CN101580686A - A kind of low-density high-impact-resistant epoxy resin potting glue and preparation method thereof - Google Patents
A kind of low-density high-impact-resistant epoxy resin potting glue and preparation method thereof Download PDFInfo
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- CN101580686A CN101580686A CNA2009100592376A CN200910059237A CN101580686A CN 101580686 A CN101580686 A CN 101580686A CN A2009100592376 A CNA2009100592376 A CN A2009100592376A CN 200910059237 A CN200910059237 A CN 200910059237A CN 101580686 A CN101580686 A CN 101580686A
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- epoxy resin
- hollow glass
- polyurethane prepolymer
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 35
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 238000004382 potting Methods 0.000 title claims 8
- 239000003292 glue Substances 0.000 title 1
- 239000011521 glass Substances 0.000 claims abstract description 43
- 229920001730 Moisture cure polyurethane Polymers 0.000 claims abstract description 36
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 239000004005 microsphere Substances 0.000 claims abstract 10
- 239000003085 diluting agent Substances 0.000 claims abstract 4
- 239000004593 Epoxy Substances 0.000 claims description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 12
- 239000013530 defoamer Substances 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical group CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 8
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 8
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 6
- 150000002009 diols Chemical class 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 claims description 4
- QNYBOILAKBSWFG-UHFFFAOYSA-N 2-(phenylmethoxymethyl)oxirane Chemical compound C1OC1COCC1=CC=CC=C1 QNYBOILAKBSWFG-UHFFFAOYSA-N 0.000 claims description 4
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 4
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 4
- 125000005442 diisocyanate group Chemical group 0.000 claims description 4
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 claims description 4
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000012662 bulk polymerization Methods 0.000 claims description 3
- 229920000728 polyester Polymers 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 3
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 2
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 2
- 229920000570 polyether Polymers 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 229920000909 polytetrahydrofuran Polymers 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 6
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical group CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims 1
- RIAHASMJDOMQER-UHFFFAOYSA-N 5-ethyl-2-methyl-1h-imidazole Chemical compound CCC1=CN=C(C)N1 RIAHASMJDOMQER-UHFFFAOYSA-N 0.000 claims 1
- 239000008393 encapsulating agent Substances 0.000 claims 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims 1
- 239000000565 sealant Substances 0.000 abstract description 29
- 239000000463 material Substances 0.000 abstract description 13
- 238000007789 sealing Methods 0.000 abstract description 3
- 239000002518 antifoaming agent Substances 0.000 abstract 1
- 231100000053 low toxicity Toxicity 0.000 abstract 1
- 229920005989 resin Polymers 0.000 description 20
- 239000011347 resin Substances 0.000 description 20
- 230000035939 shock Effects 0.000 description 15
- 239000003054 catalyst Substances 0.000 description 8
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical compound O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 7
- 239000007822 coupling agent Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- -1 polyoxyethylene Polymers 0.000 description 6
- 239000011324 bead Substances 0.000 description 5
- 239000000178 monomer Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229940015043 glyoxal Drugs 0.000 description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 239000004814 polyurethane Substances 0.000 description 4
- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 description 3
- YSUQLAYJZDEMOT-UHFFFAOYSA-N 2-(butoxymethyl)oxirane Chemical compound CCCCOCC1CO1 YSUQLAYJZDEMOT-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- ULKLGIFJWFIQFF-UHFFFAOYSA-N 5K8XI641G3 Chemical compound CCC1=NC=C(C)N1 ULKLGIFJWFIQFF-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 229920005570 flexible polymer Polymers 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 2
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 125000005474 octanoate group Chemical group 0.000 description 2
- 239000005056 polyisocyanate Substances 0.000 description 2
- 229920001228 polyisocyanate Polymers 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 239000003566 sealing material Substances 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- LUYHWJKHJNFYGV-UHFFFAOYSA-N 1,2-diisocyanato-3-phenylbenzene Chemical compound O=C=NC1=CC=CC(C=2C=CC=CC=2)=C1N=C=O LUYHWJKHJNFYGV-UHFFFAOYSA-N 0.000 description 1
- MTZUIIAIAKMWLI-UHFFFAOYSA-N 1,2-diisocyanatobenzene Chemical compound O=C=NC1=CC=CC=C1N=C=O MTZUIIAIAKMWLI-UHFFFAOYSA-N 0.000 description 1
- ZXHZWRZAWJVPIC-UHFFFAOYSA-N 1,2-diisocyanatonaphthalene Chemical compound C1=CC=CC2=C(N=C=O)C(N=C=O)=CC=C21 ZXHZWRZAWJVPIC-UHFFFAOYSA-N 0.000 description 1
