CN115584232A - 一种高伸长率,自粘型聚氨酯封装材料及其制备方法 - Google Patents
一种高伸长率,自粘型聚氨酯封装材料及其制备方法 Download PDFInfo
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- CN115584232A CN115584232A CN202210146570.6A CN202210146570A CN115584232A CN 115584232 A CN115584232 A CN 115584232A CN 202210146570 A CN202210146570 A CN 202210146570A CN 115584232 A CN115584232 A CN 115584232A
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- 229920002635 polyurethane Polymers 0.000 title claims abstract description 44
- 239000004814 polyurethane Substances 0.000 title claims abstract description 44
- 239000000853 adhesive Substances 0.000 title claims abstract description 28
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- 238000002360 preparation method Methods 0.000 title abstract description 23
- 229920005862 polyol Polymers 0.000 claims abstract description 53
- 150000003077 polyols Chemical class 0.000 claims abstract description 53
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 40
- 229920000570 polyether Polymers 0.000 claims abstract description 40
- 229920005989 resin Polymers 0.000 claims abstract description 22
- 239000011347 resin Substances 0.000 claims abstract description 22
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 17
- 150000002009 diols Chemical class 0.000 claims abstract description 13
- 239000000945 filler Substances 0.000 claims abstract description 13
- 239000004417 polycarbonate Substances 0.000 claims abstract description 13
- 229920000515 polycarbonate Polymers 0.000 claims abstract description 13
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 11
- 239000011574 phosphorus Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 4
- -1 diethyl ethylphosphate Chemical compound 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 10
- 229920000909 polytetrahydrofuran Polymers 0.000 claims description 9
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims description 8
- 229910052783 alkali metal Inorganic materials 0.000 claims description 7
- 229910000323 aluminium silicate Inorganic materials 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 7
- 150000002148 esters Chemical class 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
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- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 4
- 229920001451 polypropylene glycol Polymers 0.000 claims description 4
- HQUQLFOMPYWACS-UHFFFAOYSA-N tris(2-chloroethyl) phosphate Chemical compound ClCCOP(=O)(OCCCl)OCCCl HQUQLFOMPYWACS-UHFFFAOYSA-N 0.000 claims description 4
- 150000001340 alkali metals Chemical class 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 3
- VONWDASPFIQPDY-UHFFFAOYSA-N dimethyl methylphosphonate Chemical compound COP(C)(=O)OC VONWDASPFIQPDY-UHFFFAOYSA-N 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 230000003014 reinforcing effect Effects 0.000 claims description 3
- 239000005995 Aluminium silicate Substances 0.000 claims description 2
