CN107848881A - 夹层玻璃用中间膜、夹层玻璃用中间膜的制造方法和夹层玻璃 - Google Patents
夹层玻璃用中间膜、夹层玻璃用中间膜的制造方法和夹层玻璃 Download PDFInfo
- Publication number
- CN107848881A CN107848881A CN201680041067.7A CN201680041067A CN107848881A CN 107848881 A CN107848881 A CN 107848881A CN 201680041067 A CN201680041067 A CN 201680041067A CN 107848881 A CN107848881 A CN 107848881A
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- CN
- China
- Prior art keywords
- mentioned
- intermediate film
- laminated
- laminated glasses
- glass
- 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.)
- Granted
Links
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- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 description 3
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- 230000001154 acute effect Effects 0.000 description 2
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- 150000002367 halogens Chemical class 0.000 description 2
- JARKCYVAAOWBJS-UHFFFAOYSA-N hexanal Chemical compound CCCCCC=O JARKCYVAAOWBJS-UHFFFAOYSA-N 0.000 description 2
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- 150000003839 salts Chemical class 0.000 description 2
- MIZLGWKEZAPEFJ-UHFFFAOYSA-N 1,1,2-trifluoroethene Chemical group FC=C(F)F MIZLGWKEZAPEFJ-UHFFFAOYSA-N 0.000 description 1
- UNNGUFMVYQJGTD-UHFFFAOYSA-N 2-Ethylbutanal Chemical class CCC(CC)C=O UNNGUFMVYQJGTD-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
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- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- XECAHXYUAAWDEL-UHFFFAOYSA-N acrylonitrile butadiene styrene Chemical compound C=CC=C.C=CC#N.C=CC1=CC=CC=C1 XECAHXYUAAWDEL-UHFFFAOYSA-N 0.000 description 1
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 1
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- 230000000996 additive effect Effects 0.000 description 1
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- 239000003963 antioxidant agent Substances 0.000 description 1
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- 125000002573 ethenylidene group Chemical group [*]=C=C([H])[H] 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
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- 235000019253 formic acid Nutrition 0.000 description 1
- 239000003906 humectant Substances 0.000 description 1
- 239000004611 light stabiliser Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
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- GYHFUZHODSMOHU-UHFFFAOYSA-N nonanal Chemical compound CCCCCCCCC=O GYHFUZHODSMOHU-UHFFFAOYSA-N 0.000 description 1
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- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
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- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
- B32B17/10559—Shape of the cross-section
- B32B17/10577—Surface roughness
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
- B32B17/10559—Shape of the cross-section
- B32B17/10577—Surface roughness
