CN111907155B - 中间膜及包含该中间膜的层合玻璃 - Google Patents
中间膜及包含该中间膜的层合玻璃 Download PDFInfo
- Publication number
- CN111907155B CN111907155B CN202010291412.0A CN202010291412A CN111907155B CN 111907155 B CN111907155 B CN 111907155B CN 202010291412 A CN202010291412 A CN 202010291412A CN 111907155 B CN111907155 B CN 111907155B
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- China
- Prior art keywords
- laminated glass
- interlayer
- intermediate film
- sodium
- potassium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000005340 laminated glass Substances 0.000 title claims abstract description 155
- 239000011229 interlayer Substances 0.000 claims abstract description 58
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims abstract description 47
- 239000011521 glass Substances 0.000 claims abstract description 36
- 230000002093 peripheral effect Effects 0.000 claims abstract description 30
- 229920005989 resin Polymers 0.000 claims abstract description 27
- 239000011347 resin Substances 0.000 claims abstract description 27
- 239000004014 plasticizer Substances 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims description 23
- 159000000000 sodium salts Chemical class 0.000 claims description 12
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 11
- 239000011734 sodium Substances 0.000 claims description 11
- 229910052708 sodium Inorganic materials 0.000 claims description 10
- 159000000001 potassium salts Chemical class 0.000 claims description 9
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 8
- 239000011591 potassium Substances 0.000 claims description 8
- 229910052700 potassium Inorganic materials 0.000 claims description 8
- 150000002148 esters Chemical class 0.000 claims description 6
- -1 2-butoxyethoxy Chemical group 0.000 claims description 5
- FRQDZJMEHSJOPU-UHFFFAOYSA-N Triethylene glycol bis(2-ethylhexanoate) Chemical compound CCCCC(CC)C(=O)OCCOCCOCCOC(=O)C(CC)CCCC FRQDZJMEHSJOPU-UHFFFAOYSA-N 0.000 claims description 5
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 claims description 4
- GCDUWJFWXVRGSM-UHFFFAOYSA-N 2-[2-(2-heptanoyloxyethoxy)ethoxy]ethyl heptanoate Chemical compound CCCCCCC(=O)OCCOCCOCCOC(=O)CCCCCC GCDUWJFWXVRGSM-UHFFFAOYSA-N 0.000 claims description 3
- JEYLQCXBYFQJRO-UHFFFAOYSA-N 2-[2-[2-(2-ethylbutanoyloxy)ethoxy]ethoxy]ethyl 2-ethylbutanoate Chemical compound CCC(CC)C(=O)OCCOCCOCCOC(=O)C(CC)CC JEYLQCXBYFQJRO-UHFFFAOYSA-N 0.000 claims description 3
- SSKNCQWPZQCABD-UHFFFAOYSA-N 2-[2-[2-(2-heptanoyloxyethoxy)ethoxy]ethoxy]ethyl heptanoate Chemical compound CCCCCCC(=O)OCCOCCOCCOCCOC(=O)CCCCCC SSKNCQWPZQCABD-UHFFFAOYSA-N 0.000 claims description 3