- 239000004114 Ammonium polyphosphate Substances 0.000 claims description 2
- 239000004593 Epoxy Substances 0.000 claims description 2
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 2
- 239000013032 Hydrocarbon resin Substances 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- 235000004443 Ricinus communis Nutrition 0.000 claims description 2
- 235000012211 aluminium silicate Nutrition 0.000 claims description 2
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims description 2
- 229920001276 ammonium polyphosphate Polymers 0.000 claims description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- 239000001177 diphosphate Substances 0.000 claims description 2
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 claims description 2
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- 229920001519 homopolymer Polymers 0.000 claims description 2
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- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 2
- 229920006216 polyvinyl aromatic Polymers 0.000 claims description 2
- 239000004526 silane-modified polyether Substances 0.000 claims description 2
- 239000000454 talc Substances 0.000 claims description 2
- 229910052623 talc Inorganic materials 0.000 claims description 2
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims description 2
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims description 2
- GTRSAMFYSUBAGN-UHFFFAOYSA-N tris(2-chloropropyl) phosphate Chemical compound CC(Cl)COP(=O)(OCC(C)Cl)OCC(C)Cl GTRSAMFYSUBAGN-UHFFFAOYSA-N 0.000 claims description 2
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims 1
- CJWBPEYRTPGWPF-UHFFFAOYSA-N 2-[bis(2-chloroethoxy)phosphoryloxy]ethyl bis(2-chloroethyl) phosphate Chemical compound ClCCOP(=O)(OCCCl)OCCOP(=O)(OCCCl)OCCCl CJWBPEYRTPGWPF-UHFFFAOYSA-N 0.000 claims 1
- 125000001340 2-chloroethyl group Chemical group [H]C([H])(Cl)C([H])([H])* 0.000 claims 1
- 238000005538 encapsulation Methods 0.000 claims 1
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 claims 1
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 4
- 239000000565 sealant Substances 0.000 description 4
- 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 3
- 229920000805 Polyaspartic acid Polymers 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 239000003063 flame retardant Substances 0.000 description 3
- 108010064470 polyaspartate Proteins 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 235000012255 calcium oxide Nutrition 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 230000009477 glass transition Effects 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 239000012948 isocyanate Substances 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- FIOLEJHZNAMKAN-UHFFFAOYSA-N 1-[bis(2-chloroethoxy)phosphoryloxy]ethyl bis(2-chloroethyl) phosphate Chemical compound P(=O)(OCCCl)(OCCCl)OC(C)OP(=O)(OCCCl)OCCCl FIOLEJHZNAMKAN-UHFFFAOYSA-N 0.000 description 1