- B32B17/10587—Surface roughness created by embossing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/001—Combinations of extrusion moulding with other shaping operations
- B29C48/002—Combinations of extrusion moulding with other shaping operations combined with surface shaping
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/07—Flat, e.g. panels
- B29C48/08—Flat, e.g. panels flexible, e.g. films
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/16—Articles comprising two or more components, e.g. co-extruded layers
- B29C48/18—Articles comprising two or more components, e.g. co-extruded layers the components being layers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/16—Articles comprising two or more components, e.g. co-extruded layers
- B29C48/18—Articles comprising two or more components, e.g. co-extruded layers the components being layers
- B29C48/21—Articles comprising two or more components, e.g. co-extruded layers the components being layers the layers being joined at their surfaces
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/88—Thermal treatment of the stream of extruded material, e.g. cooling
- B29C48/911—Cooling
- B29C48/9135—Cooling of flat articles, e.g. using specially adapted supporting means
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/88—Thermal treatment of the stream of extruded material, e.g. cooling
- B29C48/919—Thermal treatment of the stream of extruded material, e.g. cooling using a bath, e.g. extruding into an open bath to coagulate or cool the material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
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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
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
-
- 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
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
- B32B17/10559—Shape of the cross-section
- B32B17/10577—Surface roughness
- B32B17/10596—Surface roughness created by melt fracture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
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Abstract
本发明的目的在于,提供能够得到光学变形的发生得到了抑制的夹层玻璃的夹层玻璃用中间膜、该夹层玻璃用中间膜的制造方法、以及使用该夹层玻璃用中间膜而成的夹层玻璃。本发明的夹层玻璃用中间膜是通过利用熔体破裂的挤压唇压花法制造的、由层叠有2层以上树脂层的层叠体构成且在至少一个表面具有多个凹凸的夹层玻璃用中间膜,其中,在所述具有凹凸的表面,根据JIS B 0601(1994)测定的最大高度Ry(μm)与所述凹凸的平均间隔Sm(μm)满足下述式(1),(Ry×Sm)/2≤3500(1)。
Description
技术领域
本发明涉及能够得到光学变形的发生得到了抑制的夹层玻璃的夹层玻璃用中间膜、该夹层玻璃用中间膜的制造方法、以及使用该夹层玻璃用中间膜而成的夹层玻璃。
背景技术
在两张玻璃板之间夹持含有塑化聚乙烯醇缩丁醛的夹层玻璃用中间膜并使它们相互粘接而得的夹层玻璃特别是作为车辆用挡风玻璃而被广泛使用。
在夹层玻璃的制造方法中,例如进行以下方法等:将由卷状体退卷的夹层玻璃用中间膜切割为合适的大小,将该夹层玻璃用中间膜夹持在至少两张玻璃板之间,将由此而得的层叠体放入橡胶袋进行减压抽吸,一边将残留在玻璃板与中间膜之间的空气进行脱气一边进行预压接,接下来,在例如高压釜内进行加热加压来进行正式压接(例如,专利文献1)。
在夹层玻璃的制造工序中,在预压接工序中层叠玻璃与夹层玻璃用中间膜时的脱气性是重要的。因此,出于确保制造夹层玻璃时的脱气性的目的,在夹层玻璃用中间膜的至少一个表面形成了多个凹凸。作为形成这类凹凸的方法,近年来进行了利用熔体破裂的挤压唇压花法(押出リップエンボス法)(例如,专利文献2)。
对于在夹层玻璃用中间膜的表面形成的凹凸,因为其是在预压接工序至正式压接工序中在层叠玻璃与夹层玻璃用中间膜后通过进行压接而被压塌,因此在所得的夹层玻璃中目视几乎观察不到所述凹凸。然而,由于该凹凸,所得的夹层玻璃存在发生光学变形的情况。尤其是在夹层玻璃用中间膜由层叠有2层以上树脂层的层叠体构成的情况下,光学变形的发生显著。在此,夹层玻璃的光学变形是指透过夹层玻璃观察物体时物体看起来扭曲的现象。