- GYHPTPQZVBYHLC-UHFFFAOYSA-N 2-[2-[2-[2-(2-ethylhexanoyloxy)ethoxy]ethoxy]ethoxy]ethyl 2-ethylhexanoate Chemical compound CCCCC(CC)C(=O)OCCOCCOCCOCCOC(=O)C(CC)CCCC GYHPTPQZVBYHLC-UHFFFAOYSA-N 0.000 claims description 3
- FTSXVYQZLNPTCM-UHFFFAOYSA-N (3-benzoyloxy-2,2,4-trimethylpentyl) benzoate Chemical compound C=1C=CC=CC=1C(=O)OCC(C)(C)C(C(C)C)OC(=O)C1=CC=CC=C1 FTSXVYQZLNPTCM-UHFFFAOYSA-N 0.000 claims description 2
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 2
- 239000004280 Sodium formate Substances 0.000 claims description 2
- 238000004587 chromatography analysis Methods 0.000 claims description 2
- 239000000084 colloidal system Substances 0.000 claims description 2
- AXZAYXJCENRGIM-UHFFFAOYSA-J dipotassium;tetrabromoplatinum(2-) Chemical compound [K+].[K+].[Br-].[Br-].[Br-].[Br-].[Pt+2] AXZAYXJCENRGIM-UHFFFAOYSA-J 0.000 claims description 2
- ZUFQCVZBBNZMKD-UHFFFAOYSA-M potassium 2-ethylhexanoate Chemical compound [K+].CCCCC(CC)C([O-])=O ZUFQCVZBBNZMKD-UHFFFAOYSA-M 0.000 claims description 2
- 235000011056 potassium acetate Nutrition 0.000 claims description 2
- WFIZEGIEIOHZCP-UHFFFAOYSA-M potassium formate Chemical compound [K+].[O-]C=O WFIZEGIEIOHZCP-UHFFFAOYSA-M 0.000 claims description 2
- 229910001487 potassium perchlorate Inorganic materials 0.000 claims description 2
- LYWPJPGMDLOUDX-UHFFFAOYSA-M potassium;2-ethylbutanoate Chemical compound [K+].CCC(CC)C([O-])=O LYWPJPGMDLOUDX-UHFFFAOYSA-M 0.000 claims description 2
- 239000001632 sodium acetate Substances 0.000 claims description 2
- 235000017281 sodium acetate Nutrition 0.000 claims description 2
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 claims description 2
- 235000019254 sodium formate Nutrition 0.000 claims description 2
- BAZAXWOYCMUHIX-UHFFFAOYSA-M sodium perchlorate Chemical compound [Na+].[O-]Cl(=O)(=O)=O BAZAXWOYCMUHIX-UHFFFAOYSA-M 0.000 claims description 2
- 229910001488 sodium perchlorate Inorganic materials 0.000 claims description 2
- BLSRNVDCHVKXSO-UHFFFAOYSA-M sodium;2-ethylbutanoate Chemical compound [Na+].CCC(CC)C([O-])=O BLSRNVDCHVKXSO-UHFFFAOYSA-M 0.000 claims description 2
- VYPDUQYOLCLEGS-UHFFFAOYSA-M sodium;2-ethylhexanoate Chemical compound [Na+].CCCCC(CC)C([O-])=O VYPDUQYOLCLEGS-UHFFFAOYSA-M 0.000 claims description 2
- PZTAGFCBNDBBFZ-UHFFFAOYSA-N tert-butyl 2-(hydroxymethyl)piperidine-1-carboxylate Chemical group CC(C)(C)OC(=O)N1CCCCC1CO PZTAGFCBNDBBFZ-UHFFFAOYSA-N 0.000 claims description 2
- DLZBUNUDESZERL-UHFFFAOYSA-N 1-o-heptyl 6-o-nonyl hexanedioate Chemical compound CCCCCCCCCOC(=O)CCCCC(=O)OCCCCCCC DLZBUNUDESZERL-UHFFFAOYSA-N 0.000 claims 1
- GPZYYYGYCRFPBU-UHFFFAOYSA-N 6-Hydroxyflavone Chemical compound C=1C(=O)C2=CC(O)=CC=C2OC=1C1=CC=CC=C1 GPZYYYGYCRFPBU-UHFFFAOYSA-N 0.000 claims 1
