JP7487140B2 - 中間膜およびそれを含む合わせガラス - Google Patents
中間膜およびそれを含む合わせガラス Download PDFInfo
- Publication number
- JP7487140B2 JP7487140B2 JP2021064808A JP2021064808A JP7487140B2 JP 7487140 B2 JP7487140 B2 JP 7487140B2 JP 2021064808 A JP2021064808 A JP 2021064808A JP 2021064808 A JP2021064808 A JP 2021064808A JP 7487140 B2 JP7487140 B2 JP 7487140B2
- Authority
- JP
- Japan
- Prior art keywords
- laminated glass
- interlayer
- interlayer film
- potassium
- sodium
- 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 description 142
- 239000011229 interlayer Substances 0.000 title claims description 97
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 46
- 239000011521 glass Substances 0.000 claims description 29
- 229920005989 resin Polymers 0.000 claims description 26
- 239000011347 resin Substances 0.000 claims description 26
- 239000000203 mixture Substances 0.000 claims description 24
- 230000002093 peripheral effect Effects 0.000 claims description 18
- 239000004014 plasticizer Substances 0.000 claims description 14
- 159000000000 sodium salts Chemical class 0.000 claims description 14
- 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 9
- 238000005227 gel permeation chromatography Methods 0.000 claims description 9
- 239000011734 sodium Substances 0.000 claims description 9
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 8
- 229910052700 potassium Inorganic materials 0.000 claims description 8
- 239000011591 potassium Substances 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 claims description 7
- 159000000001 potassium salts Chemical class 0.000 claims description 7
- 150000002148 esters Chemical class 0.000 claims description 6
- 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 4
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 claims description 4
- 238000003860 storage Methods 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 125000005461 organic phosphorous group Chemical group 0.000 claims description 3
- 235000011007 phosphoric acid Nutrition 0.000 claims description 3
- 150000003016 phosphoric acids Chemical class 0.000 claims description 3
- 150000007519 polyprotic acids Chemical class 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
- DLZBUNUDESZERL-UHFFFAOYSA-N 1-o-heptyl 6-o-nonyl hexanedioate Chemical compound CCCCCCCCCOC(=O)CCCCC(=O)OCCCCCCC DLZBUNUDESZERL-UHFFFAOYSA-N 0.000 claims description 2
- GCDUWJFWXVRGSM-UHFFFAOYSA-N 2-[2-(2-heptanoyloxyethoxy)ethoxy]ethyl heptanoate Chemical compound CCCCCCC(=O)OCCOCCOCCOC(=O)CCCCCC GCDUWJFWXVRGSM-UHFFFAOYSA-N 0.000 claims description 2
- 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 2
