling agent, a dispersing agent and a defoaming agent, and stirring for 25-35 minutes at a stirring speed of 400-700 r/mp; then vacuumizing and defoaming for 1.5-2.5 hours to obtain a component A;
wherein, the filler is baked in advance;
preparation of the component B: mixing the HDI polymer, the prepolymer P and the defoaming agent, and then stirring and dispersing for 25-35 minutes under the vacuum condition at the stirring speed of 200-500r/mp to obtain a component B.
By adopting the technical scheme, the preparation process is simple, the production efficiency is high, and the prepared glue solution is vacuumed and vacuumed, so that bubbles in a glue solution system are well removed, the glue solution is enabled to keep a compact internal structure after being cured, and the heat resistance and the high resilience of the pouring sealant are improved.
In summary, the present application has the following beneficial effects:
1. the combination of active hydrogen atoms in the polyaspartic acid ester resin and sec-butyl groups in secondary amine generates a plurality of unique performance amino groups to form urea bonds influencing hard segments, and the urea bonds can play a role in improving the temperature resistance, so that the heat resistance of the pouring sealant is effectively improved; and the butyl in the secondary amine plays a role of an internal plasticizer, so that the prepared pouring sealant has high strength and high resilience.
2. The secondary amine that this application adopted and the isocyanate reaction in the prepolymer P generate the ureido, compare in the carbamate in the polyurethane filling glue, and ureido intensity is higher than carbamate intensity, and the fracture elongation of polyaspartic acid polyurea is high, consequently, the casting glue that this application was made has higher intensity, still has stronger tensile strength simultaneously, still has the effect that the temperature toleration is good, high resilience elasticity is good simultaneously, the suitability is strong and the application effect is good.
3. The pouring sealant has lower viscosity and better fluidity, is beneficial to the dispersion of a system, can better increase the addition amount of the filler, reduce the preparation cost of the pouring sealant, and ensure that the prepared pouring sealant has better tensile strength, elongation at break and tearing strength.
Detailed Description
The present application will be described in further detail with reference to examples. The special description is as follows: the following examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer, and the starting materials used in the following examples were obtained from ordinary commercial sources unless otherwise specified.
Examples
Example 1
Preparation of component A: adding 36 parts by weight of polyaspartic ester resin and 20 parts by weight of secondary amine into a reaction kettle, mixing for 10 minutes under the protection of nitrogen and at the stirring speed of 300rpm, then adding 35 parts of filler, 5 parts of silane coupling agent, 2 parts of anti-settling agent, 0.8 part of leveling agent and 1.2 parts of defoaming agent, stirring for 30 minutes at the stirring speed of 500r/MP, then carrying out vacuum-pumping defoaming for 2 hours at the vacuum degree of-0.1 MP, and then breaking vacuum by nitrogen to obtain a component A;
wherein, the filler is subjected to baking treatment in advance, namely the filler is baked in an oven at 120 ℃ for 5 hours;
preparation of the component B: 20 parts of HDI polymer, 79.8 parts of prepolymer P and 0.2 part of defoaming agent are added into a reaction kettle to be mixed, and then stirring and dispersing are carried out for 30 minutes under the vacuum condition at the rotating speed of 200rmp, so as to obtain a component B, wherein the component B is a curing agent.
Wherein, the polyaspartic acid ester resin is F421, the secondary amine is Wanalink 6200, the flatting agent is byketol-specific, the filler is 1250-mesh silica micropowder, the defoaming agent is 1 part of GA1890 and 0.2 part of BYK-A535, the anti-settling agent is GAs silica, the silane coupling agent is CG-1601, the HDI polymer is HT-100, the prepolymer P is GB605A-100, the viscosity of the polyaspartic ester resin is F421 and is 1000cps, and the viscosity of the secondary amine is Wanalink 6200 and is 140cps.
Example 2
Preparation of the component A: adding 47 parts by weight of polyaspartic ester resin and 10 parts by weight of secondary amine into a reaction kettle, mixing for 10 minutes under the protection of nitrogen and at the stirring speed of 300rpm, then adding 35 parts by weight of filler, 4 parts by weight of silane coupling agent, 3 parts by weight of anti-settling agent, 0.5 part by weight of leveling agent and 0.5 part by weight of defoaming agent, stirring for 30 minutes at the stirring speed of 500r/MP, then carrying out vacuum-pumping defoaming for 2 hours at the vacuum degree of 0.5MP, and then breaking the vacuum by nitrogen to obtain a component A;
wherein the filler is subjected to baking treatment in advance, namely the filler is baked in an oven at the temperature of 120 ℃ for 5 hours;
preparation of the component B: 50 parts of HDI polymer, 49.8 parts of prepolymer P and 0.2 part of defoaming agent are added into a reaction kettle to be mixed, and then stirring and dispersing are carried out for 30 minutes under the vacuum condition and at the rotating speed of 500rpm, so as to obtain a component B, wherein the component B is a curing agent.