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- WNLRTRBMVRJNCN-UHFFFAOYSA-L adipate(2-) Chemical compound [O-]C(=O)CCCCC([O-])=O WNLRTRBMVRJNCN-UHFFFAOYSA-L 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- NIHJEJFQQFQLTK-UHFFFAOYSA-N butanedioic acid;hexanedioic acid Chemical compound OC(=O)CCC(O)=O.OC(=O)CCCCC(O)=O NIHJEJFQQFQLTK-UHFFFAOYSA-N 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229920001083 polybutene Polymers 0.000 description 1
- 229920001610 polycaprolactone Polymers 0.000 description 1
- 229920005906 polyester polyol Polymers 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Sealing Material Composition (AREA)
Abstract
The invention relates to a preparation method of a low-density high-impact-resistance epoxy resin pouring sealant. The epoxy resin pouring sealant disclosed by the invention is composed of epoxy resin, a curing agent and an accelerator thereof, an active diluent, polyurethane prepolymer coated hollow glass microspheres, a defoaming agent and the like. The encapsulating material has low toxicity and good wettability, and a condensate of the encapsulating material has low density, high impact resistance, low linear expansion coefficient and good weather resistance; the filling and sealing device is suitable for filling and sealing electric appliance elements under the conditions of miniaturization, light weight and impact resistance.
Description
Technical field
The invention belongs to the adhesive technology field, be specifically related to a kind of epoxide resin pouring sealant with low density and high impact resistance and preparation method thereof.
Background technology
Embedding briefly is exactly by Embedding Material the each several part element that constitutes electron device; require in accordance with regulations reasonably to arrange, assemble, connect, sealing and protection etc. and a kind of operating procedure of implementing; to prevent the intrusion of water branch, dust and obnoxious flavour to electronic devices and components; slow down vibration, prevent external force damage and stablize the parameter of electronic devices and components.At present, expansion along with range of application, integrated, the miniaturization of electronic unit and the raising of measure of precision, electronic applications not only is confined to the dielectric insulation performance to the demand of Embedding Material, also require to have particular performances such as lightweight, high impact-resistant simultaneously, so that the safety assurance that provides it to use under severe environment to be provided by the demand of embedding device low density and high impact resistance.The material that is used for the electronic devices and components embedding, Resins, epoxy is because of having excellent dielectric insulation performance, adhesiveproperties, good moisture resistance properties, and moulding process is simple, advantages such as low, the easy cast of viscosity, solidification value are low and become one of joint sealant that is most widely used at present, but it solidifies back fragility shortcoming big, the shock resistance difference and has then limited its use under severe environment.Therefore, the epoxy fill-sealing materials of exploitation low density and high impact resistance has intensive demand and application prospect.
In recent years, researcher has been carried out number of research projects to the modification aspect of epoxy pouring sealant both at home and abroad.Chinese science and technology periodical " material engineering " has been reported Hahn China of Northwestern Polytechnical University etc., and (material engineering 2005 8:32-38) adopts situ aggregation method to prepare Resins, epoxy/nanometer SiO2 Embedding Material, gives its certain toughness; " bonding " magazine has then been reported in the epoxy molecular chain and have been embedded the liquid crystal group, can reduce the viscosity of system greatly, improve the breaking tenacity of material and toughness of material (Zhong Wenbin etc., bonding 2000, (1): 17).The people such as Yshigeta of Japan think, the internal stress of system is not only shunk relevant with the vitreous state of curing system, and also relevant (Report in conference on ElectricalInsulation and Dilectric Phenomena with the elastic modulus change of system, 1996,82-86).On the other hand, hollow glass micropearl is a kind of novel non-metallic material, has lightweight, wear-resisting, high-intensity characteristics.Granted publication is number for the Chinese patent of CN2508957Y has prepared the aircraft stealth material with regard to the hollow glass micropearl that adopts metal plating layer, and the use of this coating can alleviate aircraft weight effectively.In a word, epoxy resin modification research also concentrates on simple Research on Toughening, and Shang Weijian promptly can reduce the research report that epoxy density can improve its shock strength again.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of epoxide resin pouring sealant with low density and high impact resistance, and a kind of preparation method of epoxide resin pouring sealant with low density and high impact resistance is provided simultaneously.