- SXKCDRRSQHPBOI-UHFFFAOYSA-N 6-o-cyclohexyl 1-o-hexyl hexanedioate Chemical compound CCCCCCOC(=O)CCCCC(=O)OC1CCCCC1 SXKCDRRSQHPBOI-UHFFFAOYSA-N 0.000 claims 1
- PYGXAGIECVVIOZ-UHFFFAOYSA-N Dibutyl decanedioate Chemical compound CCCCOC(=O)CCCCCCCCC(=O)OCCCC PYGXAGIECVVIOZ-UHFFFAOYSA-N 0.000 claims 1
- FANBESOFXBDQSH-UHFFFAOYSA-N Ethyladipic acid Chemical compound CCC(C(O)=O)CCCC(O)=O FANBESOFXBDQSH-UHFFFAOYSA-N 0.000 claims 1
- WNLRTRBMVRJNCN-UHFFFAOYSA-L adipate(2-) Chemical compound [O-]C(=O)CCCCC([O-])=O WNLRTRBMVRJNCN-UHFFFAOYSA-L 0.000 claims 1
- OJXOOFXUHZAXLO-UHFFFAOYSA-M magnesium;1-bromo-3-methanidylbenzene;bromide Chemical compound [Mg+2].[Br-].[CH2-]C1=CC=CC(Br)=C1 OJXOOFXUHZAXLO-UHFFFAOYSA-M 0.000 claims 1
- 229920001223 polyethylene glycol Polymers 0.000 claims 1
- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical group [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 claims 1
- UWHCKJMYHZGTIT-UHFFFAOYSA-N tetraethylene glycol Chemical compound OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 claims 1
- 238000005227 gel permeation chromatography Methods 0.000 abstract description 8
- 239000000523 sample Substances 0.000 description 22
- 239000010410 layer Substances 0.000 description 18
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 14
- 230000032798 delamination Effects 0.000 description 14
- 239000004372 Polyvinyl alcohol Substances 0.000 description 9
- 229920002451 polyvinyl alcohol Polymers 0.000 description 9
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 7
- 239000003643 water by type Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 4
- 239000005038 ethylene vinyl acetate Substances 0.000 description 4
- 229920003023 plastic Polymers 0.000 description 4
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- 230000009467 reduction Effects 0.000 description 4
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- 230000000930 thermomechanical effect Effects 0.000 description 4
- GDXHBFHOEYVPED-UHFFFAOYSA-N 1-(2-butoxyethoxy)butane Chemical compound CCCCOCCOCCCC GDXHBFHOEYVPED-UHFFFAOYSA-N 0.000 description 3
- MBGYSHXGENGTBP-UHFFFAOYSA-N 6-(2-ethylhexoxy)-6-oxohexanoic acid Chemical compound CCCCC(CC)COC(=O)CCCCC(O)=O MBGYSHXGENGTBP-UHFFFAOYSA-N 0.000 description 3
- DQXBYHZEEUGOBF-UHFFFAOYSA-N but-3-enoic acid;ethene Chemical compound C=C.OC(=O)CC=C DQXBYHZEEUGOBF-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
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- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- NXQMCAOPTPLPRL-UHFFFAOYSA-N 2-(2-benzoyloxyethoxy)ethyl benzoate Chemical compound C=1C=CC=CC=1C(=O)OCCOCCOC(=O)C1=CC=CC=C1 NXQMCAOPTPLPRL-UHFFFAOYSA-N 0.000 description 2
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
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- 230000007774 longterm Effects 0.000 description 2