作为降低夹层玻璃的光学变形的方法,例如对夹层玻璃用中间膜的表面的凹凸形状进行控制(例如,专利文献3)。然而,实际上充分地防止光学变形的发生是困难的,存在即使能够将光学变形消除至识别前方没有障碍的程度,但光学变形仍以信号、人行横道的闪变这样的形式残留的情况。
现有技术文献
专利文献
专利文献1:日本特开平8-26789号公报
专利文献2:日本特表2010-523379号公报
专利文献3:日本特开2009-190947号公报
发明内容
发明所要解决的课题
本发明鉴于上述现状,其目的在于,提供能够得到光学变形的发生得到了抑制的夹层玻璃的夹层玻璃用中间膜、该夹层玻璃用中间膜的制造方法、以及使用该夹层玻璃用中间膜而成的夹层玻璃。
用于解决课题的手段
本发明的夹层玻璃用中间膜是通过利用熔体破裂的挤压唇压花法制造的、由层叠有2层以上树脂层的层叠体构成且在至少一个表面具有多个凹凸的夹层玻璃用中间膜,在所述具有凹凸的表面,根据JIS B 0601(1994)测定的最大高度Ry(μm)与所述凹凸的平均间隔Sm(μm)满足下述式(1)。
(Ry×Sm)/2≤3500 (1)
以下对本发明进行详述。
本发明人对于在包含层叠有2层以上树脂层的层叠体的夹层玻璃用中间膜中,在通过利用熔体破裂的挤压唇压花法在表面形成凹凸时,即使对表面的凹凸形状进行控制也无法充分地防止光学变形的发生的原因进行了研究。其结果,发现:即使在夹层玻璃用中间膜的阶段控制凹凸形状,经过制造夹层玻璃时的加热、加压,光学变形也会恶化。
本发明人进一步深入研究的结果发现:通过以使夹层玻璃用中间膜的表面的凹凸的最大高度Ry与平均间隔Sm满足一定的关系的方式进行控制,从而能够得到充分地抑制了光学变形的发生的夹层玻璃,从而完成了本发明。
本发明的夹层玻璃用中间膜在至少一个表面具有多个凹凸。由此,能够确保制造夹层玻璃时的脱气性。
本发明的夹层玻璃用中间膜可以仅在一个表面具有上述凹凸,也可以在两个表面具有上述凹凸。其中,从制造夹层玻璃时的脱气性优异的方面出发,优选在两个表面具有凹凸。
对于本发明的夹层玻璃用中间膜来说,在上述具有凹凸的表面,根据JIS B 0601(1994)测定的最大高度Ry(μm)与凹凸的平均间隔Sm(μm)满足上述式(1)。
图1示出了说明上述式(1)中的“(Ry×Sm)/2”的意义的示意图。图1中夹层玻璃用中间膜的表面的凹凸1具有凸部11和凹部12。
上述最大高度Ry是凹凸的高度方向所涉及的参数,在图1中大致相当于凹凸的高度。上述最大高度Ry越小,则存在玻璃与夹层玻璃用中间膜的界面的变形变小、光学变形变小的倾向。另一方面,上述凹凸的平均间隔Sm是凹凸的凹部或凸部的宽度所涉及的参数,在图1中是指相邻的凸部11间的间隔。上述平均间隔Sm越小,则存在玻璃与夹层玻璃用中间膜的界面的变形变小、光学变形变小的倾向。
“(Ry×Sm)/2”的值大致相当于图1中用斜线部表示的三角形的面积。夹层玻璃用中间膜的表面的凹凸中,相邻的2个凸部11和与该相邻的2个凸部11之间的凹部12所围出的区域的面积近似于该三角形的面积。通过将该三角形的面积、即“(Ry×Sm)/2”的值设为3500以下,从而能够防止光学变形的发生。为了进一步防止光学变形的发生,“(Ry×Sm)/2”的值优选为3000以下,更优选为2700以下(即,更优选满足(Ry×Sm)/2≤2700(2)),进一步优选为2500以下,特别优选为2300以下,最优选为2000以下。
关于“(Ry×Sm)/2”的值的下限,没有特别限定,为了充分发挥制造夹层玻璃时的脱气性,优选为1000以上,更优选为1500以上。
只要“(Ry×Sm)/2”的值为3500以下,上述最大高度Ry的值没有特别限定,优选的下限为10μm,优选的上限为25μm。上述最大高度Ry的值在该范围内时,能够防止光学变形的发生,并且能够发挥高脱气性。上述最大高度Ry的值的更优选下限为13μm,更优选上限为22μm,进一步优选下限为15μm,进一步优选上限为20μm。
需要说明的是,上述最大高度Ry例如可以使用小坂研究所公司制“SurfcorderSE300”作为测定仪,在测定时的触针计条件为截止值=2.5mm、基准长度=2.5mm、评价长度=12.5mm、触针的前端半径=2μm、前端角度=60°、测定速度=0.5mm/s的条件下进行测定。在此,将测定时的环境设为23℃和30RH%下,将移动触针的方向设为相对于片材的流动方向的平行方向。
作为表面的凹凸的规格,除Ry之外还存在凹部的沟深度(Rzg)、十点平均粗糙度Rz等,但是即使测定同一表面,也各自呈现不同的值,没有关联。需要说明的是,凹部的沟深度(Rzg)是指JIS B-0601(1994)“表面粗糙度-定义和表示”所规定的、算出以粗糙度曲线的平均线(以使与粗糙度曲线的偏差的平方和成为最小的方式所设定的线)为基准的沟深度并算出所测定的沟数的沟深度的平均值。例如,凹部的沟深度(Rzg)可通过将使用表面粗糙度测定器(小坂研究所制“SE1700α”)测定的数字信号进行数据处理而容易地得到。另外,十点平均糙度可根据JIS B0601-1982进行测定。
只要“(Ry×Sm)/2”的值为3500以下,上述凹凸的平均间隔Sm的值就没有特别限定,优选的下限为140μm,优选的上限为408μm。上述凹凸的平均间隔Sm的值在该范围内时,能够防止光学变形的发生,并且能够发挥高脱气性。上述凹凸的平均间隔Sm的值的更优选下限为159μm,更优选上限为350μm,进一步优选下限为175μm,进一步优选上限为269μm,特别优选上限为233μm。
需要说明的是,上述凹凸的平均间隔Sm例如可以使用小坂研究所公司制“Surfcorder SE300”作为测定仪,在测定时的触针计条件为截止值=2.5mm、基准长度=2.5mm、评价长度=12.5mm、触针的前端半径=2μm、前端角度=60°、测定速度=0.5mm/s的条件下进行测定。另外,测定时的环境为23℃和30RH%下。
通过利用熔体破裂的挤压唇压花法来赋予上述凹凸形状。
熔体破裂是指:在通过将树脂熔融并从模具挤出而进行成形时,若模具出口的剪切应力超过某一临界值,则成形品的表面呈波纹状的现象。通过控制该熔体破裂,能够对夹层玻璃用中间膜的表面赋予凹凸。