- 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 2
- 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 2
- 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 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
- ZFMQKOWCDKKBIF-UHFFFAOYSA-N bis(3,5-difluorophenyl)phosphane Chemical compound FC1=CC(F)=CC(PC=2C=C(F)C=C(F)C=2)=C1 ZFMQKOWCDKKBIF-UHFFFAOYSA-N 0.000 claims description 2
- SCABKEBYDRTODC-UHFFFAOYSA-N bis[2-(2-butoxyethoxy)ethyl] hexanedioate Chemical compound CCCCOCCOCCOC(=O)CCCCC(=O)OCCOCCOCCCC SCABKEBYDRTODC-UHFFFAOYSA-N 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
- -1 hexyl cyclohexyl adipate cyclohexyladipate Chemical compound 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 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 compound CC(C)(C)OC(=O)N1CCCCC1CO PZTAGFCBNDBBFZ-UHFFFAOYSA-N 0.000 claims description 2
- UWHCKJMYHZGTIT-UHFFFAOYSA-N tetraethylene glycol Chemical compound OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 claims description 2
- SBJWEMJDCMAIOT-AHRAGLCISA-N 1-O-(4-deoxy-alpha-D-xylo-hexopyranosyl)-N-hexacosanoylsphinganine Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCC(=O)N[C@H]([C@H](O)CCCCCCCCCCCCCCC)CO[C@H]1O[C@H](CO)C[C@H](O)[C@H]1O SBJWEMJDCMAIOT-AHRAGLCISA-N 0.000 claims 1
- OBETXYAYXDNJHR-UHFFFAOYSA-N 2-Ethylhexanoic acid Chemical compound CCCCC(CC)C(O)=O OBETXYAYXDNJHR-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
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims 1
- SHZIWNPUGXLXDT-UHFFFAOYSA-N caproic acid ethyl ester Natural products CCCCCC(=O)OCC SHZIWNPUGXLXDT-UHFFFAOYSA-N 0.000 claims 1
- HHECSPXBQJHZAF-UHFFFAOYSA-N dihexyl hexanedioate Chemical compound CCCCCCOC(=O)CCCCC(=O)OCCCCCC HHECSPXBQJHZAF-UHFFFAOYSA-N 0.000 claims 1
- 229940071106 ethylenediaminetetraacetate Drugs 0.000 claims 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 claims 1
- 239000010410 layer Substances 0.000 description 33
- 239000000523 sample Substances 0.000 description 24
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 14
- 230000032798 delamination Effects 0.000 description 13
- 238000000034 method Methods 0.000 description 10
- 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
- 150000003839 salts Chemical class 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 230000000930 thermomechanical effect Effects 0.000 description 5
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000005038 ethylene vinyl acetate Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 229920003023 plastic Polymers 0.000 description 4