- 125000005461 organic phosphorous group Chemical group 0.000 description 2
- 235000011007 phosphoric acid Nutrition 0.000 description 2
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- 238000002360 preparation method Methods 0.000 description 2
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- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 2
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- 241000239290 Araneae Species 0.000 description 1
- DKMHDEWMVWNITB-UHFFFAOYSA-N C(CCCCCCC)C(C(=O)O)(CCCC(=O)O)CCCCCCCC.C(CCCCC(=O)OCCCCCCCC)(=O)OCCCCCCCC Chemical compound C(CCCCCCC)C(C(=O)O)(CCCC(=O)O)CCCCCCCC.C(CCCCC(=O)OCCCCCCCC)(=O)OCCCCCCCC DKMHDEWMVWNITB-UHFFFAOYSA-N 0.000 description 1
- 241000907903 Shorea Species 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- IRZWYOFWPMYFHG-UHFFFAOYSA-N butanal Chemical compound CCCC=O.CCCC=O IRZWYOFWPMYFHG-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
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- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
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- 239000000463 material Substances 0.000 description 1
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- 238000003908 quality control method Methods 0.000 description 1
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- 229910001415 sodium ion Inorganic materials 0.000 description 1
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Abstract
本发明公开了一种用于层合玻璃的中间膜,其包含:(a)聚乙烯醇缩丁醛(PVB)树脂,其平均分子量(Mw)以胶体渗透层析法(Gel Permeation Chromatography,GPC)测量为约175000至约210000道尔顿(Dalton);以及(b)塑化剂,其含量为约30至约50pph(parts per hundred)。该中间膜夹于二玻璃板之间而形成层合玻璃,该层合玻璃保存于50℃的温度及95%的相对湿度(RH)28天之后,该层合玻璃的外围区域较该层合玻璃的中间区域具有更大的敲击黏附力值(pummel adhesion value)。本发明的层合玻璃表现出改善的耐久性,并且即使在高温及高湿度的条件下也不会随时间分层。
Description
技术领域
本发明涉及一种中间膜(interlayer film)及包含该中间膜的一种层合玻璃。该中间膜为该层合玻璃提供改善的黏合性能,从而有助于避免玻璃分层。
背景技术
层合玻璃为一种安全玻璃,在破碎时可固定在一起。由一夹层包含在两层或更多层玻璃之间,通常该夹层由聚乙烯醇缩丁醛(PVB)或乙烯醋酸乙烯酯(EVA)所制成。即使玻璃破碎,该夹层也能保持玻璃层黏合,并且其高强度可防止玻璃破碎成大而尖锐的碎片。当撞击力不足以完全穿过玻璃时,将产生特有的“蜘蛛网”裂纹形态。
层合玻璃通常使用于可能遭人体碰撞或若玻璃破碎时可能掉落的地方,也有在建筑应用。例如,天窗玻璃及汽车挡风玻璃通常使用层合玻璃。在需要抗飓风建筑的地理区域,层合玻璃通常使用于外部店面、幕墙及窗户。
层合玻璃亦可用于提高窗户的隔音等级,例如,与相同厚度的单片玻璃窗格相比,层合玻璃显著地改善声波衰减。于此用途,可于夹层中使用特殊的“隔音PVB(acousticPVB)”化合物。在使用EVA材料的情况下,则不需要额外的隔音材料,因为EVA即具有隔音性能。于窗户应用层合玻璃的另一优势是可通过PVB及EVA夹层阻隔紫外线辐射。
层合玻璃的问题在于,在高湿度及高温的条件下,水分倾向于穿透玻璃层与夹层之间的开口,进而破坏夹层(例如PVB片)与玻璃层之间的氢键,导致层合玻璃分层。因此,需要改善夹层的黏合性能,以避免分层产生。
发明内容
本发明提供了一种用于层合玻璃的中间膜(interlayer film)(或称夹层膜/间层膜/层间膜/互层膜;亦可简称夹层(interlayer));以及一种包含该中间膜的层合玻璃。该中间膜展现出改善的黏合性,致使包含该中间膜的层合玻璃的质量及耐久性获得改善,例如,避免层合玻璃分层。即使长时间处于高湿度及高温的条件之下,该中间膜使得层合玻璃具有优异的耐高湿度及耐高温的性能。前述性能改善可以至少部分地通过控制该夹层的流动性质来达到,包括在该夹层中含有特定平均分子量的聚乙烯醇缩丁醛(polyvinylbutyral,PVB),以及通过使用金属盐、塑化剂等。
于一实施例中,本发明的中间膜包括:
(a)聚乙烯醇缩丁醛(PVB)树脂,其平均分子量(Mw)以胶体渗透层析法(GelPermeation Chromatography,GPC)测量为约175,000至约210,000道尔顿(Dalton);以及
(b)塑化剂,其含量为约30至约50pph(parts per hundred)。
其中,该中间膜夹于二玻璃板之间而形成层合玻璃,该层合玻璃保存于50℃的温度及95%的相对湿度(RH)28天之后,该层合玻璃的外围区域较该层合玻璃的中间区域具有更大的敲击黏附力值(pummel adhesion value)。该层合玻璃的外围区域为由该层合玻璃周边的外边缘朝向该层合玻璃的中心向内延伸5mm的距离所形成的区域;以及该层合玻璃的中间区域位于该层合玻璃中间,具有50mm x 50mm尺寸的区域。
在一些实施例中,该中间膜夹于二玻璃板之间而形成的层合玻璃,即使该层合玻璃保存于50℃的温度及95%的相对湿度28天之后,该层合玻璃具有的敲击黏附力值,其在该层合玻璃的中间区域基本上不变。
如上所述,本发明实施例的PVB树脂通常具有约175,000至约210,000道尔顿的平均分子量。在一些实施例中,若该PVB树脂还具有至少10wt.%的平均分子量小于50,000的PVB是有利的。
所述的塑化剂的非限制性实例包括一元酸酯、多元酸酯、有机磷酸、有机亚磷酸及其混合物。
该中间膜的各种实施方案可包含金属盐,例如钠盐、钾盐或其混合物。钠盐、钾盐或其混合物的总量可以是,例如,以总量达约80ppm作为钠含量、钾含量或其混合物含量。在一些实施例中,该钠盐不超过40ppm的钠含量,该钾盐不超过40ppm的钾含量。
最后,本发明涉及一种包含本发明的中间膜的层合玻璃。
附图说明
图1为本发明层合玻璃的一实施例的示意图;
图2a为层合玻璃的示意图,其中夹层膜具有不良流动性,导致分层;
图2b为层合玻璃的示意图,其中夹层膜具有良好流动性,因此避免分层;
图3为说明本发明PVB树脂制备方法的流程图;
图4为说明本发明中间膜制备方法的流程图;
图5为说明本发明层合玻璃制备方法的流程图。
附图标记说明:
100 层合玻璃
102 玻璃板
104 中间膜
106 玻璃板
108 周边
110 外围区域
112 中间区域
200 层合玻璃
202 层合玻璃。
具体实施方式
下面通过参考附图描述的实施例是示例性的,仅用于解释本发明,而不能解释为对本发明的限制。
本发明的中间膜包括:
(a)聚乙烯醇缩丁醛(PVB)树脂,其平均分子量(Mw)以胶体渗透层析仪(GPC)测量为约175,000至约210,000道尔顿(Dalton);以及
(b)塑化剂,其含量为约30至约50pph(parts per hundred)。
其中,该中间膜夹于二玻璃板之间而形成层合玻璃,该层合玻璃保存于50℃的温度及95%的相对湿度(RH)28天之后,该层合玻璃的外围区域较该层合玻璃的中间区域具有更大的敲击黏附力值(pummel adhesion value)。该层合玻璃的外围区域为由该层合玻璃周边的外边缘朝向该层合玻璃的中心向内延伸5mm的距离所形成的区域;以及该层合玻璃的中间区域位于该层合玻璃中间,具有50mmx50mm尺寸的区域。
该中间膜(interlayer film,或称夹层膜/间层膜/层间膜/互层膜;亦可简称夹层,interlayer)通常具有至少250μm的流动。本文所用的术语“流动”指当从初始温度加热至最终温度时,在厚度方向上朝该中间膜的表面施加负载压力所造成的变形(厚度减少),其通过热机械分析仪量测。该流动指该中间膜的直径为6mm的样品在其厚度方向上的减少量,前述厚度减少量的计算是将其放入具有2.8mm直径的膨胀探头的热机械分析仪中且负载压力为1.0N,通过将45℃的样品厚度减去135℃的样品厚度而得。
该中间膜的流动通常至少为250μm,并且在一些实施例中可高达500μm。在一些实施例中,该中间膜的流动可为250μm至450μm、250μm至400μm、250μm至350μm、250μm至300μm、255μm至500μm、255μm至450μm、255μm至400μm、255μm至350μm、255μm至300μm、260μm至500μm、260μm至450μm、260μm至400μm、260μm至350μm或260μm至300μm。
本发明中间膜所含的PVB树脂通常具有约175,000至约210,000道尔顿的平均分子量。在一些实施例中,PVB树脂的平均分子量通常为约175,000至约205,000道尔顿、约175,000至约200,000道尔顿、约180,000至约210,000道尔顿、约180,000至约205,000道尔顿或约180,000至约200,000道尔顿。
在一些实施例中,该PVB树脂包含至少10wt.%的平均分子量小于50,000的PVB是有利的。此外,在一些实施例中,该PVB树脂包含至少11wt.%、至少12wt.%或至少13wt.%的平均分子量小于50,000的PVB。例如,该PVB树脂可包含约10至约25wt.%的平均分子量小于50,000的PVB。在一些实施例中,该PVB树脂可包含约11至约25wt.%、约11至约20wt.%、约12至约25wt.%、约12至约20wt.%、约13至约25wt.%或约13至约20wt.%的平均分子量小于50,000的PVB。
在一些实施例中,该PVB树脂具有约60至约80mol.%的缩丁醛化程度是有利的。在一些实施例中,该PVB树脂的缩丁醛化程度可为约60至约75mol.%、约60至约70mol.%、约65至约80mol.%、约65至约75mol.%或约65至约70mol.%。
