CN101580686B - Epoxide resin pouring sealant with low density and high impact resistance and preparation method thereof - Google Patents
Epoxide resin pouring sealant with low density and high impact resistance and preparation method thereof Download PDFInfo
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- CN101580686B CN101580686B CN 200910059237 CN200910059237A CN101580686B CN 101580686 B CN101580686 B CN 101580686B CN 200910059237 CN200910059237 CN 200910059237 CN 200910059237 A CN200910059237 A CN 200910059237A CN 101580686 B CN101580686 B CN 101580686B
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- impact resistance
- low density
- pouring sealant
- hollow glass
- high impact
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 56
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 56
- 239000000565 sealant Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 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 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical compound O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 8
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 8
- 239000011324 bead Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 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
- 230000008569 process Effects 0.000 claims description 6
- 229940015043 glyoxal Drugs 0.000 claims description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 5
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 claims 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 claims description 4
- YSUQLAYJZDEMOT-UHFFFAOYSA-N 2-(butoxymethyl)oxirane Chemical compound CCCCOCC1CO1 YSUQLAYJZDEMOT-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
- 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
- 238000002156 mixing Methods 0.000 claims description 4
- 238000012662 bulk polymerization Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 229920000728 polyester Polymers 0.000 claims description 3
- 238000002203 pretreatment Methods 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
- 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
- 239000000463 material Substances 0.000 abstract description 12
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 239000003085 diluting agent Substances 0.000 abstract 1
- 238000005538 encapsulation Methods 0.000 abstract 1
- 239000006260 foam Substances 0.000 abstract 1
- 231100000053 low toxicity Toxicity 0.000 abstract 1
- 238000009736 wetting Methods 0.000 abstract 1
- 230000035939 shock Effects 0.000 description 15
- 239000004593 Epoxy Substances 0.000 description 10
- 239000003054 catalyst Substances 0.000 description 8
- 239000007822 coupling agent Substances 0.000 description 7
- -1 benzyl diamines Chemical class 0.000 description 6
- 239000000178 monomer Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 239000004814 polyurethane Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000009413 insulation 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
- WNLRTRBMVRJNCN-UHFFFAOYSA-L adipate(2-) Chemical compound [O-]C(=O)CCCCC([O-])=O WNLRTRBMVRJNCN-UHFFFAOYSA-L 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
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 description 2
- 238000000605 extraction Methods 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
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 125000005474 octanoate group Chemical group 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 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
- 229920000538 Poly[(phenyl isocyanate)-co-formaldehyde] Polymers 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000000853 adhesive Substances 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
- 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
- 125000005442 diisocyanate group Chemical group 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
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
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- 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
- 229920001748 polybutylene Polymers 0.000 description 1
- 229920001610 polycaprolactone Polymers 0.000 description 1
- 229920005906 polyester polyol Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000005056 polyisocyanate Substances 0.000 description 1
- 229920001228 polyisocyanate Polymers 0.000 description 1
- 229920001155 polypropylene 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
- 238000007789 sealing Methods 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
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- 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 for epoxide resin pouring sealant with low density and high impact resistance. The epoxide resin pouring sealant in the invention comprises epoxide resin,curing agent and promoter thereof, reactive diluent, polyurethane prepolymer coating hollow glass microballoon, foam killer and the like. The encapsulating material has low toxicity, fine wetting qua lity, and condensate thereof has low density, high impact resistance, low linear expansibility and good weather resistance. The pouring sealant is applicable to encapsulation of electrical apparatus elements under the condition 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; By specified requirement reasonably 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 miniaturized 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 requires to have particular performances such as lightweight, highly anti-impact simultaneously; To satisfy by the demand of embedding device low density and high impact resistance the safety assurance that provides it under severe environment, to use.The material that is used for the electronic devices and components embedding; Epoxy resin is because of having excellent dielectric insulation performance, adhesiveproperties; Good moisture resistance properties; Advantages such as and moulding process is simple, and viscosity is low, be prone to cast, solidification value is low and become present application one of joint sealant the most widely, 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 epoxy resin/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 material breaking tenacity 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 Electrical Insulation 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 number is used stealth material for the Chinese patent of CN2508957Y has prepared aircraft 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 that the present invention will solve 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 epoxy resin
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 skimmer.
Described epoxy resin 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 epoxy resin;
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 divalent alcohol through bulk polymerization, wherein the mole proportioning of vulcabond and divalent alcohol is :-NCO :-OH=1.1～5; The molecular weight of divalent alcohol is 500～3000.
B. the pre-treatment of hollow glass micropearl
Earlier with commercially available hollow glass micropearl at 100 ℃～120 ℃ dry 2h; Then hollow glass micropearl is added in the ethanolic soln of KH-550 silane coupling agent, mixes; Be heated to 40 ℃～60 ℃, through supersound process 60min, reheat to 80 ℃～120 ℃ is removed ethanol, and it is subsequent use 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 epoxy resin, reactive thinner and skimmer 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; Divalent alcohol is a kind of in polyether glycol or the polyester glycol.
The KH-550 dosage of silane coupling agent is 0.5%～3% of a cenosphere quality among the said step b.
The mass ratio of base polyurethane prepolymer for use as and pretreated hollow glass micropearl is among the said step c: 1: (1～10).