The polyurethane comprises a base material, a filler, a silane coupling agent, a polyaspartic acid ester resin, a secondary amine, a leveling agent, a defoaming agent, a silane coupling agent and a prepolymer P, wherein the polyaspartic acid ester resin is F524, the secondary amine is E100, the leveling agent is BYK-354, the filler is 800-mesh silica micropowder, the defoaming agent is BYK-A535, the anti-settling agent is fumed silica, the silane coupling agent is CG-1601, the HDI polymer is 20 parts of HT-100 and 30 parts of E402-100, the prepolymer P is GB605A-100, the viscosity of the polyaspartic acid ester resin is 900cps, and the viscosity of the secondary amine is 152cps.
Example 3
Preparation of component A: adding 40 parts by weight of polyaspartic acid ester resin and 15 parts by weight of secondary amine into a reaction kettle, mixing, stirring for 10 minutes under the protection of nitrogen and at the stirring speed of 300rpm, then adding 30 parts of filler, 3 parts of silane coupling agent, 1 part of anti-settling agent, 0.5 part of flatting agent and 0.5 part of defoaming agent, stirring for 30 minutes at the stirring speed of 500r/MP, then carrying out vacuum-pumping defoaming for 2 hours at the vacuum degree of 1MP, and then breaking the vacuum by nitrogen to obtain a component A;
wherein, the filler is subjected to baking treatment in advance, namely the filler is baked in an oven at 120 ℃ for 5 hours;
preparation of the component B: adding 55 parts of HDI polymer, 44.8 parts of prepolymer P and 0.3 part of defoaming agent into a reaction kettle for mixing, and then stirring and dispersing for 30 minutes under vacuum condition at the rotating speed of 300rmp to obtain a component B, wherein the component B is a curing agent.
The polyurethane comprises a base material, a filler, a silane coupling agent, a polyaspartic acid ester resin, a secondary amine, a leveling agent, a defoaming agent, a silane coupling agent and a polyurethane, wherein the polyaspartic acid ester resin is F520, the secondary amine is E300, the leveling agent is BYK-354, the filler is 800-mesh silica micropowder, the defoaming agent is BYK-A535, the anti-settling agent is aerosil, the silane coupling agent is CG-1601, 15 parts of HT-100 and 40 parts of E402-100 of HDI polymer, the prepolymer P is GB605A-100, the viscosity of the polyaspartic acid ester resin is 970cps, and the viscosity of the secondary amine is 160cps.
Example 4
Preparation of component A: adding 40 parts by weight of polyaspartic acid ester resin and 30 parts by weight of secondary amine into a reaction kettle, mixing, stirring for 10 minutes under the protection of nitrogen and at the stirring speed of 300rpm, then adding 26 parts of filler, 2.5 parts of silane coupling agent, 1 part of anti-settling agent, 0.3 part of leveling agent and 0.2 part of defoaming agent, stirring for 30 minutes at the stirring speed of 500r/MP, then carrying out vacuum-pumping defoaming for 2 hours at the vacuum degree of 1MP, and then breaking the vacuum by nitrogen to obtain a component A;
wherein, the filler is subjected to baking treatment in advance, namely the filler is baked in an oven at 120 ℃ for 5 hours;
preparation of the component B: 70 parts of HDI polymer, 29.8 parts of prepolymer P and 0.2 part of defoaming agent are added into a reaction kettle to be mixed, and then stirring and dispersing are carried out for 30 minutes under the vacuum condition at the rotating speed of 300rmp, so as to obtain a component B, wherein the component B is a curing agent.