如上所述,本发明的中间膜可包括一种或多种塑化剂。有用的塑化剂的非限制性实例包括一元酸酯、多元酸酯、有机磷酸、有机亚磷酸及其混合物。更具体但非限制性的实例包括:二丙二醇二苯甲酸酯(dipropylene glycol dibenzonate)、2,2,4-三甲基-1,3-戊二醇二苯甲酸酯(2,2,4-trimethyl-1,3-pentanediol dibenzoate)、三乙二醇二(2-乙基己酸酯)(triethylene glycol di-(2-ethylhexanoate))、四乙二醇二(2-乙基己酸酯)(tetraethylene glycol di-(2-ethylhexanoate))、三乙二醇二(2-乙基丁酸酯)(triethylene glycol di-(2-ethylbutyrate))、三乙二醇二庚酸酯(triethylene glycoldiheptanoate)、四乙二醇二庚酸酯(tetraethylene glycol diheptanoate)、己二酸二己酯(dihexyladipate)、己二酸二辛酯(dioctyladipate)、己二酸己基环己基酯(hexylcyclohexyladipate)、己二酸二异壬酯(diisononyladipate)、己二酸庚基壬基酯(heptylnonyladipate)、癸二酸二丁酯(dibutylsebacate)、三乙二醇双(2-乙基己酸酯)(triethylene glycol bis(2-ethylhexanoate),3GO)、四乙二醇二-2-乙基丁酸酯(tetraethylene glycol di-2-ethylbutyrate,4GH)、己二酸双[2-(2-丁氧基乙氧基)乙酯](bis[2-(2-butoxyethoxy)ethyl]adipate,D600)及其混合物。
本发明的中间膜可包含约30至约50pph的塑化剂。在一些实施例中,该塑化剂的总量为约35至约50pph或约35至约45pph。
本发明的中间膜可任选地包含盐类,例如钠盐、钾盐或其混合物。该钠盐的非限制性实例包括:过氯酸钠、甲酸钠、乙酸钠、2-乙基丁酸钠、2-乙基己酸钠及其混合物。该钾盐的非限制性实例包括:过氯酸钾、甲酸钾、乙酸钾、2-乙基丁酸钾、2-乙基己酸钾及其混合物。该中间膜可仅包含钠盐、仅包含钾盐或同时包含钠盐及钾盐的组合。
该钠盐及/或该钾盐的总量可以为约10至约80ppm(parts per million)的钠含量、钾含量或其混合物含量。在一些实施例中,该钠盐及/或该钾盐的总量可以为约15至约80ppm、约20至约80ppm、约30至约80ppm、约40至约80ppm、约45至约80ppm、约10至约75ppm、约20至约75ppm、约30至约75ppm、约40至约75ppm或约50至约75ppm的钠含量、钾含量或其混合物含量。
该钠盐总量可为约10至约80ppm、约10至约70ppm、约10至约60ppm、约10至约50ppm或约10至约40ppm的钠含量。同样地,该钾盐总量可为约10至约80ppm、约10至约70ppm、约10至约60ppm、约10至约50ppm或约10至约40ppm的钾含量。因此,在一些实施例中,该钠盐总量不超过40ppm的钠含量及/或该钾盐总量不超过40ppm的钾含量。
本发明的中间膜当夹于二玻璃板之间时形成层合玻璃,该层合玻璃具有敲击黏附力值,该层合玻璃保存于50℃的温度及95%的相对湿度28天之后,该层合玻璃的外围区域较该层合玻璃的中间区域具有更大的敲击黏附力值。该层合玻璃的外围区域为由该层合玻璃周边的外边缘朝向该层合玻璃的中心向内延伸5mm的距离所形成的区域。该层合玻璃的中间区域位于该层合玻璃中间,具有50mm x 50mm尺寸的区域。
该中间膜的总面积及厚度可改变。该中间膜的面积通常取决于使用该中间膜的层合玻璃的尺寸。关于厚度,该中间膜可具有约0.3mm至约1.5mm的厚度。在一些实施例中,该中间膜的厚度可为约0.4至约1.5mm、约0.5至约1.5mm、约0.6至约1.5mm、约0.7至约1.5mm、约0.8至约1.5mm、约0.9至约1.5mm、约1至约1.5mm、约0.3至约1.4mm、约0.3至约1.3mm、约0.3至约1.2mm、约0.3至约1.1mm、约0.3至约1mm或约0.5至约1mm。
包含本发明中间膜的层合玻璃保存于50℃的温度及95%的相对湿度28天之后,该层合玻璃的外围区域的敲击黏附力值相较于该层合玻璃的中间区域的敲击黏附力值更大。例如,前述该层合玻璃的外围区域的敲击黏附力值与该层合玻璃的中间区域的敲击黏附力值间的差值可至少为1、至少为2、至少为3、至少为4或至少为5。
在一些实施例中,该层合玻璃保存于50℃的温度及95%的相对湿度28天之后,该层合玻璃的外围区域的敲击黏附力值至少为7。相似地,该层合玻璃保存于50℃的温度及95%的相对湿度28天之后,该层合玻璃的外围区域的敲击黏附力值可至少为8或至少为9。进一步地,该层合玻璃保存于50℃的温度及95%的相对湿度28天之后,该层合玻璃的外围区域的敲击黏附力等级(pummel adhesion level)可至少为7、8或9,并且该层合玻璃的外围区域的敲击黏附力值较该层合玻璃的中间区域的敲击黏附力值更大,两者间的差值至少为1、2、3、4或5。
经保存于50℃的温度及95%的相对湿度28天之后,该层合玻璃的中间区域的敲击黏附力值可为2至8。在一些实施例中,该层合玻璃保存于50℃的温度及95%的相对湿度28天之后,该层合玻璃的中间区域的敲击黏附力值为2至7、3至8、3至7、4至8或4至7。进一步地,该层合玻璃保存于50℃的温度及95%的相对湿度28天之后,该层合玻璃的中间区域的敲击黏附力值可为2至8、2至7、3至8、3至7、4至8或4至7;并且该层合玻璃的外围区域的敲击黏附力值较该层合玻璃的中间区域的敲击黏附力值更大,两者间的差值至少为1、2、3、4或5。
进一步地,通常该层合玻璃的外围区域的敲击黏附力值在该层合玻璃保存于50℃的温度及95%的相对湿度28天之后,较在该层合玻璃保存于50℃的温度及95%的相对湿度28天之前更高。易言之,将该层合玻璃保存于50℃的温度及95%的相对湿度28天,致使该层合玻璃的外围区域的敲击黏附力值增加。前述敲击黏附力值可增加1、2、3、4或5。例如,该层合玻璃的外围区域的敲击黏附力值起初为4(即,在该层合玻璃保存于50℃的温度及95%的相对湿度28天之前,该层合玻璃的外围区域的敲击黏附力值为4),在该层合玻璃保存于50℃的温度及95%的相对湿度28天之后,其敲击黏附力值可增加1、2、3、4或5,使该敲击黏附力值提升为5、6、7、8或9。相似地,例如,起初为6的敲击黏附力值可增加至7、8或9;起初为7的敲击黏附力值可增加至8或9;以及,起初为8的敲击黏附力值可增加至9。
本发明不仅涉及为层合玻璃板提供改善的敲击黏附力值的中间膜,也涉及包含该中间膜的层合玻璃板。通常,层合玻璃板的尺寸(面积)会依据其用途或应用而变化。某些用途或应用需要较大块的层合玻璃板(具有较大面积的层合玻璃),例如:大窗户、墙壁、建筑物外部等。另一方面,某些用途或应用需要较小块的层合玻璃板,例如:手机、计算机屏幕、手表等。