为了赋予“(Ry×Sm)/2”的值为3500以下的凹凸,在利用熔体破裂的挤压唇压花法中,对模具入口的树脂压力、树脂的温度、模具的温度、模具出口的宽度、每模具出口的宽度的挤出量、刚从模具出口排出后的膜表面温度、从模具出口至冷却水槽的距离、冷却水槽内的水温等进行控制。例如,升高树脂的温度、模具的温度时,上述最大高度Ry变小,而减小模具出口的宽度时,上述凹凸的平均间隔Sm变小。需要说明的是,上述树脂的温度是指模具入口的树脂温度。此外,通过提高模具入口的树脂压力、增大每模具出口的宽度的挤出量、提高刚从模具出口排出后的膜表面温度、延长从模具出口至冷却水槽的距离、提高冷却水槽内的水温等方法,能够减小Ry。相反地,平均间隔Sm可以通过提高模具入口的树脂压力、增大每模具出口的宽度的挤出量、提高刚从模具出口排出后的膜表面温度、延长从模具出口至冷却水槽的距离、提高冷却水槽内的水温等方法而增大。更具体而言,例如,在40~150kgf/cm2的范围内调节模具入口的树脂压力、在160~250℃的范围内调节树脂的温度、在100~270℃的范围内调节模具的温度、在700~3500mm的范围内调节模具出口的宽度、在130~1700kg/hr·m的范围内调节每模具出口的宽度的挤出量、在170~250℃的范围内调节刚从模具出口排出后的膜表面温度、在10~400mm的范围内调节从模具出口至冷却水槽的距离、在10~70℃的范围内调节冷却水槽内的水温,赋予“(Ry×Sm)/2”的值为3500以下的凹凸。
制造本发明的夹层玻璃用中间膜的方法也是本发明之一,所述制造方法包括通过利用熔体破裂的挤压唇压花法对夹层玻璃用中间膜的至少一个表面赋予多个凹凸的工序,在该工序中,在使用共挤出机对各树脂进行共挤出时,设为以下条件:将模具入口的树脂压力设为40~150kgf/cm2,将树脂的温度设为160~250℃,将模具的温度设为100~270℃,将模具出口的宽度设为700~3500mm,将每模具出口的宽度的挤出量设为130~1700kg/hr·m,将刚从模具出口排出后的膜表面温度设为170~250℃,将从模具出口至冷却水槽的距离设为10~400mm,冷却水槽内的水温设为10~70℃。
本发明的夹层玻璃用中间膜也可以在至少一个表面进一步赋予具有底部连续的沟形状的多个凹部来作为比“(Ry×Sm)/2”的值为3500以下的凹凸(以下,为了进行区别,也称为“第1形状”)更大的凹部(以下也称为“第2形状”)。通过具有这种第2形状,能够进一步提高制造夹层玻璃时的脱气性。
上述第2形状的凹部只要具有至少底部连续的形状(沟形状)即可,可以使用例如刻线状、网格状(块状、球状)等通常对夹层玻璃用中间膜的表面赋予的凹部的形状。上述凹部的形状也可以为压花辊所转印的形状。
上述第2形状的凹部优选:具有底部连续的沟形状,且相邻的上述凹部平行并规则地排列(以下,也称为“刻线状”)。通常,在对在两张玻璃板之间层叠有夹层玻璃用中间膜的层叠体进行压接时的空气的脱气容易度与上述凹部的底部的连通性和平滑性有密切的关系。通过将上述凹部的形状设为刻线状,从而使得该底部的连通性更优异,脱气性显著提高。
需要说明的是,“规则地排列”是指可以为相邻的上述沟形状的凹部平行并等间隔地排列,也可以为相邻的上述刻线状的凹部平行地排列,但并非全部的相邻的上述刻线状的凹部的间隔为等间隔。
图2和图3示出了表示沟形状的凹部等间隔并平行地排列的夹层玻璃用中间膜的一例的示意图。另外,图4示出了表示沟形状的凹部不是等间隔但平行地排列的夹层玻璃用中间膜的一例的示意图。图4中,凹部21和凹部22的间隔A与凹部21和凹部23的间隔B不同。
进而,图5示出了表示在表面具有块状形状的夹层玻璃用中间膜的一例的示意图,图6示出了表示在表面具有球状形状的夹层玻璃用中间膜的一例的示意图。
上述第2形状的凹部根据JIS B 0601(1994)测定的最大高度Ry的优选下限为10μm,优选上限为75μm。通过将上述第2形状的最大高度Ry设为10μm以上,从而能够发挥极优异的脱气性,通过设为75μm以下,从而在夹持于两张玻璃板之间进行压接时凹部变得易于坍塌,能够降低压接时的温度。上述第2形状的最大高度Ry的更优选下限为15μm,更优选上限为50μm,进一步优选下限为25μm,进一步优选上限为40μm。
在上述第2形状的凹部具有底部连续的沟形状且相邻的上述凹部平行并规则地排列的情况下,上述刻线状的凹部的间隔Sm优选为400μm以下,更优选为200μm以下,进一步优选为150μm以下。优选的下限为80μm。
在上述第2形状的凹部具有底部连续的沟形状且相邻的上述凹部平行并规则地排列,并且位于夹层玻璃用中间膜的两面的情况下,优选一个面所具有的上述底部连续的沟形状的凹部与另一个面所具有的上述底部连续的沟形状的凹部的交叉角度θ为10°以上。由此,能够防止保管中层叠的夹层玻璃用中间膜彼此发生粘接(自粘)。上述交叉角θ更优选为20°以上,进一步优选为45°以上,特别优选为90°。
对于上述交叉角θ,例如通过目视或光学显微镜来观察夹层玻璃用中间膜,对于第1表面所具有的底部连续的沟形状的凹部与第2表面所具有的底部连续的沟形状的凹部的交叉角θ,在目视的情况下在两面在凹部平行地用墨液描绘直线,使用量角器对所描绘的直线彼此所成的锐角进行测定。在使用光学显微镜的情况下,对放大了的表面进行拍摄,通过利用图像处理软件等对锐角的角度进行测定,从而能够测定所述交叉角θ。
与上述第2形状的凹部对应地形成的凸部的顶部可以为平面形状,也可以不是平面的形状。需要说明的是,上述凸部的顶部为平面形状的情况下,可以对该顶部的平面进一步施加微细的凹凸。
进而,各凹凸的凸部的高度可以为相同高度,也可以为不同高度,对于上述凹部的深度,只要该凹部的底边连续,则可以为相同深度,也可以为不同深度。
上述凸部的回转半径R优选为200μm以下,更优选为100μm以下,进一步优选为40μm以下,特别优选为25μm以下。由此,能够进一步降低在层叠的状态下保管夹层玻璃用中间膜时的夹层玻璃用中间膜彼此的粘接力(自粘力)。
上述凸部的回转半径R例如可以通过以下方法来测定:将中间膜在相对于刻线状的凹部的方向的垂直方向且膜厚方向进行切割,对其截面用显微镜(例如,OlympusCorporation制“DSX-100”)进行观察,以测定倍率为277倍进行拍摄,进而在将拍摄图像以成为50μ/20mm的方式进行放大显示的状态下,使用附带软件内的测量软件,将描绘内接于凸形状的顶点的圆时的该圆的半径设为该凸部的前端的回转半径。另外,测定时的环境为23℃和30RH%下。
赋予上述第2形状的方法没有特别限定,可举出例如压花辊法、压延辊法、异形挤出法等。其中,从容易获得相邻的该刻线状的凹部平行地形成的形状和并列的形状出发,优选压花辊法。
对于本发明的夹层玻璃用中间膜,优选将夹层玻璃用中间膜浸渍于50℃的温水中10分钟后的流动方向的收缩率为4%以下。通过如上所述地控制夹层玻璃用中间膜的表面的凹凸并且将上述收缩率设为4%以下,从而即使经历制造夹层玻璃时的加热、加压也能够得到充分地抑制了光学变形的发生的夹层玻璃。上述收缩率更优选为3%以下,进一步优选为1.5%以下。
上述收缩率可如下所述地算出:将夹层玻璃用中间膜切割为长条状而制成测定样品,在浸渍于50℃的温水中10分钟的前后对测定样品的流动方向的长度进行测定,通过以下式算出。
收缩率(%)=(浸渍后的流动方向的长度)/(浸渍前的流动方向的长度)×100
需要说明的是,本说明书中夹层玻璃用中间膜的流动方向是指:在制造夹层玻璃用中间膜时,从挤出机挤出原料树脂组合物的方向。