The resin composition comprises a polyaspartic acid ester resin, a filler, a defoaming agent, a leveling agent, a silane coupling agent, an HDI polymer, a prepolymer P and a polyurethane resin, wherein the polyaspartic acid ester resin is F520 and F421, the addition ratio of F421 to F520 is 1, secondary amine is WanalLINK 6200, the leveling agent is 0.1 part of byketol-special and 0.2 part of BYK-354, the filler is 1250-mesh silica micropowder, the defoaming agent is BYK-A535, the anti-settling agent is aerosil, the silane coupling agent is CG-1601, the HDI polymer is 40 parts of HT-100 and 30 parts of E402-100, the prepolymer P is GB605A-100, the viscosity of the polyaspartic acid ester resin F520 is 970cps, and the viscosity of the secondary amine E300 is 160cps.
Example 5
Preparation of component A: adding 55 parts by weight of polyaspartic ester resin and 10 parts by weight of secondary amine into a reaction kettle, mixing for 10 minutes under the protection of nitrogen and at the stirring speed of 300rpm, then adding 30.5 parts of filler, 3 parts of silane coupling agent, 1 part of anti-settling agent and 0.5 part of defoaming agent, stirring for 30 minutes at the stirring speed of 500r/MP, then carrying out vacuum-pumping defoaming for 2 hours at the vacuum degree of 1MP, and then breaking the vacuum by nitrogen to obtain a component A;
wherein, the filler is subjected to baking treatment in advance, namely the filler is baked in an oven at 120 ℃ for 5 hours;
preparation of the component B: adding 77.8 parts of HDI polymer, 20 parts of prepolymer P, 0.5 part of leveling agent and 0.2 part of defoaming agent into a reaction kettle for mixing, and then stirring and dispersing for 30 minutes under the vacuum condition and at the rotating speed of 300 people and P to obtain a component B, wherein the component B is a curing agent.
The anti-settling agent is GAs silicon, the silane coupling agent is CG-1601, the HDI polymer is 20 parts of HT-100 and 59.8 parts of E402-100, the prepolymer P is GB605A-100, the viscosity of the polyaspartic acid ester resin F520 is 970cps, and the viscosity of the secondary amine is E300 is 160cps.
Example 6
Preparation of component A: adding 30 parts of polyaspartic acid ester resin and 40 parts of secondary amine into a reaction kettle, mixing, stirring for 10 minutes at the stirring speed of 300rpm under the protection of nitrogen, then adding 26 parts of filler, 2 parts of silane coupling agent, 1 part of anti-settling agent, 0.8 part of flatting agent and 0.2 part of defoaming agent, stirring for 30 minutes at the stirring speed of 500r/MP, then vacuumizing and defoaming for 2 hours at the vacuum degree of 1MP, and then breaking the vacuum with nitrogen to obtain a component A;
wherein, the filler is subjected to baking treatment in advance, namely the filler is baked in an oven at 120 ℃ for 5 hours;
preparation of the component B: adding 65 parts of HDI polymer, 34.8 parts of prepolymer P and 0.2 part of defoaming agent into a reaction kettle for mixing, and then stirring and dispersing for 30 minutes under vacuum conditions at the rotating speed of 300rmp to obtain a component B, wherein the component B is a curing agent.
The polyurethane coating comprises a base material and a filler, wherein the base material comprises a polyaspartic acid ester resin F524, secondary amine Wanalink 6200, the filler is 800-mesh silica powder, a defoaming agent GA1890, an anti-settling agent is aerosil, a leveling agent is 0.5 part of byketol-special and 0.3 part of BYK-354, a silane coupling agent is CG-1601, an HDI polymer is 30 parts of HT-100 and 35 parts of E402-100, a prepolymer P is GB605A-100, the viscosity of the polyaspartic acid ester resin F520 is 970cps, and the viscosity of the secondary amine E300 is 160cps.
In other embodiments, the polyaspartic ester resin can also be one or a combination of several of N, N '- (methylenebis-4, 1-cyclohexanediyl) tetraaspartic acid tetraethyl ester and N, N' - (methylenebis-4, 1-cyclohexanediyl) tetraaspartic acid tetrabutyl ester; the secondary amine can also be one or a combination of more of 4,4 '-methylenebis [ N-sec-butylaniline ], 4' 4-bis-sec-butylaminodiphenylmethane; the filler is 1250-mesh heavy calcium, 800-mesh heavy calcium or the combination of a plurality of them; the silane coupling agent is one or a combination of several of KH550, KH560 and OFS-6040.
Comparative example
Comparative example 1
The difference from example 4 is that the polyaspartic acid ester resin in comparative example 1 was added in 40 parts of F421 and 20 parts of F520, and no secondary amine was added.