- 239000004033 plastic Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 230000009286 beneficial effect Effects 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
- 239000005329 float glass Substances 0.000 description 3
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000010079 rubber tapping Methods 0.000 description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 description 2
- SXKCDRRSQHPBOI-UHFFFAOYSA-N 6-o-cyclohexyl 1-o-hexyl hexanedioate Chemical compound CCCCCCOC(=O)CCCCC(=O)OC1CCCCC1 SXKCDRRSQHPBOI-UHFFFAOYSA-N 0.000 description 1
- 241000239290 Araneae Species 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000001143 conditioned effect Effects 0.000 description 1
- LNPWYCDENKBQEN-UHFFFAOYSA-N decanedioic acid dibutyl decanedioate Chemical compound C(CCCCCCCCC(=O)OCCCC)(=O)OCCCC.C(CCCCCCCCC(=O)O)(=O)O LNPWYCDENKBQEN-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J129/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Adhesives based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Adhesives based on derivatives of such polymers
- C09J129/14—Homopolymers or copolymers of acetals or ketals obtained by polymerisation of unsaturated acetals or ketals or by after-treatment of polymers of unsaturated alcohols
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/50—Properties of the layers or laminate having particular mechanical properties
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/14—Homopolymers or copolymers of acetals or ketals obtained by polymerisation of unsaturated acetals or ketals or by after-treatment of polymers of unsaturated alcohols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/11—Esters; Ether-esters of acyclic polycarboxylic acids
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Description
(a)ゲル浸透クロマトグラフィー(Gel Permeation Chromatography、GPC)で測定した重量平均分子量(Mw)が175,000~210,000ダルトンの範囲内であるポリビニルブチラール(PVB)樹脂と、
(b)含有量が約30~約50pph(parts per hundred)の範囲である可塑剤と、
を含み、
ここで、2枚のガラス板の間に該中間膜が挟まれて合わせガラスを形成し、該合わせガラスは温度50℃、相対湿度(RH)95%で28日間保存された後、該合わせガラスの周囲部が該合わせガラスの中央部に対比して、より大きなパンメル接着値(pummel
adhesion value)を有する。該合わせガラスの周囲部は、該合わせガラス周辺の外周縁から該合わせガラスの中心に向かって内側に5mmの距離延びて形成される領域であり;該合わせガラスの中央部は、該合わせガラスの中央に位置し、寸法50mm×50mmを有する領域である。
(a)ゲル浸透クロマトグラフィー(GPC)で測定した重量平均分子量(Mw)が175,000~210,000ダルトン(dalton)の範囲内であるポリビニルブチラール(PVB)樹脂と、
(b)含有量が約30~約50pph(parts per hundred)の範囲である可塑剤と、
を含み、
ここで、2枚のガラス板の間に該中間膜が挟まれて合わせガラスを形成し、該合わせガラスは温度50℃、相対湿度(RH)95%で28日間保存された後、該合わせガラスの周囲部が該合わせガラスの中央部に対比して、より大きなパンメル接着値(pummel
adhesion value)を有する。該合わせガラスの周囲部は、該合わせガラス周辺の外周縁から該合わせガラスの中心に向かって内側に5mmの距離延びて形成される領域であり;該合わせガラスの中央部は、該合わせガラスの中央に位置し、寸法50mm×50mmを有する領域である。
することには有益である。幾つかの実施形態では、該PVB樹脂のブチラール化度は、約60~約75モル%、約60~約70モル%、約65~約80モル%、約65~約75モル%または約65~約70モル%であり得る。