夹层玻璃用中间膜的流动方向例如可以通过以下的方法进行确认。即,可以通过以下方式确认:将夹层玻璃用中间膜在140℃的恒温槽中保管30分钟后,膜的平行方向与垂直方向中收缩率大的方向为流动方向。此外,可以通过该夹层玻璃用中间膜的卷状体的卷曲方向来确认。这是依据:因为夹层玻璃用中间膜的卷状体是在制造夹层玻璃用中间膜时的膜的流动方向进行卷曲,因此卷状体的卷曲方向与制造夹层玻璃用中间膜时的膜的流动方向是相同的。
使夹层玻璃用中间膜的收缩率成为4%以下的方法没有特别限定,可举出降低各工序内、工序间的速度比;通过退火来松弛内部应力等方法。
本发明的夹层玻璃用中间膜包含层叠有2层以上的树脂层的层叠体。
对于上述2层以上的树脂层,通过具有第1树脂层和第2树脂层并且第1树脂层与第2树脂层具有不同的性质,从而能够提供具有仅1层难以实现的各种性能的夹层玻璃用中间膜。
优选上述树脂层包含热塑性树脂。
作为上述热塑性树脂,可举出例如聚偏二氟乙烯、聚四氟乙烯、偏二氟乙烯-六氟丙烯共聚物、聚三氟乙烯、丙烯腈-丁二烯-苯乙烯共聚物、聚酯、聚醚、聚酰胺、聚碳酸酯、聚丙烯酸酯、聚甲基丙烯酸酯、聚氯乙烯、聚乙烯、聚丙烯、聚苯乙烯、聚乙烯醇缩醛、乙烯-乙酸乙烯酯共聚物等。其中,优选上述树脂层含有聚乙烯醇缩醛或乙烯-乙酸乙烯酯共聚物,更优选含有聚乙烯醇缩醛。
上述聚乙烯醇缩醛例如可以通过将聚乙烯醇用醛进行缩醛化来制造。上述聚乙烯醇例如可以通过将聚乙酸乙烯酯进行皂化来制造。上述聚乙烯醇的皂化度通常为70~99.8摩尔%的范围内。
上述聚乙烯醇的平均聚合度优选为200以上、更优选为500以上、进一步优选为1700以上、特别优选大于1700,优选为5000以下、更优选为4000以下、进一步优选为3000以下、特别优选小于3000。上述平均聚合度为上述下限以上时,夹层玻璃的耐贯通性进一步提高。上述平均聚合度为上述上限以下时,中间膜的成形变容易。
需要说明的是,上述聚乙烯醇的平均聚合度通过根据JIS K6726“聚乙烯醇试验方法”的方法求出。
上述聚乙烯醇缩醛所含的缩醛基的碳数没有特别限定。制造上述聚乙烯醇缩醛时使用的醛没有特别限定。上述聚乙烯醇缩醛中的缩醛基的碳数的优选下限为3,优选上限为6。上述聚乙烯醇缩醛中的缩醛基的碳数为3以上时,中间膜的玻璃化转变温度充分降低,另外,能够防止增塑剂的渗出。通过将醛的碳数设为6以下,能够容易地进行聚乙烯醇缩醛的合成,确保生产率。作为上述碳数为3~6的醛,可以为直链状的醛,也可以为支链状的醛,可举出例如正丁醛、正戊醛等。
上述醛没有特别限定。作为上述醛,通常适合使用碳数为1~10的醛。作为上述碳数为1~10的醛,可举出例如丙醛、正丁醛、异丁醛、正戊醛、2-乙基丁醛、正己醛、正辛醛、正壬醛、正癸醛、甲醛、乙醛和苯甲醛等。其中,优选丙醛、正丁醛、异丁醛、正己醛或正戊醛,更优选丙醛、正丁醛或异丁醛,进一步优选正丁醛。上述醛可以仅使用1种,也可以并用2种以上。
上述聚乙烯醇缩醛的羟基的含有率(羟基量)优选为10摩尔%以上、更优选为15摩尔%以上、进一步优选为18摩尔%以上,优选为40摩尔%以下、更优选为35摩尔%以下。上述羟基的含有率为上述下限以上时,中间膜的粘接力进一步提高。另外,上述羟基的含有率为上述上限以下时,中间膜的柔软性提高,中间膜的处理变容易。
上述聚乙烯醇缩醛的羟基的含有率是将羟基所键合的乙烯基量除以主链的全部乙烯基量而求出的摩尔分率用百分率表示的值。上述羟基所键合的乙烯基量例如能够通过根据JIS K6726“聚乙烯醇试验方法”或根据ASTM D1396-92进行测定来求出。
上述聚乙烯醇缩醛的乙酰化度(乙酰基量)优选为0.1摩尔%以上、更优选为0.3摩尔%以上、进一步优选为0.5摩尔%以上,优选为30摩尔%以下、更优选为25摩尔%以下、进一步优选为20摩尔%以下。上述乙酰化度为上述下限以上时,聚乙烯醇缩醛与增塑剂的相容性变高。上述乙酰化度为上述上限以下时,中间膜和夹层玻璃的耐湿性变高。
上述乙酰化度是将从主链的全部乙烯基量中减去缩醛基所键合的乙烯基量和羟基所键合的乙烯基量而得的值除以主链的全部乙烯基量而求出的摩尔分率用百分率表示的值。上述缩醛基所键合的乙烯基量例如能够根据JIS K6728“聚乙烯醇缩丁醛试验方法”或根据ASTM D1396-92进行测定。
上述聚乙烯醇缩醛的缩醛化度(聚乙烯醇缩丁醛树脂的情况下,为缩丁醛化度)优选为50摩尔%以上、更优选为53摩尔%以上、进一步优选为60摩尔%以上、特别优选为63摩尔%以上,优选为85摩尔%以下、更优选为75摩尔%以下、进一步优选为70摩尔%以下。上述缩醛化度为上述下限以上时,聚乙烯醇缩醛与增塑剂的相容性变高。上述缩醛化度为上述上限以下时,用于制造聚乙烯醇缩醛所需的反应时间缩短。
上述缩醛化度是将缩醛基所键合的乙烯基量除以主链的全部乙烯基量而求出的摩尔分率用百分率表示的值。
上述缩醛化度能够通过以下方式算出:通过根据JIS K6728“聚乙烯醇缩丁醛试验方法”的方法或根据ASTM D1396-92的方法,测定乙酰化度和羟基的含有率,由所得的测定结果算出摩尔分率,接下来,从100摩尔%中减去乙酰化度和羟基的含有率,由此算出缩醛化度。
需要说明的是,优选上述羟基的含有率(羟基量)、缩醛化度(缩丁醛化度)和乙酰化度是由通过根据JIS K6728“聚乙烯醇缩丁醛试验方法”的方法测定的结果算出的。聚乙烯醇缩醛为聚乙烯醇缩丁醛树脂的情况下,优选上述羟基的含有率(羟基量)、缩醛化度(缩丁醛化度)和乙酰化度是由通过根据JIS K6728“聚乙烯醇缩丁醛试验方法”的方法测定的结果算出的。
上述树脂层优选包含聚乙烯醇缩醛和增塑剂。
作为上述增塑剂,只要是在夹层玻璃用中间膜中通常使用的增塑剂,则没有特别限定,可举出例如一元有机酸酯、多元有机酸酯等有机增塑剂、有机磷酸化合物、有机亚磷酸化合物等磷酸增塑剂等。
作为上述有机增塑剂,可举出例如三乙二醇-二-2-乙基己酸酯、三乙二醇-二-2-乙基丁酸酯、三乙二醇-二-正庚酸酯、四乙二醇-二-2-乙基己酸酯、四乙二醇-二-2-乙基丁酸酯、四乙二醇-二-正庚酸酯、二乙二醇-二-2-乙基己酸酯、二乙二醇-二-2-乙基丁酸酯、二乙二醇-二-正庚酸酯等。其中,上述树脂层优选包含三乙二醇-二-2-乙基己酸酯、三乙二醇-二-2-乙基丁酸酯或三乙二醇-二-正庚酸酯,更优选包含三乙二醇-二-2-乙基己酸酯。
上述增塑剂的含量没有特别限定。相对于上述热塑性树脂100质量份,上述增塑剂的含量优选为25质量份以上、更优选为30质量份以上,优选为80质量份以下、更优选为70质量份以下。上述增塑剂的含量为上述下限以上时,夹层玻璃的耐贯通性进一步提高。上述增塑剂的含量为上述上限以下时,中间膜的透明性进一步提高。
上述树脂层优选含有粘接力调节剂。特别是制造夹层玻璃时,与玻璃接触的树脂层优选含有上述粘接力调节剂。
作为上述粘接力调节剂,适合使用例如碱金属盐或碱土金属盐。作为上述粘接力调节剂,可举出例如钾、钠、镁等的盐。
作为构成上述盐的酸,可举出例如辛酸、己酸、2-乙基丁酸、丁酸、乙酸、甲酸等羧酸有机酸、或盐酸、硝酸等无机酸。制造夹层玻璃时,对于与玻璃接触的树脂层,作为粘接力调节剂,优选包含镁盐,这是因为能够容易地调节玻璃与树脂层的粘接力。