Epoxide resin pouring sealant with low density and high impact resistance of the present invention, composed of the following components:
100 parts of Resins, epoxy
10～30 parts in solidifying agent
0.1～3 part of promotor
5～20 parts of reactive thinners
1～40 part of the hollow glass micropearl that base polyurethane prepolymer for use as coats
0.5～3 part of defoamer
Described Resins, epoxy is bisphenol A type epoxy resin E-51, E-44 or the mixture of the two;
Described solidifying agent is the general solidifying agent of Resins, epoxy, preferred 593 solidifying agent;
Described promotor is one or more among glyoxal ethyline, 2-methyl-4-ethyl imidazol(e), the DMP-30.
Described reactive thinner is one or more in epoxy propane butyl ether, propylene oxide phenyl ether, n-butyl glycidyl ether, benzyl glycidyl ether, the fatty glycidyl ether;
The preparation method of described epoxide resin pouring sealant with low density and high impact resistance is characterized in that may further comprise the steps:
A. the preparation of base polyurethane prepolymer for use as
At 80 ℃～100 ℃, make base polyurethane prepolymer for use as by vulcabond and dibasic alcohol by bulk polymerization, wherein the mole proportioning of vulcabond and dibasic alcohol is :-NCO :-OH=1.1～5;
B. the pre-treatment of hollow glass micropearl
Earlier with commercially available hollow glass micropearl at 100 ℃～120 ℃ dry 2h; Hollow glass micropearl is added in the ethanolic soln of KH-550 silane coupling agent then, mixes; Be heated to 40 ℃～60 ℃, through supersound process 60min, reheat to 80 ℃～120 ℃ is removed ethanol, and it is standby to be cooled to room temperature;
C. the preparation of base polyurethane prepolymer for use as coated hollow glass bead
The base polyurethane prepolymer for use as that step a is made joins dissolving fully in the acetone solvent; And then hollow glass micropearl pretreated among the step b is added in the base polyurethane prepolymer for use as solution, heat temperature raising to 40 ℃ stirs 1h, drying for standby;
D. the preparation of epoxide resin pouring sealant with low density and high impact resistance
With the base polyurethane prepolymer for use as coated hollow glass bead for preparing among the step c add configuration in proportion Resins, epoxy, reactive thinner and defoamer system in, stir; Add solidifying agent and promotor thereof more in proportion, mixing and stirring, vacuum defoamation, embedding, curing.
Vulcabond described in the step a is one or more in isophorone diisocyanate, hexamethylene diisocyanate, the tolylene diisocyanate; Dibasic alcohol is one or more in polyoxyethylene glycol, polytetrahydrofuran diol, polyether glycol or the polyester glycol.
The KH-550 dosage of silane coupling agent is 0.5%～3% of a cenosphere quality among the described step b.
The mass ratio of base polyurethane prepolymer for use as and pretreated hollow glass micropearl is among the described step c: 1: (1～10).
The present invention is based on the coupling agent modified hollow glass micropearl of γ-An Bingjisanyiyangjiguiwan, introduce active group (NH on the hollow glass micropearl surface
2), simultaneously, prepare isocyanate-terminated base polyurethane prepolymer for use as, by the covalent linkage that forms between isocyanate group in the base polyurethane prepolymer for use as and the amino on the hollow glass micropearl it is coated on the hollow glass micropearl surface; Thereby obtain the hollow glass micropearl that base polyurethane prepolymer for use as coats; Be introduced in the epoxy systems, remaining isocyanate group then can be reacted with the secondary hydroxyl in the Resins, epoxy in the base polyurethane prepolymer for use as, so just can form the flexible polymer transition layer between Resins, epoxy and hollow glass micropearl again.