を約10℃以下に冷却する。ステップS304において、ステップS302のPVA水溶液に対し塩酸(HCl)を添加して撹拌する。ステップS306において、ステップS304の溶液に対しブチルアルデヒド(n-butyraldehyde)を添加して撹拌し、PVB樹脂を得た。ステップS308において、ステップS306のPVB樹脂を約53℃(すなわち、約44℃~約60℃)に加熱し、この温度で約4時間保持する。ステップS310において、該PVB樹脂を少なくとも35℃まで冷却し、重炭酸ナトリウムで中和する。ステップS312において、該PVB樹脂を分離し、水で洗浄して乾燥させる。
PVB樹脂の重量平均分子量は、以下の手順に従って測定できる。中間膜サンプル(0.08g)を15mLのテトラヒドロフラン(tetrahydrofuran、THF)に溶解させ、ゲル浸透クロマトグラフィー(Gel Permeation Chromatography、GPC)で分析し、次にポリスチレン標準品(Waters PS STD)面積に対応する比率でその分子量を計算する。次のGPCパラメータを使用する。
装置:Waters 1515 PUMP system
検出器:Waters 2414 RI
溶出条件:1.0mL/min、THF
カラム:Waters Styragel HR5 THF、Waters Styragel HR4 THF、Waters Styragel HR3 THF、Waters Styragel HR1 THF
流動は、初期温度から最終温度まで加熱されたときに、サンプルの表面に厚み方向に負荷圧力を加えることによって生じる変形(サンプル厚み減少)を熱機械分析装置で測定したものである。乾燥機に保管されている中間膜サンプルを直径6mmのディスクに切断する。該ディスクを2枚の平板の間に配置すると共に熱機械分析装置内に入れる(該熱機械分析装置がTMA Q400 Texas Instrumentで、その拡張プローブ(expansion probe)の直径が2.8mm、加えた力(Force)が1.0Nである)。該ディスクを1分間当たり10℃の加熱速度で25℃から145℃に加熱する。45℃と135℃との間の変形(サンプル厚み減少)を測定し、45℃下での該ディスクの厚みから135℃下での該ディスクの厚みを差し引いて流動を計算した。
中間膜のガラスへの接着力は、合わせガラス産業での品質管理に一般的に使用されるパンメル接着力試験(pummel adhesion test)によって測定される。合わせガラスのサンプル(ガラス/中間膜/ガラス)を作製して、-18°Cの温度に2時間放置して調整し、そして20~25°Cの温度で自動タッピングマシンで3分間打撃
する。打たれた合わせガラスのサンプルの中間膜の露出度を評価し、標準見本と比較した。各パンメルレベル(pummel level)に1個の標準見本がある。打たれた試験用サンプルと各パンメルレベルの標準見本を比較して該試験用サンプルのパンメルレベルを決定する。
、10段階評価尺度に従って分類した。
合わせガラスのサンプル(幅150mm×長さ300mm)を用意し、温度50℃、相対湿度95%で28日保存する。室温下で合わせガラスのサンプル縁端の層間剥離を肉眼で判定した。20枚の合わせガラスのサンプルの膨れおよび/または層間剥離状況を目視検査し、グレード分けを次の表2に示す。
合わせガラスの接着性に対する長期高温高湿の影響を確認するため、合わせガラスを製造し、直ちに温度50℃、相対湿度95%で28日保存される。温度50℃、相対湿度95%で28日保存された後、上記方法で合わせガラスに対しパンメル接着力の試験を行っ
た。
重合度が1,700~約1,800のポリビニルアルコール(PVA)100gを水807gに溶解し、95℃に加熱してPVA水溶液を得た。該PVA水溶液を10℃に冷却し、塩酸64gを加えた。10分間混合した後、ブチルアルデヒド54gを加え、混合物を15分間撹拌してポリビニルブチラール(PVB)を形成した。PVBを含有する該混合物を53℃に加熱し、この温度に約4時間保持する。約4時間経った後、該混合物を35℃に冷却し、重炭酸ナトリウムで中和した。該PVBを分離、洗浄並びに乾燥した。
36~42重量部(parts by weight)の可塑剤(トリエチレングリコールビス(2-エチルヘキサノエート)),3GO)、約100重量部のPVB樹脂(実施例1)および金属塩を混合(最終的に中間膜には10~200ppmのナトリウムイオンまたはカリウムイオンが含まれる)して混合物を調製する。該混合物をミキサー(ドイツのブラベンダー製ミキサー50 EHT)を用い、35rpmで120℃、15分間混練し、周囲温度まで冷却してプラスチックブロックを得た。熱プレス機(台湾GOTECH社製GT-7014-A)を用い、150℃で該プラスチックブロックを3分間熱プレスして厚み0.76mmのフィルムを得た。
実施例2の厚み0.76mmのフィルムを一対のフロートガラス板の間に挟むことで、合わせガラスサンプルを得た。使用したガラス板は、クリーンフロートガラス(clean float glass)(厚み2mm、台湾台玻グループ製)であり、あるいはSYPフランスF-緑色着色ガラス(F Green Tinted Glass、厚み2mm、上海耀皮玻璃集團股▲分▼有限公司製)を使用した。各ガラス板の幅が150mm、長さが300mmとする。熱プレス機(台湾GOTECH社製GT-7014-A)を用い、150℃で該合わせガラスサンプルを3分間予備圧着した。予備圧着ステップの後に、該合わせガラスサンプルを135℃のオートクレーブで13barの圧力で120分間熱圧着し、次いで周囲温度まで冷却してラミネート手順を完了することで、合わせガラスのサンプル1~8および比較サンプルC-1、C-2およびC-3を得た。その結果を表3に示す。
なく、本発明の範囲は特許請求の範囲によってのみ制限される。
102 ガラス板
104 中間膜
106 ガラス板
108 周辺
110 周囲部
112 中央部