Comparative example 2
The difference from example 6 is that 70 parts of F524 was added to the polyaspartic acid ester resin in comparative example 2, and no secondary amine was added.
Table 1: component proportion Table of the Aspartame polyurea potting Compounds prepared in examples 1-6 and comparative examples 1-2
Performance test
The following performance tests were performed on the components A and B and the cured gel of the polyurea aspart casting compounds prepared in examples 1 to 6 and comparative examples 1 to 2, and the specific test data are shown in Table 2:
the Shore hardness test is carried out according to the ISO868:2003 standard;
the tensile strength test is carried out according to the GB/T2567-2008 standard;
detecting the elongation at break GB/T2567-2008 test;
dielectric strength was measured according to IEC60243-1
The resistivity was measured according to IEC 62631-3-1
Dielectric constant IEC 60250
Table 2: test data for the Aspartame polyurea casting sealants prepared in examples 1-6 and comparative examples 1-2
It can be seen from the combination of examples 1-6 and comparative example 1 and table 2 that the pouring sealant prepared in examples 1-6 of the present application has good performance in several aspects of tensile strength, elongation at break, hardness, etc. In addition, the structural site resistance of the secondary amine selected by the application is smaller than that of the polyaspartic acid ester resin, so that the crosslinking density of the secondary amine and the polyaspartic acid ester resin is higher, the crosslinking density is high, the heat resistance of the prepared pouring sealant can be improved, and the pouring sealant has the characteristics of better rebound resilience and difficulty in deformation when the temperature is high.
Generally, the test principle of the shore durometer is to determine the hardness of the potting adhesive by the depth of the needle penetrating into the potting adhesive, and the smaller the change of the hardness of the potting adhesive is, the larger the resilience force generated by the compression of the potting adhesive is, so as to show that the resilience performance of the potting adhesive is better. Therefore, by testing the hardness of the pouring sealant at normal temperature and high temperature and then judging the hardness change conditions of the pouring sealant in the two states, when the hardness change is large, the deformation of the pouring sealant is large, which indicates that the rebound force of the pouring sealant is poorer. As can be seen from the table, the hardness changes measured at normal temperature and high temperature of the pouring sealant prepared in the examples 1-6 are smaller, so that the pouring sealant prepared in the examples 1-6 has better rebound resilience at high temperature; the pouring sealant prepared in the comparative example 1 has large hardness change measured at normal temperature and high temperature, so the prepared pouring sealant has poor resilience. The hardness 46D of the potting adhesive in comparative example 1 is greater than the maximum hardness 94A of example 2, so that the hardness of comparative example 1 is reduced from 46D to 30A, the hardness changes greatly, and the potting adhesive prepared in comparative example 1 is severely softened at 100 ℃ and has poor resilience.
As can be seen from Table 2, the pouring sealant prepared in the comparative example 1 has smaller hardness at 100 ℃, and the pouring sealant is soft, so that the pouring sealant prepared in the comparative example becomes seriously soft at high temperature, and the use effect of the pouring sealant is seriously influenced. The pouring sealant prepared in the embodiments 1 to 6 can still maintain high hardness at high temperature, and is not easy to soften, so that the pouring sealant prepared by the application has good temperature resistance by adding secondary amine, and can still maintain high hardness at high temperature.
As can be seen from Table 2, the tensile strength and elongation at break of the potting compounds prepared in examples 1 to 6 at high temperature are also significantly higher than those of the potting compound prepared in comparative example 1. The pouring sealants prepared in examples 1 to 6 have small changes in tensile strength at 25 ℃ and 100 ℃ as compared with the pouring sealant prepared in comparative example 1 having large changes in tensile strength at 25 ℃ and 100 ℃, and thus the pouring sealant prepared in comparative example 1 has poor deformation resistance and is easily deformed by stress. In addition, the elongation at break of the pouring sealant prepared in the comparative example 1 is greatly changed at 25 ℃ and 100 ℃, which shows that the pouring sealant prepared in the comparative example 1 has higher flexibility and is easier to deform. Therefore, the secondary amine is added, so that the change of the tensile strength and the elongation at break of the pouring sealant at high temperature is small, the pouring sealant is not easy to deform at high temperature, and the pouring sealant prepared by the method has good high-temperature resistance.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. The heat-resistant high-resilience asparaguese polyurea pouring sealant is characterized by comprising a component A and a component B;
the component A comprises the following raw materials in parts by weight:
polyaspartic acid ester resin: 30-55 parts of
Secondary amine: 10-40 parts of
Filling: 26 to 35 portions of
Silane coupling agent: 2-5 parts of
Anti-settling agent: 1 to 3 portions of
Leveling agent: 0 to 0.8 portion
Defoaming agent: 0.2-1.2 parts;
the component B comprises the following raw materials in parts by weight:
HDI polymer: 20 to 79.8 portions of
Prepolymer P:20 to 79.8 portions of
Defoaming agent: 0.1-0.3 portion.