- VCUFZILGIRCDQQ-KRWDZBQOSA-N N-[[(5S)-2-oxo-3-(2-oxo-3H-1,3-benzoxazol-6-yl)-1,3-oxazolidin-5-yl]methyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C1O[C@H](CN1C1=CC2=C(NC(O2)=O)C=C1)CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F VCUFZILGIRCDQQ-KRWDZBQOSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000004359 castor oil Substances 0.000 description 1
- 235000019438 castor oil Nutrition 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
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- 230000026058 directional locomotion Effects 0.000 description 1
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- 230000005684 electric field Effects 0.000 description 1
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- 239000004611 light stabiliser Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229920005906 polyester polyol Polymers 0.000 description 1
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- 239000000377 silicon dioxide Substances 0.000 description 1
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- 239000013008 thixotropic agent Substances 0.000 description 1
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 description 1
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- 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
- C09J175/04—Polyurethanes
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- 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
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- 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
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- 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
- C08G18/44—Polycarbonates
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- 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
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
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- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
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- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
- C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
- C08G18/7671—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl group
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- 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
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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Abstract
本发明公开了一种高伸长率,自粘型聚氨酯封装材料,制备原料包括:改性聚醚多元醇、自制预聚体、有机磷、聚醚多元醇、填料、助剂、增强树脂、固化剂,通过利用聚碳酸酯二醇和MDI‑50合成自制预聚体,与改性聚醚多元醇、有机磷、聚醚多元醇、填料、助剂、增强树脂、固化剂分批次加入充分混合制备聚氨酯封装材料。所得密封材料具有长久自粘性、高伸长率、高拉伸强度、高绝缘性。此外,该聚氨酯密封材料还具有耐水、防霉、防震、导热、耐高温阻燃等特性,可广泛用于电子元器件密封胶领域,很好地保护电子元器件。而且本申请为单组分聚氨酯密封材料,制备工艺简单,条件可控易实现,而且可以直接使用。
Description
技术领域
本发明涉及的是封装材料是制备领域,C08G18/48,尤其涉及一种高伸长率,自粘型聚氨酯封装材料及其制备方法。
背景技术