上述树脂层根据需要也可以含有抗氧化剂、光稳定剂、作为粘接力调节剂的改性硅油、阻燃剂、抗静电剂、耐湿剂、热射线反射剂、热射线吸收剂等添加剂。
本发明的夹层玻璃用中间膜的厚度没有特别限定。从实用方面的观点、以及充分提高隔热性的观点出发,中间膜的厚度优选为0.1mm以上、更优选为0.25mm以上,优选为3mm以下、更优选为1.5mm以下。中间膜的厚度为上述下限以上时,夹层玻璃的耐贯通性提高。
在本发明的夹层玻璃用中间膜中,对于2层以上的树脂层来说,优选:至少具有第1树脂层和第2树脂层,上述第1树脂层所含的聚乙烯醇缩醛(以下,称为聚乙烯醇缩醛A)的羟基量与上述第2树脂层所含的聚乙烯醇缩醛(以下,称为聚乙烯醇缩醛B)的羟基量不同。
由于聚乙烯醇缩醛A与聚乙烯醇缩醛B的性质不同,因此能够提供具有仅1层难以实现的各种性能的夹层玻璃用中间膜。例如,在2层上述第2树脂层之间层叠上述第1树脂层并且聚乙烯醇缩醛A的羟基量低于聚乙烯醇缩醛B的羟基量的情况下,上述第1树脂层与上述第2树脂层相比具有玻璃化转变温度降低的倾向。其结果是,上述第1树脂层比上述第2树脂层更软,夹层玻璃用中间膜的隔音性提高。另外,在2层上述第2树脂层之间层叠上述第1树脂层并且聚乙烯醇缩醛A的羟基量高于聚乙烯醇缩醛B的羟基量的情况下,上述第1树脂层与上述第2树脂层相比具有玻璃化转变温度变高的倾向。其结果是,上述第1树脂层比上述第2树脂层更硬,夹层玻璃用中间膜的耐贯通性提高。
进而,在上述第1树脂层和上述第2树脂层包含增塑剂的情况下,优选上述第1树脂层中的相对于聚乙烯醇缩醛100质量份的增塑剂的含量(以下,称为含量A)与上述第2树脂层中的相对于聚乙烯醇缩醛100质量份的增塑剂的含量(以下,称为含量B)不同。例如,在2层上述第2树脂层之间层叠上述第1树脂层并且上述含量A比上述含量B多的情况下,上述第1树脂层与上述第2树脂层相比具有玻璃化转变温度变低的倾向。其结果是,上述第1树脂层比上述第2树脂层更软,夹层玻璃用中间膜的隔音性提高。另外,在2层上述第2树脂层之间层叠上述第1树脂层并且上述含量A比上述含量B少的情况下,上述第1树脂层与上述第2树脂层相比具有玻璃化转变温度变高的倾向。其结果是,上述第1树脂层比上述第2树脂层更硬,夹层玻璃用中间膜的耐贯通性提高。
作为构成本发明的夹层玻璃用中间膜的2层以上的树脂层的组合,例如为了提高夹层玻璃的隔音性,可举出作为上述第1树脂层的隔音层与作为上述第2树脂层的保护层的组合。从夹层玻璃的隔音性提高的方面出发,优选:上述隔音层包含聚乙烯醇缩醛X和增塑剂,上述保护层包含聚乙烯醇缩醛Y和增塑剂。进而,在2层上述保护层之间层叠上述隔音层的情况下,能够得到具有优异的隔音性的夹层玻璃用中间膜(以下,也称为隔音中间膜)。以下,对隔音中间膜进行更具体的说明。
在上述隔音中间膜中,上述隔音层具有赋予隔音性的作用。上述隔音层优选含有聚乙烯醇缩醛X和增塑剂。
上述聚乙烯醇缩醛X可以通过将聚乙烯醇用醛进行缩醛化来制备。上述聚乙烯醇通常通过使聚乙酸乙烯酯进行皂化而得到。
上述聚乙烯醇的平均聚合度的优选下限为200,优选上限为5000。通过将上述聚乙烯醇的平均聚合度设为200以上,能够提高所得的隔音中间膜的耐贯通性,通过设为5000以下,能够确保隔音层的成形性。上述聚乙烯醇的平均聚合度的更优选下限为500,更优选上限为4000。
需要说明的是,上述聚乙烯醇的平均聚合度通过根据JIS K6726“聚乙烯醇试验方法”的方法求出。
用于将上述聚乙烯醇进行缩醛化的醛的碳数的优选下限为4,优选上限为6。通过将醛的碳数设为4以上,能够稳定地含有充足量的增塑剂,能够发挥优异的隔音性能。另外,能够防止增塑剂的渗出。通过将醛的碳数设为6以下,能够易于进行聚乙烯醇缩醛X的合成,能够确保生产率。作为上述碳数为4~6的醛,可以为直链状的醛,也可以为支链状的醛,可举出例如正丁醛、正戊醛等。
上述聚乙烯醇缩醛X的羟基量的优选上限为30摩尔%。通过将上述聚乙烯醇缩醛X的羟基量设为30摩尔%以下,能够含有发挥隔音性所必需量的增塑剂,能够防止增塑剂的渗出。上述聚乙烯醇缩醛X的羟基量的更优选的上限为28摩尔%、进一步优选的上限为26摩尔%、特别优选的上限为24摩尔%,优选的下限为10摩尔%、更优选的下限为15摩尔%、进一步优选的下限为20摩尔%。上述聚乙烯醇缩醛X的羟基量是将羟基所键合的乙烯基量除以主链的全部乙烯基量而求出的摩尔分率用百分率(摩尔%)表示的值。上述羟基所键合的乙烯基量例如能够通过根据JIS K6728“聚乙烯醇缩丁醛试验方法”的方法,通过测定上述聚乙烯醇缩醛X的羟基所键合的乙烯基量而求出。
上述聚乙烯醇缩醛X的缩醛基量的优选下限为60摩尔%,优选上限为85摩尔%。通过将上述聚乙烯醇缩醛X的缩醛基量设为60摩尔%以上,能够提高隔音层的疏水性,含有发挥隔音性所必需量的增塑剂,能够防止增塑剂的渗出或白化。通过将上述聚乙烯醇缩醛X的缩醛基量设为85摩尔%以下,能够易于进行聚乙烯醇缩醛X的合成,确保生产率。上述聚乙烯醇缩醛X的缩醛基量的下限更优选为65摩尔%,进一步优选为68摩尔%以上。
上述缩醛基量能够通过根据JIS K6728“聚乙烯醇缩丁醛试验方法”的方法,通过测定上述聚乙烯醇缩醛X的缩醛基所键合的乙烯基量而求出。
上述聚乙烯醇缩醛X的乙酰基量的优选下限为0.1摩尔%,优选上限为30摩尔%。通过将上述聚乙烯醇缩醛X的乙酰基量设为0.1摩尔%以上,能够含有发挥隔音性所必需量的增塑剂,能够防止渗出。另外,通过将上述聚乙烯醇缩醛X的乙酰基量设为30摩尔%以下,能够提高隔音层的疏水性,防止白化。上述乙酰基量的更优选的下限为1摩尔%、进一步优选的下限为5摩尔%、特别优选的下限为8摩尔%,更优选的上限为25摩尔%、进一步优选的上限为20摩尔%。上述乙酰基量是将从主链的全部乙烯基量中减去缩醛基所键合的乙烯基量和羟基所键合的乙烯基量而得的值除以主链的全部乙烯基量而求出的摩尔分率用百分率(摩尔%)表示的值。
特别是,从能够使上述隔音层容易地含有发挥隔音性所必需量的增塑剂的方面出发,上述聚乙烯醇缩醛X优选为上述乙酰基量为8摩尔%以上的聚乙烯醇缩醛、或上述乙酰基量小于8摩尔%且缩醛基量为65摩尔%以上的聚乙烯醇缩醛。另外,上述聚乙烯醇缩醛X更优选为上述乙酰基量为8摩尔%以上的聚乙烯醇缩醛、或上述乙酰基量小于8摩尔%且缩醛基量为68摩尔%以上的聚乙烯醇缩醛。
对于上述隔音层中的增塑剂的含量,相对于上述聚乙烯醇缩醛X100质量份的优选下限为45质量份、优选上限为80质量份。通过将上述增塑剂的含量设为45质量份以上,能够发挥高的隔音性,通过设为80质量份以下,能够防止发生增塑剂的渗出,从而防止夹层玻璃用中间膜的透明性或粘接性的下降。上述增塑剂的含量的更优选的下限为50质量份、进一步优选的下限为55质量份,更优选的上限为75质量份、进一步优选的上限为70质量份。
上述隔音层的厚度的优选下限为50μm。通过将上述隔音层的厚度设为50μm以上,能够发挥充分的隔音性。上述隔音层的厚度的更优选的下限为80μm。需要说明的是,上限没有特别限定,考虑到作为夹层玻璃用中间膜的厚度,优选的上限为300μm。