The present invention adopts hollow glass micropearl as filler, can reduce the density of epoxy pouring sealant greatly; Further, coat base polyurethane prepolymer for use as, not only can improve the consistency of glass microballon and Resins, epoxy by cenosphere being carried out the surface; Simultaneously, PU can form the flexible polymer layer in bead surface, and when material was subjected to external impacts, it can play and stop the crazing further growth, endergonic effect, thus improved the shock resistance of material greatly.Adopt the epoxy pouring sealant of the present invention's preparation, not only have the dielectric insulation performance of good shock resistance, excellence, and have characteristics such as low density, light weight.The present invention is applicable to the embedding of the electric elements under miniaturization, lightweight, the shock resistance condition.
Embodiment
The present invention is described in further detail below in conjunction with embodiment.
Epoxide resin pouring sealant with low density and high impact resistance preparation method of the present invention comprises the steps:
A. the preparation of base polyurethane prepolymer for use as
At 80 ℃～100 ℃, make base polyurethane prepolymer for use as by vulcabond and dibasic alcohol by bulk polymerization, wherein the mole proportioning of vulcabond and dibasic alcohol is :-NCO :-OH=1.1～5;
B. the pre-treatment of hollow glass micropearl
Earlier with commercially available hollow glass micropearl at 100 ℃～120 ℃ dry 2h; Hollow glass micropearl is added in the ethanolic soln of KH-550 silane coupling agent then, mixes; Be heated to 40 ℃～60 ℃, through supersound process 60min, reheat to 80 ℃～120 ℃ is removed ethanol, and it is standby to be cooled to room temperature;
C. the preparation of base polyurethane prepolymer for use as coated hollow glass bead
The base polyurethane prepolymer for use as that step a is made joins dissolving fully in the acetone solvent; And then hollow glass micropearl pretreated among the step b is added in the base polyurethane prepolymer for use as solution, heat temperature raising to 40 ℃ stirs 1h, drying for standby;
D. the preparation of epoxide resin pouring sealant with low density and high impact resistance
With the base polyurethane prepolymer for use as coated hollow glass bead for preparing among the step c add configuration in proportion Resins, epoxy, reactive thinner and defoamer system in, stir; Add solidifying agent and promotor thereof more in proportion, mixing and stirring, vacuum defoamation, embedding, curing.
A kind of epoxide resin pouring sealant with low density and high impact resistance that the present invention relates to, composed of the following components:
100 parts of Resins, epoxy
10～30 parts in solidifying agent
0.1～3 part of promotor
5～20 parts of reactive thinners
1～40 part of the hollow glass micropearl that the PU performed polymer coats
0.5～3 part of defoamer
The Resins, epoxy that uses is low molecule liquid bisphenol A type Resins, epoxy, and this resin viscosity is less, oxirane value is high, commonly used E-44, E-51 etc. are arranged; Usually select for use a kind of Resins, epoxy to use separately, also can select for use two kinds of mixed with resin to use.
The solidifying agent that uses is amine curing agent, preferred 593 amine curing agents.
The curing catalyst that uses is tertiary amines such as benzyl diamines, DMP-30.Also can use the metal-salt of glyoxaline compound and carboxylic acid, as 2-ethyl-4-methylimidazole, glyoxal ethyline etc.Usually select for use a kind of curing catalyst to use separately, also can select for use the mixing of two or more promotor to use.
The reactive thinner that uses is: epoxy propane butyl ether, propylene oxide phenyl ether, n-butyl glycidyl ether, benzyl glycidyl ether, fatty glycidyl ether or their mixture
The hollow glass micropearl that uses is generally pure white, and particle diameter is 10 μ m～50 μ m, and ultimate compression strength is 37.9MPa, the about 0.38g/m of tap density
3
The preferred γ-An Bingjisanyiyangjiguiwan coupling agent of the silane coupling agent of hollow glass micropearl modification
The main raw material of preparation base polyurethane prepolymer for use as is dibasic alcohol and vulcabond, and its amount ratio decide on soft, the hardness of required polymkeric substance, but all should guarantee-the NCO base is excessive, with the generation end group is-performed polymer of NCO base.In the starting material-NCO base and-molar ratio of OH base is between 1.1～5.