电子元器件的封装主要用于防止外部恶劣环境对电子元器件性能造成的损伤,提高对湿气、灰尘、外部冲击、振动的抵抗力,同时防止电子元器件由于故障引发的安全性问题,改善内部元件与线路间的绝缘性、传热导热,所以需要封装材料具有优异的耐水耐潮性、绝缘性、导热性、以及强拉伸强度和抗震性。现阶段,用作电子密封材料的高分子聚合物主要有环氧树脂、有机硅、聚氨酯三大类,但是环氧树脂类具有很高的脆性,有机硅类的拉伸强度低,且粘性较差,进而导致密封性下降,而聚氨酯类密封材料可以很好地克服了这些问题,是理想的电子元器件的密封材料。
专利CN201810659754.6提供了一种多组份聚氨酯灌封胶及其制备方法,分为A、B组分,其中A组分包括蓖麻油多元醇、聚酯多元醇、聚醚多元醇、填料、阻燃剂、催化剂,B组分包括固化剂和稀释剂,所得多组分聚氨酯灌封胶具有耐电痕、无卤阻燃和粘结强度高的特点,但其伸长率、硬度、拉伸强度有待改善。专利CN202011624815.9公开了一种单组分聚氨酯电子元器件固定胶及其制备方法和应用,在含有异氰酸酯基的预聚体中加入硅烷偶联剂、阻燃粉料、阻燃触变剂、抗氧化剂、光稳定剂、潜固化剂,所得固定胶交联度高,保证制备的电子固定胶具有一定的高强度并附有一定弹性,且有良好的附着力、耐湿热老化性能,但其断裂伸长率、拉伸强度均较弱。
发明内容
本发明通过提供一种高伸长率,自粘型聚氨酯封装材料及其制备方法,解决了现有技术中独权能解决的技术问题,实现了技术效果。
本发明第一方面提供了一种高伸长率,自粘型聚氨酯封装材料,按重量百分比计,制备原料包括:
改性聚醚多元醇50~60%、自制预聚体10~20%;有机磷2~4%、聚醚多元醇10~20%、填料3~6%、助剂0.2~0.5%、增强树脂1~10%、固化剂1~20%;
作为一种优选的实施方案,所述改性聚醚多元醇选自硅烷改性聚醚多元醇、环氧树脂改性聚醚多元醇、氧化乙烯均聚物、聚氧化乙烯多元醇、氧化丙烯均聚物、聚氧化丙烯多元醇、聚四氢呋喃多元醇、蓖麻油改性聚醚多元醇中的一种或多种;优选地,所述改性聚醚多元醇为聚四氢呋喃多元醇;进一步优选地,所述聚四氢呋喃多元醇为聚四氢呋喃醚二醇;
作为一种优选的实施方案,所述自制预聚体的制备方法为:
在容器中加入脱水处理的聚碳酸酯二醇,打开搅拌,温度升到60℃时,开始缓慢滴加计量的MDI-50,维持反应温度在70~80℃,控制滴加在1小时完成,继续在此温度下反应2小时,出料。
其中,所述聚碳酸酯二醇的平均分子量为500~1500;优选地,所述聚碳酸酯二醇的平均分子量为1000;
所述MDI-50为2,4-二苯基甲烷二异氰酸酯与4,4-二苯基甲烷二异氰酸酯的混合物;
所述聚碳酸酯二醇和MDI-50的重量份之比为1~4:1;
作为一种优选的实施方案,所述有机磷选自磷酸三(2-氯乙基)酯、磷酸三(2-氯丙基)酯、甲基膦酸二甲酯、磷酸三乙酯、三(2-氯乙基)磷酸酯、四(2-氯乙基)二亚乙基醚二磷酸酯、四(2-氯乙基)亚乙基二磷酸酯、聚磷酸铵、磷酸三苯酯、乙基磷酸二乙酯中的一种或多种;优选地,所述有机磷为甲基膦酸二甲酯;
作为一种优选的实施方案,所述聚醚多元醇的平均分子量为3500~4500,羟值为20~30mgKOH/g;优选地,所述聚醚多元醇的平均分子量为4000,羟值为26.5~29.5mgKOH/g;
作为一种优选的实施方案,所述填料选自碳酸钙、氧化钙、炭黑、碱金属硅铝酸盐、高岭土、滑石粉、硅微粉中的一种或多种;优选地,所述填料为碱金属硅铝酸盐;进一步优选地,所述碱金属硅铝酸盐的平均有效孔径为0.1~1μm;更进一步优选地,所述碱金属硅铝酸盐的平均有效孔径为0.3μm;
作为一种优选的实施方案,所述助剂选自聚硅氧烷混合物、聚醚改性聚硅氧烷、生石灰、有机硅、丙烯酸类物质中的一种或多种;优选地,所述助剂选自聚硅氧烷混合物;进一步优选地,所述聚硅氧烷混合物的相对密度为0.95~1.00g/cm3;更进一步优选地,所述聚硅氧烷混合物的相对密度为0.99g/cm3;
作为一种优选的实施方案,所述增强树脂选自聚乙烯基芳香烃树脂、聚天门冬氨酸酯树脂中的一种或多种;优选地,所述增强树脂为聚天门冬氨酸酯树脂;
作为一种优选的实施方案,所述聚天门冬氨酸酯树脂中NH当量为260~290g/mol,25℃时粘度为700-2500mPas;优选地,所述聚天门冬氨酸酯树脂中NH当量为277g/mol,25℃时粘度为800-2000mPas;
作为一种优选的实施方案,所述固化剂为自制所得,其制备方法为:
将70~80重量份二苯基甲烷二异氰酸酯和20~30重量份MDI-50混合后常压搅拌20~50min,真空脱泡15min,随后加入0.2~0.5重量份助剂搅拌5~20min,真空脱泡5min,放空即得。
其中,所述二苯基甲烷二异氰酸酯的-NOC值为30~35%,25℃时粘度为200-300cPs;优选地,所述二苯基甲烷二异氰酸酯的-NOC值为30.8%,25℃时粘度为220cPs
本发明第二方面提供了一种高伸长率,自粘型聚氨酯封装材料的制备方法,包括如下步骤:
(1)将改性聚醚多元醇、有机磷、聚醚多元醇投入反应釜中,在真空状态下,升温到110~120℃,真空:0.094MP,保持2.5-3小时;
(2)冷却到75~85℃取样测水分,水分在0.05%左右,加入填料,真空搅拌下保温反应0.5~2小时;
(3)冷却到60~70℃加入增强树脂、自制预聚体、助剂、固化剂真空下搅拌30~60min取样测粘度和水分,合格后放料。
有益效果:
(1)本申请中通过利用聚碳酸酯二醇和MDI-50合成自制预聚体,与改性聚醚多元醇、有机磷、聚醚多元醇、填料、助剂、增强树脂、固化剂分批次加入充分混合制备聚氨酯封装材料。所得密封材料具有长久自粘性、高伸长率、高拉伸强度、高绝缘性。此外,该聚氨酯密封材料还具有耐水、防霉、防震、导热、耐高温阻燃等特性,可广泛用于电子元器件密封胶领域,很好地保护电子元器件。
(2)本申请中加入的异氰酸酯为基体的固化剂与改性聚醚多元醇、聚醚多元醇发生交联固化反应,制备得到从聚氨酯密封材料具有优异的粘结性、高玻璃化转变温度和拉伸强度、低介电常数,但是同时其伸长率也较低。本申请人意外发现,通过将70~80重量份二苯基甲烷二异氰酸酯、20~30重量份MDI-50、0.2~0.5重量份助剂特定混合后作为固化剂,在自制预聚体、增强树脂等组分的协同作用下,可以与体系中的改性聚醚多元醇、聚醚多元醇,尤其是与聚四氢呋喃醚二醇、平均分子量为4000,羟值为26.5~29.5mgKOH/g的聚醚多元醇更好地作用,维持聚氨酯密封材料优异的粘结性、高玻璃化转变温度和拉伸强度、低介电常数的同时,赋予其更高的伸长率。可能原因是,选用两种异氰酸酯复配与助剂混合后,增加了体系中硬段含量,分子间交联密度增大,分子间作用力增加,极性基团在电场中取向运动受到抑制,同时又不会由于刚性基团的增加使介电常数升高,而且改善了密封材料的粘度,使其保持适宜的硬度,密封胶固化后不会太脆或太软。
(3)本申请为单组分聚氨酯密封材料,制备工艺简单,条件可控易实现,而且可以直接使用,避免了双组份聚氨酯密封材料使用过程中两组分不能均匀混合导致密封效果差的问题。
具体实施方式
实施例1.