200 合わせガラス
202 合わせガラス
Claims (18)
- (a)ゲル浸透クロマトグラフィー(Gel Permeation Chromatography、GPC)で測定した重量平均分子量(Mw)は、175,000~210,000ダルトン(dalton)の範囲内であるポリビニルブチラール(PVB)樹脂と、
(b)含有量が30~50pph(parts per hundred)の範囲である可塑剤と、
を含み、
前記ポリビニルブチラール樹脂は、50,000未満の重量平均分子量を有する少なくとも10重量%のポリビニルブチラールを含有する、中間膜。 - 少なくとも250μmの流動を有する、請求項1に記載の中間膜。
- (c)ナトリウム塩、カリウム塩またはこれらの混合物をさらに含み、その総量は、ナトリウム含有量、カリウム含有量またはこれらの混合物含有量として80ppmまでとする、請求項1に記載の中間膜。
- 前記ナトリウム塩は、ナトリウム含有量として40ppmを超えず、前記カリウム塩がカリウム含有量として40ppmを超えない、請求項3に記載の中間膜。
- 前記ポリビニルブチラール樹脂のブチラール化度は、60~80モル%である、請求項1に記載の中間膜。
- 可塑剤は、一塩基酸エステル、多塩基酸エステル、有機リン酸、有機亜リン酸またはこれらの混合物から選択される、請求項1に記載の中間膜。
- 前記可塑剤は、ジプロピレングリコールジベンゾアート(dipropylene glycol dibenzoate)、2,2,4-トリメチル-1,3-ペンタンジオールジベンゾエート(2,2,4-trimethyl-1,3-pentanediol dibenzoate)、トリエチレングリコールジ(2-エチルヘキサノエート)(triethylene glycol di-(2-ethylhexanoate))、テトラエチレングリコールジ(2-エチルヘキサノエート)(tetraethylene glycol di-(2-ethylhexanoate))、トリエチレングリコールジ(2-エチルブチレート)(triethylene glycol di-(2-ethylbutyrate))、トリエチレングリコールジヘプタノエート(triethylene glycol diheptanoate)、テトラエチレングリコールジヘプタノエート(tetraethylene glycol diheptanoate)、ヘキサン二酸ジヘキシル(dihexyladipate)、ジオクチルアジパート(dioctyladipate)、アジピン酸ヘキシルシクロヘキシル(hexyl cyclohexyladipate)、アジピン酸ジイソノニル(diisononyladipate)、アジピン酸ヘプチルノニル(heptylnonyladipate)、セバシン酸ジブチル(dibutylsebacate)、トリエチレングリコールビス(2-エチルヘキサノエート)(triethylene glycol bis(2-ethylhexanoate),3GO)、テトラエチレングリコールジ-2-エチルブチレート(tetraethylene glycol di-2-ethylbutyrate,4GH)、アジピン酸ビス[2-(2-ブトキシエトキシ)エチル] (bis[2-(2-butoxyethoxy)ethyl] adipate、D600)またはこれらの混合物から選択される、請求項1に記載の中間膜。
- 1種以上の前記ナトリウム塩を含み、前記ナトリウム塩は、過塩素酸ナトリウム、ギ酸ナトリウム、酢酸ナトリウム、2-エチル酪酸ナトリウム、2-エチルヘキサン酸ナトリウムまたはこれらの混合物から選択される、請求項3に記載の中間膜。
- 1種以上の前記カリウム塩を含み、前記カリウム塩は、過塩素酸カリウム、ギ酸カリウム、酢酸カリウム、2-エチル酪酸カリウム、2-エチルヘキサン酸カリウムまたはこれらの混合物から選択される、請求項3に記載の中間膜。
- 少なくとも250μm~500μmの範囲の流動を有する、請求項2に記載の中間膜。
- 0.3mm~1.5mmの範囲の厚みを有する、請求項1に記載の中間膜。
- 2枚のガラス板の間に前記中間膜が挟まれて合わせガラスを形成し、前記合わせガラスは温度50℃、相対湿度(RH)95%で28日間保存された後、前記合わせガラスの周囲部が前記合わせガラスの中央部に対比して、より大きなパンメル接着値(pummel adhesion value)を有し、
前記合わせガラスの周囲部は、前記合わせガラス周辺の外周縁から前記合わせガラスの中心に向かって内側に5mmの距離延びて形成される領域であり、
前記合わせガラスの中央部は、前記合わせガラスの中央に位置し、寸法50mm×50mmを有する領域である、請求項1に記載の中間膜。 - 前記合わせガラスは、温度50℃、相対湿度95%で28日間保存された後、前記合わせガラスの周囲部のパンメル接着値と前記合わせガラスの中央部のパンメル接着値との差は、少なくとも2である、請求項12に記載の中間膜。
- 前記合わせガラスが温度50℃、相対湿度95%で28日間保存された後、前記合わせガラスの周囲部は、少なくとも8のパンメル接着値を有する、請求項12に記載の中間膜。
- 前記合わせガラスが温度50℃、相対湿度95%で28日間保存された後、前記合わせガラスの周囲部は、少なくとも9のパンメル接着値を有する、請求項12に記載の中間膜。
- 前記合わせガラスが温度50℃、相対湿度95%で28日間保存された後、前記合わせガラスの中央部は、4~7の範囲のパンメル接着値を有し、かつ前記合わせガラスの周囲部のパンメル接着値と前記合わせガラスの中央部のパンメル接着値間との差が少なくとも2である、請求項12に記載の中間膜。
- 前記合わせガラスが温度50℃、相対湿度95%で28日間保存された後、前記合わせガラスの中央部のパンメル接着値は、実質的に変わらない、請求項12に記載の中間膜。
- 請求項1に記載の中間膜を含む、合わせガラス。
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