The dibasic alcohol monomer that uses can be selected polyether-type dibasic alcohol monomer for use, also can select polyester type dibasic alcohol monomer for use, and its molecular weight can be selected between 500～3000 according to the demand of product performance.The polyester polyol that uses can be polyethylene glycol adipate, polypropylene adipate (PPA), poly adipate succinic acid ester, poly-epsilon-caprolactone, polybutene diacid glycol ester etc.Usually selecting for use two or more to mix uses.
The polyisocyanates monomer that diisocyanate monomer uses is selected inexpensive aromatic diisocyanate usually for use, as: tolylene diisocyanate, diphenylmethanediisocyanate, phenylene diisocyanate, biphenyl diisocyanate, naphthalene diisocyanate etc.Usually select for use a kind of vulcabond to use separately, also can select for use two or more polyisocyanates to mix and use.
Elaborate below in conjunction with some embodiment.Subject area involved in the present invention is not limited only in following examples.
Embodiment 1
The preparation of epoxide resin pouring sealant with low density and high impact resistance.
Proportioning following (is example with configuration 100g joint sealant):
Form the umber quality
E-51 Resins, epoxy 100 51.8g
593 solidifying agent, 30 15.5g
Promotor 3 1.6g
Reactive thinner 20 10.4g
Hollow glass micropearl 40 20.8g that the PU performed polymer coats
Defoamer 3 1.5g
Preparation process: join in the there-necked flask after getting 37.5g PTMG-1000 vacuum hydro-extraction, heat temperature raising to 90 ℃～95 ℃ of fusings fully, add 3 in 12.5g isophorone diisocyanate, the inferior tin of octoate catalyst again, logical nitrogen 10 minutes, thermostatically heating continues reaction 3 hours, system temperature is reduced to room temperature promptly get base polyurethane prepolymer for use as;
Elder generation 120 ℃ of oven dry, adds the 19g hollow glass micropearl in the ethanolic soln of KH-550 silane coupling agent with it then, and the consumption of coupling agent is 1% of a cenosphere quality; Behind 60 ℃ of supersound process 60min, again the oven dry, be cooled to room temperature sieve the bottling standby.
Get top synthetic base polyurethane prepolymer for use as 2g and join in an amount of acetone, be stirred to base polyurethane prepolymer for use as and dissolve fully; And then the coupling agent modified hollow glass micropearl of adding 19g, 40 ℃ are stirred 1h, dry back adds 51.8g E-51 Resins, epoxy, 10.4g epoxy propane butyl ether reactive thinner is warming up to 60 ℃, constant temperature stirs 2h, be cooled to room temperature and add 15.5g 593 solidifying agent, 1.6g DMP-30 promotor and 1.5g defoamer again, vacuum defoamation, embedding, self-vulcanizing 24h.Obtaining resistance to impact shock is 12KJ/m
2, density is 0.8g/cm
3, cure shrinkage is 0.4%, viscosity is the epoxy fill-sealing materials of 2000mPaS.
Embodiment 2
Change the PTMG-1000 among the embodiment 1 into PTMG-2000, other condition is constant, can obtain epoxide resin pouring sealant with low density and high impact resistance, and its impact resistance is 15KJ/m
2
Embodiment 3
Coupling agent modified hollow glass micropearl in the present embodiment is 10g, and other condition is identical with embodiment 1, can obtain epoxide resin pouring sealant with low density and high impact resistance, and its viscosity is 1500mPaS, and density is 1.0g/cm
3, cure shrinkage is 0.613%.