上述隔音层可以具有下述形状:具有一端和在上述一端的相反侧的另一端,上述另一端的厚度大于上述一端的厚度。上述隔音层优选具有厚度方向的截面形状为楔形的部分。这种情况下,上述隔音层的最小厚度的优选下限为50μm。通过将上述隔音层的最小厚度设为50μm以上,能够发挥充分的隔音性。上述隔音层的最小厚度的更优选的下限为80μm,进一步优选的下限为100μm。需要说明的是,上述隔音层的最大厚度的上限没有特别限定,考虑到作为夹层玻璃用中间膜的厚度,优选的上限为300μm。上述隔音层的最大厚度的更优选的上限为220μm。
上述保护层具有以下作用:防止隔音层所含的大量的增塑剂渗出而使夹层玻璃用中间膜与玻璃的粘接性降低,另外,对夹层玻璃用中间膜赋予耐贯通性。
上述保护层例如优选含有聚乙烯醇缩醛Y和增塑剂,更优选含有羟基量比聚乙烯醇缩醛X更大的聚乙烯醇缩醛Y和增塑剂。
上述聚乙烯醇缩醛Y可以通过将聚乙烯醇用醛进行缩醛化来制备。上述聚乙烯醇通常通过将聚乙酸乙烯酯进行皂化而得到。
另外,上述聚乙烯醇的平均聚合度的优选下限为200,优选上限为5000。通过将上述聚乙烯醇的平均聚合度设为200以上,能够提高夹层玻璃用中间膜的耐贯通性,通过设为5000以下,能够确保保护层的成形性。上述聚乙烯醇的平均聚合度的更优选的下限为500,更优选的上限为4000。
用于将上述聚乙烯醇进行缩醛化的醛的碳数的优选下限为3,优选上限为4。通过将醛的碳数设为3以上,夹层玻璃用中间膜的耐贯通性提高。通过将醛的碳数设为4以下,聚乙烯醇缩醛Y的生产率提高。
作为上述碳数为3~4的醛,可以为直链状的醛,也可以为支链状的醛,可举出例如正丁醛等。
上述聚乙烯醇缩醛Y的羟基量的优选上限为33摩尔%,优选下限为28摩尔%。通过将上述聚乙烯醇缩醛Y的羟基量设为33摩尔%以下,能够防止夹层玻璃用中间膜的白化。通过将上述聚乙烯醇缩醛Y的羟基量设为28摩尔%以上,夹层玻璃用中间膜的耐贯通性提高。
上述聚乙烯醇缩醛Y的缩醛基量的优选下限为60摩尔%,优选上限为80摩尔%。通过将上述缩醛基量设为60摩尔%以上,能够含有发挥充分的耐贯通性所必需量的增塑剂。通过将上述缩醛基量设为80摩尔%以下,能够确保上述保护层与玻璃的粘接力。上述缩醛基量的更优选的下限为65摩尔%,更优选的上限为69摩尔%。
上述聚乙烯醇缩醛Y的乙酰基量的优选上限为7摩尔%。通过将上述聚乙烯醇缩醛Y的乙酰基量设为7摩尔%以下,能够提高保护层的疏水性,防止白化。上述乙酰基量的更优选的上限为2摩尔%,优选的下限为0.1摩尔%。需要说明的是,聚乙烯醇缩醛A、B、和Y的羟基量、缩醛基量和乙酰基量能够利用与聚乙烯醇缩醛X相同的方法测定。
对于上述保护层中的增塑剂的含量,相对于上述聚乙烯醇缩醛Y100质量份的优选下限为20质量份,优选上限为45质量份。通过将上述增塑剂的含量设为20质量份以上,能够确保耐贯通性,通过设为45质量份以下,能够防止增塑剂的渗出,防止夹层玻璃用中间膜的透明性、粘接性的降低。上述增塑剂的含量的更优选的下限为30质量份、进一步优选的下限为35质量份,更优选的上限为43质量份、进一步优选的上限为41质量份。从夹层玻璃的隔音性进一步提高的方面出发,优选上述保护层中的增塑剂的含量小于上述隔音层中的增塑剂的含量。
从夹层玻璃的隔音性进一步提高的方面出发,优选聚乙烯醇缩醛Y的羟基量大于聚乙烯醇缩醛X的羟基量,更优选大1摩尔%以上,进一步优选大5摩尔%以上,特别优选大8摩尔%以上。通过调节聚乙烯醇缩醛X和聚乙烯醇缩醛Y的羟基量,能够控制上述隔音层和上述保护层中的增塑剂的含量,上述隔音层的玻璃化转变温度降低。其结果是,夹层玻璃的隔音性进一步提高。
另外,从夹层玻璃的隔音性进一步提高的方面出发,优选上述隔音层中的相对于聚乙烯醇缩醛X100质量份的增塑剂的含量(以下,也称为含量X)大于上述保护层中的相对于聚乙烯醇缩醛Y100质量份的增塑剂的含量(以下,也称为含量Y),更优选大5质量份以上,进一步优选大15质量份以上,特别优选大20质量份以上。通过调节含量X和含量Y,上述隔音层的玻璃化转变温度降低。其结果是,夹层玻璃的隔音性进一步提高。
本发明的夹层玻璃用中间膜可以具有一端和在上述一端的相反侧的另一端。上述一端和上述另一端是中间膜中彼此相对的两侧的端部。在本发明的夹层玻璃用中间膜中,优选上述另一端的厚度大于上述一端的厚度。通过具有这种一端与另一端的厚度不同的形状,能够将使用本发明的夹层玻璃用中间膜的夹层玻璃作为平视显示器合适地使用,此时,能够有效地抑制平视显示器的重影的发生。本发明的夹层玻璃用中间膜的截面形状可以为楔形。若夹层玻璃用中间膜的截面形状为楔形,则通过对应于夹层玻璃的安装角度来调节楔形的楔角θ,从而能够在平视显示器中实现防止重影的发生的图像显示。从进一步抑制重影的观点出发,上述楔角θ的优选的下限为0.1mrad、更优选的下限为0.2mrad、进一步优选的下限为0.3mrad,优选的上限为1mrad、更优选的上限为0.9mrad。需要说明的是,在例如通过使用挤出机对树脂组合物进行挤出成形的方法来制造截面形状为楔形的夹层玻璃用中间膜的情况下,有时成为以下形状:在自较薄一侧的一个端部起略微朝向内侧的区域(具体而言,将一端与另一端之间的距离记作X时,自较薄一侧的一端起朝向内侧为0X~0.2X的距离的区域)内具有最小厚度,并且,在自较厚一侧的一个端部起略微朝向内侧的区域(具体而言,将一端与另一端之间的距离记作X时,自较厚一侧的一端起朝向内侧为0X~0.2X的距离的区域)内具有最大厚度的形状。本说明书中,这种形状也包含在楔形内。
本发明的夹层玻璃用中间膜的截面形状为楔形的情况下,也可以制成具有包含隔音层和保护层的多层结构的膜。通过将上述隔音层的厚度设为一定范围并且层叠上述保护层,从而能够以夹层玻璃用中间膜整体的截面形状成为呈一定的楔角的楔形的方式进行调整。
上述保护层的厚度只要调节至能够实现上述保护层的作用的范围即可,没有特别限定。然而,在上述保护层上具有凹凸的情况下,为了能够抑制凹凸转印至与直接接触的上述隔音层的界面,优选在可能的范围内增厚。具体而言,上述保护层的厚度的优选的下限为100μm,更优选的下限为300μm,进一步优选的下限为400μm,特别优选的下限为450μm。对上述保护层的厚度的上限没有特别限定,为了确保隔音层的厚度为能够达到充分的隔音性的程度,实质上500μm左右为上限。
上述保护层可以具有下述形状:具有一端和在上述一端的相反侧的另一端且上述另一端的厚度大于上述一端的厚度。上述保护层优选具有厚度方向的截面形状为楔形的部分。上述保护层的厚度只要调节至能够实现上述保护层的作用的范围即可,没有特别限定。然而,在上述保护层上具有凹凸的情况下,为了能够抑制凹凸转印至与直接接触的上述隔音层的界面,优选在可能的范围内增厚。具体而言,上述保护层的最小厚度的优选的下限为100μm,更优选的下限为300μm,进一步优选的下限为400μm,特别优选的下限为450μm。对上述保护层的最大厚度的上限没有特别限定,为了确保隔音层的厚度为能够达到充分的隔音性的程度,实质上1000μm左右为上限,优选为800μm。