关于厚度,该层合玻璃板可具有约2mm至约8mm的厚度。易言之,两片玻璃加上夹在该两片玻璃之间的中间膜的厚度可为约2mm至约6mm、约3mm至约6mm、约4mm至约6mm、约2mm至约5mm、约3mm至约5mm或约4mm至约5mm。该层合玻璃板的每片单独的玻璃板可具有相同或不同的厚度。例如,单片玻璃板的厚度可为约0.5mm至约3mm、约1mm至约3mm或约1mm至约2mm。
图1为根据本发明其中一方面的层合玻璃的示例性结构示意图。如图1所示,层合玻璃100包括三层。第一层为一底层102,其为玻璃板。第二层为一夹层104,又称中间膜104。第三层为一上层106,亦为玻璃板。底层102及上层106又分别称为第一层102及第三层106。该层合玻璃100具有一外围区域110以及一中间区域112,该外围区域110由该层合玻璃100的周边108的外边缘所形成,该中间区域112为位于该层合玻璃100中间尺寸为50mm x 50mm的区域。
图2a示出一层合玻璃,其中该夹层具有“不良的流动”。在示例性结构的层合玻璃200中,上层106与夹层104之间存在间隙。图2b示出一层合玻璃,其中该夹层具有“良好的流动”。在示例性结构的层合玻璃202中,良好的流动使得上层106与夹层104之间没有间隙。增加的流动致使该夹层能够更容易地填充间隙。此特性防止水分渗入底层102、夹层104及上层106之间,从而防止该层合玻璃分层。
图3所示为于本发明一较佳实施例中制备PVB的方法。于步骤S300中,将聚乙烯醇(PVA)树脂溶于水并加热以提供一PVA溶液。于步骤S302中,将步骤S300的PVA溶液冷却至约10℃或更低。于步骤S304中,添加盐酸(HCl)于步骤S302的PVA溶液并搅拌。于步骤S306中,添加正丁醛(n-butyraldehyde)于步骤S304的溶液并搅拌以提供PVB树脂。于步骤S308中,将步骤S306的PVB树脂加热至约53℃(即,约44℃至约60℃),并维持于此温度约4小时。于步骤S310中,冷却该PVB树脂至至少35℃,并以碳酸氢钠中和。于步骤S312中,分离该PVB树脂,以水清洗并干燥。
图4所示为制备根据本发明的中间膜的方法。于步骤S400中,混合塑化剂、PVB树脂及金属盐。于步骤S402中,搓揉该塑化剂、PVB树脂及金属盐的混合物,并冷却至室温以提供塑料块。于步骤S404中,以热压机热压步骤S402的塑料块以提供一中间膜。
图5所示为制造根据本发明的层合玻璃的方法。于步骤S500中,将一中间膜夹于一对透明的浮制玻璃板之间。于步骤S502中,使用热压以预压该层合玻璃样品。于步骤S504中,以高压釜(autoclave)热压并冷却以提供层合玻璃。
“平均分子量的测定”
该PVB树脂的平均分子量可依据以下程序测定。将一中间膜样品(0.08g)溶解于15mL的四氢呋喃(tetrahydrofuran,THF),并以胶体渗透层析法(GelPermeationChromatography,GPC)分析,接着以对应聚苯乙烯标准品(Waters PS STD)面积的比率计算其分子量。使用以下GPC参数:
装置:Waters 1515PUMP system
探测器:Waters 2414RI
冲提条件:1.0mL/min,THF
管柱:Waters Styragel HR5 THF、Waters Styragel HR4 THF、Waters StyragelHR3 THF、Waters Styragel HR1 THF
“流动的测定”
流动为当使用热机械分析仪测量从初始温度加热至最终温度时,在厚度方向上对样品表面施加负载压力所造成的变形(样品厚度减少)的量测。将储存在干燥器中的中间膜样品切割成直径为6mm的圆盘。将该圆盘置于两平板之间并放入热机械分析仪中,所述的热机械分析仪例如:TMA Q400 Texas Instrument,其膨胀探针(expansion probe)的直径为2.8mm,施力(Force)为1.0N。以每分钟10℃的加热速率将该圆盘从25℃加热至145℃。测量45℃与135℃之间的变形(样品厚度减少),并通过该圆盘在45℃下的厚度减去该圆盘在135℃下的厚度来计算流动。
“敲击黏附力值的测定”
中间膜对于玻璃的黏附力通过敲击黏附力测试(pummel adhesion test)测量,所述的敲击黏附力测试通常用于层合玻璃工业中的质量控管。制备一层合玻璃样品(玻璃/中间膜/玻璃),于-18℃的温度下调节2小时,然后在20至25℃的温度下以自动敲击机器敲击3分钟。对经敲击的层合玻璃样品的中间膜的暴露程度进行评估,并与标准样品进行比较。每一敲击等级(pummel level)皆有一个标准样品。将经敲击的测试样品与每一敲击等级的标准样品进行比较,以确定该测试样品的敲击等级。
预备一层合玻璃样品(宽150mmx长300mm)并以具有尺寸32mm且重量约1lb的锤子的自动敲击机器(例如:GOTECH,中国台湾)敲击。该样品以9mm的水平间隔及10mm的垂直间隔进行敲击,敲击力为94lb-cm/sec。然后确定暴露程度,并依10分制分类,如下表1所示:
表1
暴露程度 | 敲击黏附力值 |
95% | 0 |
85% | 1 |
75% | 2 |
65% | 3 |
55% | 4 |
45% | 5 |
35% | 6 |
25% | 7 |
15% | 8 |
低于5% | 9 |
“分层的测定”
预备层合玻璃样品(宽150mm x长300mm),并保存于50℃的温度及95%的相对湿度28天。在室温下以肉眼判断层合玻璃样品边缘的分层。目视检查20片层合玻璃样品的起泡及/或分层情况,并按照下表2进行分级。
表2
“长期高温及高湿度测试”
为了确定长期高温及高湿度对层合玻璃的黏合性能的影响,制造层合玻璃,并将其立即保存于50℃的温度及95%的相对湿度28天。经保存于50℃的温度及95%的相对湿度28天之后,以上述方法对层合玻璃进行敲击黏附力测试。
以下实施例提供本发明的实施方式。该些实施例是用于说明本发明的技术,而非本质上的限定本发明。
实施例1:制备聚乙烯醇缩丁醛树脂
将100g的聚合度为1,700至约1,800的聚乙烯醇(PVA)溶解于807g的水中,并加热至95℃,以提供一PVA溶液。将该PVA溶液冷却至10℃并加入64g的盐酸。混合10分钟之后,加入54g的正丁醛,搅拌该混合物15分钟,形成聚乙烯醇缩丁醛(PVB)。将含有PVB的该混合物加热至53℃,并在该温度下保持约4小时。经过约4小时后,将该混合物冷却至35℃并以碳酸氢钠中和。将该PVB分离、清洗并干燥。
实施例2:制备中间膜