2. The heat-resistant high-resilience aspartyl polyurea pouring sealant as claimed in claim 1, wherein: the polyaspartic acid ester resin is one or a combination of more of N, N '- (methylenedi-4, 1-cyclohexanediyl) tetraaspartic acid tetraethyl ester, N' - (methylenedi-4, 1-cyclohexanediyl) tetraaspartic acid tetrabutyl ester, F421, F524 and F520.
3. The heat-resistant high-resilience aspartyl polyurea pouring sealant as claimed in claim 1, wherein: the viscosity of the polyaspartic ester resin is less than 1500cps; the secondary amine has a viscosity of less than 200cps.
4. The heat-resistant high-resilience aspartyl polyurea pouring sealant as claimed in claim 1, wherein: the secondary amine is one or a combination of more of 4,4 '-methylenebis [ N-sec-butylaniline ], 4' 4-bis-sec-butylaminodiphenylmethane, wanaLINK 6200, E100 and E300.
5. The heat-resistant high-resilience aspartyl polyurea pouring sealant as claimed in claim 1, wherein: the leveling agent is one or a combination of byketol-specific and BYK-354.
6. The heat-resistant high-resilience aspartic polyurea pouring sealant as claimed in claim 1, wherein: the filler is one or a combination of more of 1250-mesh silicon micropowder, 800-mesh silicon micropowder, 1250-mesh coarse whiting and 800-mesh coarse whiting.
7. The heat-resistant high-resilience aspartic polyurea pouring sealant as claimed in claim 1, wherein: the defoaming agent is one or a combination of more of BYK-A535 and GA 1890.
8. The heat-resistant high-resilience aspartic polyurea pouring sealant as claimed in claim 1, wherein: the silane coupling agent is one of KH550, KH560, OFS-6040 and CG-1601.
9. The heat-resistant high-resilience aspartyl polyurea pouring sealant as claimed in claim 1, wherein: the HDI polymer is at least one of HT-100 and E402-100, and the prepolymer P is GB605A-100.
10. The preparation method of the heat-resistant high-resilience aspartic polyurea pouring sealant as claimed in any one of claims 1 to 9, characterized by comprising the following steps:
preparation of component A: mixing polyaspartic acid ester resin and secondary amine, stirring for 8-12 minutes under the protection of nitrogen and at the stirring speed of 200-500rpm, then adding filler, silane coupling agent, anti-settling agent, leveling agent, dispersing agent and defoaming agent, and stirring for 25-35 minutes at the stirring speed of 400-700 r/mp; then vacuumizing and defoaming for 1.5-2.5 hours to obtain a component A;
wherein, the filler is baked in advance;
preparation of the component B: mixing the HDI polymer, the prepolymer P and the defoaming agent, and then stirring and dispersing for 25-35 minutes under the vacuum condition at the stirring speed of 200-500r/mp to obtain a component B.
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| CN103788913A (en) * | 2014-03-04 | 2014-05-14 | 大连怿文新材料科技发展有限公司 | Polyaspartic acid ester sealant for petroleum pipeline end socket and preparation method thereof |
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| CN113122175A (en) * | 2021-04-27 | 2021-07-16 | 深圳飞扬骏研新材料股份有限公司 | Preparation method of elastic polyaspartic ester pouring sealant and product thereof |
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| CN116179077A (en) * | 2022-12-12 | 2023-05-30 | 广州集泰化工股份有限公司 | Primer for addition type organosilicon pouring sealant and preparation method thereof |
| CN116376353A (en) * | 2023-05-10 | 2023-07-04 | 深圳飞扬骏研新材料股份有限公司 | Silk screen printing ink and preparation method thereof |
| CN116376353B (en) * | 2023-05-10 | 2024-04-02 | 深圳飞扬骏研新材料股份有限公司 | Silk screen printing ink and preparation method thereof |
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