1、一种高伸长率,自粘型聚氨酯封装材料,按重量百分比计,制备原料包括:
改性聚醚多元醇55%、自制预聚体15%;有机磷3%、聚醚多元醇15%、填料5%、助剂0.3%、增强树脂5%、固化剂补充至100%;
所述改性聚醚多元醇为聚四氢呋喃多元醇;所述聚四氢呋喃多元醇为聚四氢呋喃醚二醇(日本保土谷化学);
所述自制预聚体的制备方法为:
在容器中加入脱水处理的聚碳酸酯二醇,打开搅拌,温度升到60℃时,开始缓慢滴加计量的MDI-50,维持反应温度在75℃,控制滴加在1小时完成,继续在此温度下反应2小时,出料。
所述聚碳酸酯二醇的平均分子量为1000(日本旭化成化学株式会社,型号T5651);
所述聚碳酸酯二醇和MDI-50的重量份之比为2.5:1;
所述有机磷为甲基膦酸二甲酯;
所述聚醚多元醇的平均分子量为4000,羟值为26.5~29.5mgKOH/g(济南汇锦川商贸有限公司,型号:DL-4000D);
所述填料为碱金属硅铝酸盐;所述碱金属硅铝酸盐的平均有效孔径为0.3μm;
所述助剂选自聚硅氧烷混合物;所述聚硅氧烷混合物的相对密度为0.99g/cm3;
所述增强树脂为聚天门冬氨酸酯树脂;所述聚天门冬氨酸酯树脂中NH当量为277g/mol,25℃时粘度为800-2000mPas(深圳飞扬骏研新材料股份有限公司,型号:F420);
所述固化剂为自制所得,其制备方法为:
将75重量份二苯基甲烷二异氰酸酯和25重量份MDI-50混合后常压搅拌30min,真空脱泡15min,随后加入0.3重量份助剂搅拌5min,真空脱泡5min,放空即得。
所述二苯基甲烷二异氰酸酯的-NOC值为30.8%,25℃时粘度为220cPs(亨斯迈,型号5005);
2、一种高伸长率,自粘型聚氨酯封装材料的制备方法,包括如下步骤:
(1)将改性聚醚多元醇、有机磷、聚醚多元醇投入反应釜中,在真空状态下,升温到115℃,真空:0.094MP,保持3小时;
(2)冷却到80℃取样测水分,水分在0.05%,加入填料,真空搅拌下保温反应1小时;
(3)冷却到65℃加入增强树脂、自制预聚体、助剂、固化剂真空下搅拌45min取样测粘度和水分,合格后放料。
实施例2:
1、一种高伸长率,自粘型聚氨酯封装材料,与实施例1的不同之处在于:
改性聚醚多元醇55%、自制预聚体16%;有机磷3%、聚醚多元醇15%、填料4%、助剂0.4%、增强树脂6%、固化剂补充至100%;
2、一种高伸长率,自粘型聚氨酯封装材料的制备方法,同实施例1。
对比例1:
1、一种高伸长率,自粘型聚氨酯封装材料,与实施例1的不同之处在于:
所述自制预聚体的制备方法为:
在容器中加入脱水处理的聚碳酸酯二醇,打开搅拌,温度升到60℃时,开始缓慢滴加计量的MDI-50,维持反应温度在75℃,控制滴加在1小时完成,继续在此温度下反应2小时,出料。
所述聚碳酸酯二醇的平均分子量为2000(日本旭化成化学株式会社,型号T5652)
2、一种高伸长率,自粘型聚氨酯封装材料的制备方法,同实施例1。
对比例2:
1、一种高伸长率,自粘型聚氨酯封装材料,与实施例1的不同之处在于:
所述固化剂为自制所得,其制备方法为:
将75重量份二苯基甲烷二异氰酸酯和25重量份MDI-50混合后常压搅拌30min,真空脱泡15min放空即得。
2、一种高伸长率,自粘型聚氨酯封装材料的制备方法,同实施例1。
对比例3:
1、一种高伸长率,自粘型聚氨酯封装材料,与实施例1的不同之处在于:
所述聚醚多元醇的平均分子量为2000,羟值为54.5-57.5mgKOH/g;(济南汇锦川商贸有限公司,型号:DL-2000D)