The present invention is based on the coupling agent modified hollow glass micropearl of γ-An Bingjisanyiyangjiguiwan, introduce reactive group (NH on the hollow glass micropearl surface
2), simultaneously, prepare isocyanate-terminated base polyurethane prepolymer for use as, through the covalent linkage that forms between NCO 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 NCO then can react with the secondary hydroxyl in the epoxy resin in the base polyurethane prepolymer for use as, so just can between epoxy resin and hollow glass micropearl, form the flexible polymer transition layer 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 epoxy resin through cenosphere being carried out the surface; Simultaneously, PU can form the flexible polymer layer in bead surface, and when material received 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 miniaturized, lightweight, the shock resistance condition.
Embodiment
Below in conjunction with embodiment the present invention is done further detailed description.
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 divalent alcohol through bulk polymerization, wherein the mole proportioning of vulcabond and divalent alcohol is :-NCO :-OH=1.1～5; The molecular weight of divalent alcohol is 500～3000.
B. the pre-treatment of hollow glass micropearl
Earlier with commercially available hollow glass micropearl at 100 ℃～120 ℃ dry 2h; Then hollow glass micropearl is added in the ethanolic soln of KH-550 silane coupling agent, mixes; Be heated to 40 ℃～60 ℃, through supersound process 60min, reheat to 80 ℃～120 ℃ is removed ethanol, and it is subsequent use 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 epoxy resin, reactive thinner and skimmer 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 epoxy resin
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 skimmer.
The epoxy resin that uses is low molecule liquid bisphenol A type epoxy resin, 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 epoxy resin 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, like 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 divalent alcohol and vulcabond, and its amount ratio is looked soft, the hardness of required polymkeric substance and decide, but all should guarantee-the NCO base is excessive, to generate end group be-the basic performed polymer of NCO.In the starting material-NCO base and-molar ratio of OH base is between 1.1～5.
The divalent alcohol monomer that uses can be selected polyether-type divalent alcohol monomer for use, also can select polyester type divalent 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, polybutylenes 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 POLYMETHYLENE POLYPHENYLISOCYANATE 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 is (is example with configuration 100g joint sealant) as follows:
| Form | Umber | Quality |
| E-51 epoxy resin | 100 | 51.8g |
| 593 solidifying agent | 30 | 15.5g |
| Promotor | 3 | 1.6g |
| Reactive thinner | 20 | 10.4g |
| The hollow glass micropearl that the PU performed polymer coats | 40 | 20.8g |
| Skimmer | 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 subsequent use.
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, and dry back adds 51.8g E-51 epoxy resin, 10.4g epoxy propane butyl ether reactive thinner is warming up to 60 ℃, and constant temperature stirs 2h; Be cooled to room temperature and add 15.5g 593 solidifying agent, 1.6g DMP-30 promotor and 1.5g skimmer 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 18 KJ/m
2, density is 0.8g/cm
3
Embodiment 5
The vulcabond in the present embodiment and the mol ratio of divalent 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 8 KJ/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 following:
| Form | Umber | Quality |
| E-44 epoxy resin | 100 | 63.3g |
| Reactive thinner | 15 | 9.5g |
| Solidifying agent | 20? | 12.7g |
| Curing catalyst | 2 | 1.3g |
| The hollow glass micropearl that the PU performed polymer coats | 5 | 3.2g |
| Skimmer | 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 subsequent use.
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, and dry back adds 63.3g E-44 epoxy resin, 9.5g n-butyl glycidyl ether reactive thinner is warming up to 60 ℃, and 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 skimmer 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
Skimmer 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)
1. epoxide resin pouring sealant with low density and high impact resistance, composed of the following components:
100 parts of epoxy resin
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 skimmer.
2. epoxide resin pouring sealant with low density and high impact resistance according to claim 1 is characterized in that: epoxy resin is bisphenol A type epoxy resin.
3. epoxide resin pouring sealant with low density and high impact resistance according to claim 1 is characterized in that: described solidifying agent is the general solidifying agent of epoxy resin.
4. epoxide resin pouring sealant with low density and high impact resistance according to claim 1 is characterized in that: described promotor is one or more among glyoxal ethyline, 2-methyl-4-ethyl imidazol(e), the DMP-30.
5. epoxide resin pouring sealant with low density and high impact resistance according to claim 1 is characterized in that: described reactive thinner is one or more in epoxy propane butyl ether, propylene oxide phenyl ether, n-butyl glycidyl ether, the benzyl glycidyl ether.
6. the preparation method who is used for the described epoxide resin pouring sealant with low density and high impact resistance of claim 1 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 divalent alcohol through bulk polymerization, wherein the mole proportioning of vulcabond and divalent alcohol is :-NCO :-OH=1.1～5; The molecular weight of divalent alcohol is 500～3000;
B. the pre-treatment of hollow glass micropearl
Earlier with commercially available hollow glass micropearl at 100～120 ℃ of dry 2h; Then hollow glass micropearl is added in the ethanolic soln of KH-550 silane coupling agent, mixes; Be heated to 40～60 ℃, through supersound process 60min, ethanol ℃ is removed in reheat to 80～120, and it is subsequent use 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 epoxy resin, reactive thinner and skimmer system in, stir; Add solidifying agent and promotor thereof more in proportion, mixing and stirring, vacuum defoamation, embedding, curing.
7. preparation method according to claim 6 is characterized in that: the vulcabond described in the said step a is one or more in isophorone diisocyanate, hexamethylene diisocyanate, the tolylene diisocyanate; Divalent alcohol is a kind of in polyether glycol or the polyester glycol.
8. preparation method according to claim 6 is characterized in that: the KH-550 dosage of silane coupling agent is 0.5%～3% of a cenosphere quality among the said step b.
9. preparation method according to claim 6 is characterized in that: the mass ratio of base polyurethane prepolymer for use as and pretreated hollow glass micropearl is among the said step c: 1: (1～10).
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