Embodiment 4
Base polyurethane prepolymer for use as in the present embodiment is 5g, and other condition is identical with embodiment 1, can obtain epoxide resin pouring sealant with low density and high impact resistance, and its resistance to impact shock is 18KJ/m
2, density is 0.8g/cm
3
Embodiment 5
The vulcabond in the present embodiment and the mol ratio of dibasic alcohol are 3, and other condition is identical with embodiment 1, can obtain epoxide resin pouring sealant with low density and high impact resistance, and its resistance to impact shock is 8KJ/m
2, density is 0.8g/cm
3
Embodiment 6
Reactive thinner in the present embodiment is 5g, and other condition is identical with embodiment 1, obtains epoxide resin pouring sealant with low density and high impact resistance, and it is 3200mPaS that its viscosity increases, and be 30h set time, and resistance to impact shock is 12KJ/m
2, density is 0.8g/cm
3
Embodiment 7
Proportioning is as follows:
Form the umber quality
E-44 Resins, epoxy 100 63.3g
Reactive thinner 15 9.5g
Solidifying agent 20 12.7g
Curing catalyst 2 1.3g
Hollow glass micropearl 5 3.2g that the PU performed polymer coats
Defoamer 1 0.6g
Preparation process: join in the there-necked flask after getting 37.5g PTMG-1000 vacuum hydro-extraction, heat temperature raising to 90 ℃～95 ℃ of fusings fully, add 3 in 12.5g isophorone diisocyanate, the inferior tin of octoate catalyst again, logical nitrogen 10 minutes, thermostatically heating continues reaction 3 hours, system temperature is reduced to room temperature promptly get base polyurethane prepolymer for use as;
Elder generation 120 ℃ of oven dry, adds the 2.9g hollow glass micropearl in the ethanolic soln of KH-550 silane coupling agent with it then, and the consumption of coupling agent is 1% of a cenosphere quality; Behind 60 ℃ of supersound process 60min, again the oven dry, be cooled to room temperature sieve the bottling standby.
Get top synthetic base polyurethane prepolymer for use as 0.3g and join in an amount of acetone, be stirred to base polyurethane prepolymer for use as and dissolve fully; And then the coupling agent modified hollow glass micropearl of adding 2.9g, 40 ℃ are stirred 1h, dry back adds 63.3g E-44 Resins, epoxy, 9.5g n-butyl glycidyl ether reactive thinner is warming up to 60 ℃, constant temperature stirs 2h, be cooled to room temperature and add 12.7g 593 solidifying agent, 1.3g benzyl diamines curing catalyst and 0.6g defoamer again, vacuum defoamation 10min, embedding, self-vulcanizing 24h.Obtaining resistance to impact shock is 12KJ/m
2, density is 1.0g/cm
3, cure shrinkage is 0.8%, viscosity is the epoxy pouring sealant of 1800mPaS.
Embodiment 8
593 solidifying agent in the present embodiment are 5g, and other condition is identical with embodiment 7, obtains the low density and high impact resistance epoxy pouring sealant, and be 32h its set time, and resistance to impact shock is 12KJ/m
2, density is 1.0g/cm
3
Embodiment 9
Defoamer in the present embodiment is 0.3g, and other condition is identical with embodiment 7, and the system bubble increases, and froth in vacuum 30min obtains epoxide resin pouring sealant with low density and high impact resistance, and its resistance to impact shock is 12KJ/m
2, density is 1.0g/cm
3
Embodiment 10:
Curing catalyst in the present embodiment is a glyoxal ethyline, and other condition is identical with embodiment 7, obtains epoxide resin pouring sealant with low density and high impact resistance, and its resistance to impact shock is 12KJ/m
2, density is 1.0g/cm
3
Embodiment 11:
Curing catalyst in the present embodiment is the equal proportion mixture of 2-ethyl-4-methylimidazole and glyoxal ethyline, and other condition is identical with embodiment 7, obtains epoxide resin pouring sealant with low density and high impact resistance, and its resistance to impact shock is 12KJ/m
2, density is 1.0g/cm
3
Embodiment 12:
Reactive thinner in the present embodiment is the equal proportion mixture of propylene oxide phenyl ether and benzyl glycidyl ether, and other condition is identical with embodiment 7, obtains epoxide resin pouring sealant with low density and high impact resistance, and its resistance to impact shock is 12KJ/m
2, density is 1.0g/cm
3
Claims (9)
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