2、一种高伸长率,自粘型聚氨酯封装材料的制备方法,同实施例1。
性能测试
依据国家标准对实施例及对比例进行
表1 实施例1测试结果
表2 实施例及对比例测试结果
硬度(Shore-A) | 介电常数 | 拉伸强度 | 伸长率 | |
实施例1 | 10 | 4 | 36MPa | 500% |
实施例2 | 9 | 5 | 37MPa | 489% |
对比例1 | 15 | 8 | 38MPa | 451% |
对比例2 | 17 | 10 | 28MPa | 432% |
对比例3 | 14 | 13 | 23MPa | 463% |
Claims (10)
1.一种高伸长率,自粘型聚氨酯封装材料,按重量份计,其特征在于,按重量百分比计,制备原料包括:
改性聚醚多元醇50~60%、自制预聚体10~20%、有机磷2~4%、聚醚多元醇10~20%、填料3~6%、助剂0.2~0.5%、增强树脂1~10%、固化剂1~20%。
2.如权利要求1所述的一种高伸长率,自粘型聚氨酯封装材料,其特征在于,所述改性聚醚多元醇选自硅烷改性聚醚多元醇、环氧树脂改性聚醚多元醇、氧化乙烯均聚物、聚氧化乙烯多元醇、氧化丙烯均聚物、聚氧化丙烯多元醇、聚四氢呋喃多元醇、蓖麻油改性聚醚多元醇中的一种或多种。
3.如权利要求1或2所述的一种高伸长率,自粘型聚氨酯封装材料,其特征在于,所述改性聚醚多元醇为聚四氢呋喃多元醇。
4.如权利要求1所述的一种高伸长率,自粘型聚氨酯封装材料,其特征在于,所述自制预聚体的制备方法为:
在容器中加入脱水处理的聚碳酸酯二醇,打开搅拌,温度升到60℃时,开始缓慢滴加计量的MDI-50,维持反应温度在70~80℃,控制滴加在1小时完成,继续在此温度下反应2小时,出料。
5.如权利要求4所述的一种高伸长率,自粘型聚氨酯封装材料,其特征在于,所述聚碳酸酯二醇的平均分子量为500~1500。
6.如权利要求1所述的一种高伸长率,自粘型聚氨酯封装材料,其特征在于,所述有机磷选自磷酸三(2-氯乙基)酯、磷酸三(2-氯丙基)酯、甲基膦酸二甲酯、磷酸三乙酯、三(2-氯乙基)磷酸酯、四(2-氯乙基)二亚乙基醚二磷酸酯、四(2-氯乙基)亚乙基二磷酸酯、聚磷酸铵、磷酸三苯酯、乙基磷酸二乙酯中的一种或多种。
7.如权利要求1所述的一种高伸长率,自粘型聚氨酯封装材料,其特征在于,所述填料选自碳酸钙、氧化钙、炭黑、碱金属硅铝酸盐、高岭土、滑石粉、硅微粉中的一种或多种。
8.如权利要求1所述的一种高伸长率,自粘型聚氨酯封装材料,其特征在于,所述增强树脂选自聚乙烯基芳香烃树脂、聚天门冬氨酸酯树脂中的一种或多种。
9.如权利要求1所述的一种高伸长率,自粘型聚氨酯封装材料,其特征在于,所述固化剂为自制所得,其制备方法为:
将70~80重量份二苯基甲烷二异氰酸酯和20~30重量份MDI-50混合后常压搅拌20~50min,真空脱泡15min,随后加入0.2~0.5重量份助剂搅拌5~20min,真空脱泡5min,放空即得。
10.一种如权利要求1所述的高伸长率,自粘型聚氨酯封装材料的制备方法,其特征在于,包括如下步骤:
(1)将改性聚醚多元醇、有机磷、聚醚多元醇投入反应釜中,在真空状态下,升温到110~120℃,真空:0.094MP,保持2.5-3小时;
(2)冷却到75~85℃取样测水分,水分在0.05%左右,加入填料,真空搅拌下保温反应0.5~2小时;
(3)冷却到60~70℃加入增强树脂、自制预聚体、助剂、固化剂真空下搅拌30~60min取样测粘度和水分,合格后放料。
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