将36至42重量份(parts by weight)的塑化剂(三乙二醇双(2-乙基己酸酯),3GO)、约100重量份的PVB树脂(实施例1)及金属盐混合(最终该中间膜含有10至200ppm的钠离子或钾离子)以制备一混合物。使用混合机(德国,Mixer 50EHT)在120℃下以35rpm搓揉该混合物15分钟,并冷却至环境温度以提供塑料块。使用热压机(GOTECH,中国台湾,GT-7014-A)在150℃下热压该塑料块3分钟,获得一厚度为0.76mm的薄膜。
实施例3:制造层合玻璃
将实施例2的厚度为0.76mm的薄膜夹于一对浮制玻璃板之间以提供一层合玻璃样品。所使用的玻璃板为洁净浮制玻璃(clean float glass)(厚度2mm,由台玻集团制造),或使用SYP法国绿染色玻璃(F Green Tinted Glass,厚度2mm,由上海耀皮玻璃集团股份有限公司制造)。每块玻璃板宽150mm,长300mm。使用热压机(GOTECH,中国台湾GT-7014-A)在150℃下将该层合玻璃样品预压3分钟。在预压步骤之后,将该层合玻璃样品在135℃及13bar下以高压釜热压120分钟,接着冷却至环境温度以完成层压程序,从而提供层合玻璃样品1至8及对比样品C-1、C-2及C-3。对应的结果如表3所示。
表3
分层测试的结果显示,样品2、3及6没有起泡或分层,样品1、4、5、7及8没有分层但有一些起泡,而在对比样品C-1、C-2及C-3的分层试验中,层合玻璃则出现起泡且分层。
此外,层合玻璃样品1至8的外围区域的敲击黏附力值在保存于50℃的温度及95%的相对湿度28天之后,较保存于50℃的温度及95%的相对湿度28天之前更大。易言之,将层合玻璃样品1至8保存于50℃的温度及95%的相对湿度28天致使其外围区域的敲击黏附力值增加。然而,在对比样品(即,C-1、C-2及C-3)中并未观察到此般结果。由结果可以观察到,层合玻璃样品1至8的敲击黏附力值增加了2至5,尤其在层合玻璃样品3中,其敲击黏附力值(于外围区域)由初始值4增加至9。
如上所述,本发明提供一种中间膜及包含其的层合玻璃,其中该中间膜表现出改善的黏合性能,致使包含该中间膜的层合玻璃的质量及耐久性获得改善。例如,避免层合玻璃分层。此外,本发明的中间膜使得层合玻璃即使经过长时间也能具有优异的耐高湿度及高温的性能。
以上依据图式所示的实施例详细说明了本发明的构造、特征及作用效果,以上所述仅为本发明的较佳实施例,但本发明不以图面所示限定实施范围,凡是依照本发明的构想所作的改变,或修改为等同变化的等效实施例,仍未超出说明书与图示所涵盖的精神时,均应在本发明的保护范围内。
Claims (17)
1.一种中间膜,其特征在于,其包括:
(a)聚乙烯醇缩丁醛树脂,其平均分子量以胶体渗透层析法测量为175000至210000道尔顿;以及
(b)塑化剂,其含量为30至50pph;
其中,该聚乙烯醇缩丁醛树脂包含至少10wt.%的平均分子量小于50000的聚乙烯醇缩丁醛;
其中,该中间膜夹于二玻璃板之间而形成层合玻璃,该层合玻璃保存于50℃的温度及95%的相对湿度28天之后,该层合玻璃的外围区域较该层合玻璃的中间区域具有更大的敲击黏附力值,该层合玻璃的外围区域为由该层合玻璃周边的外边缘朝向该层合玻璃的中心向内延伸5mm的距离所形成的区域,以及
该层合玻璃的中间区域位于该层合玻璃中间,具有50mmx50mm尺寸的区域。
2.根据权利要求1所述的中间膜,其特征在于,其具有至少250μm的流动。
3.根据权利要求1所述的中间膜,其特征在于,其进一步包括:
(c)钠盐、钾盐或其混合物,其总量至高达到80ppm的钠含量、80ppm的钾含量或80ppm的其混合物含量。
4.根据权利要求3所述的中间膜,其特征在于,其中,该钠盐不超过40ppm的钠含量,该钾盐不超过40ppm的钾含量。
5.根据权利要求1所述的中间膜,其特征在于,其中,该聚乙烯醇缩丁醛树脂的缩丁醛化程度为60至80mol.%。
6.根据权利要求1所述的中间膜,其特征在于,其中,该塑化剂选自一元酸酯、多元酸酯、有机磷酸、有机亚磷酸或其混合物。
7.根据权利要求1所述的中间膜,其特征在于,其中,该塑化剂选自二丙二醇二苯甲酸酯、2,2,4-三甲基-1,3-戊二醇二苯甲酸酯、三乙二醇二(2-乙基己酸酯)、四乙二醇二(2-乙基己酸酯)、三乙二醇二(2-乙基丁酸酯)、三乙二醇二庚酸酯、四乙二醇二庚酸酯、己二酸二己酯、己二酸二辛酯oc、己二酸己基环己基酯、己二酸二异壬酯、己二酸庚基壬基酯、癸二酸二丁酯、三乙二醇双(2-乙基己酸酯)、四乙二醇二-2-乙基丁酸酯、己二酸双[2-(2-丁氧基乙氧基)乙酯]或其混合物。
8.根据权利要求3所述的中间膜,其特征在于,其包含一种或多种钠盐,该钠盐选自过氯酸钠、甲酸钠、乙酸钠、2-乙基丁酸钠、2-乙基己酸钠或其混合物。
9.根据权利要求3所述的中间膜,其特征在于,其包含一种或多种钾盐,该钾盐选自过氯酸钾、甲酸钾、乙酸钾、2-乙基丁酸钾、2-乙基己酸钾或其混合物。
10.根据权利要求2所述的中间膜,其特征在于,其具有至少250μm至500μm的流动。
11.根据权利要求1所述的中间膜,其特征在于,其具有0.3mm至1.5mm的厚度。
12.根据权利要求1所述的中间膜,其特征在于,其中,该层合玻璃保存于50℃的温度及95%的相对湿度28天之后,该层合玻璃的外围区域的敲击黏附力值与该层合玻璃的中间区域的敲击黏附力值间的差值至少为2。
13.根据权利要求1所述的中间膜,其特征在于,其中,该层合玻璃保存于50℃的温度及95%的相对湿度28天之后,该层合玻璃的外围区域的敲击黏附力值至少为8。
14.根据权利要求1所述的中间膜,其特征在于,其中,该层合玻璃保存于50℃的温度及95%的相对湿度28天之后,该层合玻璃的外围区域的敲击黏附力值至少为9。
15.根据权利要求1所述的中间膜,其特征在于,其中,该层合玻璃保存于50℃的温度及95%的相对湿度28天之后,该层合玻璃的中间区域的敲击黏附力值为4至7,且该层合玻璃的外围区域的敲击黏附力值与该层合玻璃的中间区域的敲击黏附力值间的差值至少为2。
16.根据权利要求1所述的中间膜,其特征在于,其中,该层合玻璃保存于50℃的温度及95%的相对湿度28天之后,该层合玻璃的中间区域的敲击黏附力值不改变。
17.一种层合玻璃,其特征在于,其包括如权利要求1的中间膜。
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