作为制造上述隔音中间膜的方法,没有特别限定,可举出例如将上述隔音层和保护层通过挤出法、压延法、压制法等通常的制膜法制成片状膜后进行层叠的方法等。
包含一对玻璃板和层叠于该一对玻璃板之间的本发明的夹层玻璃用中间膜的夹层玻璃也是本发明之一。
上述玻璃板可以使用通常使用的透明板玻璃。可列举出例如浮法板玻璃、抛光板玻璃、模塑板玻璃、丝网玻璃、夹丝板玻璃、着色的板玻璃、热射线吸收玻璃、热射线反射玻璃、生玻璃等无机玻璃。此外,也可以使用在玻璃表面具有紫外线遮蔽涂层的紫外线遮蔽玻璃。进而,还可以使用聚对苯二甲酸乙二醇酯、聚碳酸酯、聚丙烯酸酯等有机塑料板。
作为上述玻璃板,可以使用两种以上的玻璃板。可列举出例如:在透明浮法板玻璃与生玻璃之类的着色玻璃板之间层叠有本发明的夹层玻璃用中间膜而得到的夹层玻璃。此外,作为上述玻璃板,也可以使用两种以上的厚度不同的玻璃板。
发明效果
根据本发明,能够提供能够得到光学变形的发生得以抑制的夹层玻璃的夹层玻璃用中间膜、该夹层玻璃用中间膜的制造方法、以及使用该夹层玻璃用中间膜而成的夹层玻璃。
附图说明
图1是说明式(1)中的“(Ry×Sm)/2”的含义的示意图。
图2是表示在表面上底部连续的沟形状的凹部等间隔并且相邻的凹部平行地排列的夹层玻璃用中间膜的一例的示意图。
图3是表示在表面上底部连续的沟形状的凹部等间隔并且相邻的凹部平行地排列的夹层玻璃用中间膜的一例的示意图。
图4是表示在表面上底部连续的沟形状的凹部不为等间隔并且相邻的凹部平行地排列的夹层玻璃用中间膜的一例的示意图。
图5是表示表面具有块状形状的夹层玻璃用中间膜的一例的示意图。
图6是表示表面具有球状形状的夹层玻璃用中间膜的一例的示意图。
具体实施方式
以下列举实施例对本发明的方案进行更详细的说明,但本发明不仅限定于这些实施例。
(实施例1)
(1)保护层用树脂组合物的制备
相对于将平均聚合度为1700的聚乙烯醇用正丁醛进行缩醛化而得的聚乙烯醇缩丁醛(乙酰基量1摩尔%、缩丁醛基量69摩尔%、羟基量30摩尔%)100质量份,添加作为增塑剂的三乙二醇-二-2-乙基己酸酯(3GO)40质量份,用混合辊充分混炼,得到保护层用树脂组合物。
(2)隔音层用树脂组合物的制备
相对于将平均聚合度为2300的聚乙烯醇用正丁醛进行缩醛化而得的聚乙烯醇缩丁醛(乙酰基量12.5摩尔%、缩丁醛基量64.5摩尔%、羟基量23.0摩尔%)100质量份,添加作为增塑剂的三乙二醇-二-2-乙基己酸酯(3GO)60质量份,用混合辊充分混炼,得到隔音层用树脂组合物。
(3)夹层玻璃用中间膜的制作
将所得的保护层用树脂组合物和隔音层用树脂组合物用共挤出机进行共挤出,由此得到依次层叠有由保护层用树脂组合物构成的厚度350μm的第1表面层(保护层)、由隔音层用树脂组合物构成的厚度100μm的中间层(隔音层)和由保护层用树脂组合物构成的厚度350μm的第2表面层(保护层)的3层结构的层叠体。通过将共挤出时的条件设定为以下条件,从而通过利用熔体破裂的挤压唇压花法而将夹层玻璃用中间膜成膜,与此同时赋予凹凸。
即,在利用熔体破裂的挤压唇压花法中,在将模具入口的树脂压力设为70kgf/cm2、模具入口的树脂组合物的温度设为200℃、模具的温度设为210℃、模具出口的宽度设为1000mm、每模具出口的宽度的挤出量设为300kg/hr·m、刚从模具出口排出后的膜表面温度设为200℃、从模具出口至冷却水槽的距离设为170mm、冷却水槽内的水温设为10~20℃的条件下,在将夹层玻璃用中间膜成膜,与此同时,在其两面赋予凹凸形状。
所得的夹层玻璃用中间膜的厚度为800μm。
(4)表面的凹凸的测定
(4-1)Ry值的测定
通过根据JIS B 0601(1994)的方法,测定所得的夹层玻璃用中间膜的两面的最大高度(Ry)。使用小坂研究所公司制“Surfcorder SE300”作为测定机,在将测定时的触针计条件设为截止值=2.5mm、基准长度=2.5mm、评价长度=12.5mm、触针的前端半径=2μm、前端角度=60°、测定速度=0.5mm/s的条件下进行测定。测定时的环境为23℃和30RH%下。移动触针的方向设为相对于片材的流动方向的平行方向,在宽度方向上以3mm间隔移动5次,算出由此测定的各个值的平均值而作为Ry的值。需要说明的是,所得的Ry的值在两面均相同。
(4-2)Sm值的测定
通过根据JIS B 0601(1994)的方法,测定所得的夹层玻璃用中间膜的两面的凸凹的平均间隔(Sm)。使用小坂研究所公司制“Surfcorder SE300”作为测定机,在将测定时的触针计条件设为截止值=2.5mm、基准长度=2.5mm、评价长度=12.5mm、触针的前端半径=2μm、前端角度=60°、测定速度=0.5mm/s的条件下进行测定。测定时的环境为23℃和30RH%下。移动触针的方向设为相对于片材的流动方向的平行方向,在宽度方向上以3mm间隔移动5次,算出由此测定的各个值的平均值而作为Sm的值。
需要说明的是,所得的Sm的值在两面上相同。
(5)收缩率的测定
将夹层玻璃用中间膜切割为15cm×10cm的长条状来得到测定样品。此时,使流动方向为长边。浸渍于50℃的温水中10分钟后,擦拭表面的水分,冷却至23℃。然后,对测定样品的流动方向的长度进行测定,根据以下式算出流动方向的收缩率。
收缩率(%)={1-(浸渍后的流动方向的长度)/(浸渍前的流动方向的长度)}×100
(实施例2~8、比较例1~4)
除了变更基于利用熔体破裂的挤压唇压花法的、赋予凹凸的条件以外,与实施例1同样地制造夹层玻璃用中间膜,进行其表面凹凸的测定和收缩率的测定。具体而言,调节模具入口的树脂压力、模具入口的树脂组合物的温度、模具的温度、每模具出口的宽度的挤出量、刚从模具出口排出后的膜表面温度、从模具出口至冷却水槽的距离、冷却水槽内的水温。
(评价)
将在实施例和比较例中得到的夹层玻璃用中间膜以纵向(流动方向)15cm、横向30cm的大小进行切割。接下来,将所切割的夹层玻璃用中间膜用两张透明浮法玻璃(纵15cm×横30cm、厚2.5mm)夹持,在240℃进行3分钟的预压制处理,由此进行预压接工序。然后,使用高压釜在135℃、压力1.2MPa的条件下进行20分钟压接,由此进行正式压接工序,得到夹层玻璃。
对所得的夹层玻璃照射从光源(卤素灯)透过狭缝的光,由传感器(相机)接收在屏幕上显示的投影变形,用计算机进行数据处理,作为光学变形值。可以说光学变形值越高,则光学变形(图像的变形)越大。
以下对光学变形值的测定方法的详细情况进行描述。使用日本特开平7-306152号公报所记载的装置、即具有:向具有透光性的被检查物照射照明光的光源单元、狭缝、将透过被检查物的该照明光进行投影的投影面、拍摄投影面来生成灰白图像的图像输入部、以及基于由图像输入部获得的灰白图像的灰白水平的偏差程度来判定有无变形的图像处理部的光学变形检测装置来测定光学变形值。具体而言,使用岩崎电气公司制的EYE DICHO-COOL HALOGEN(15V100W)作为光源,以使由基于JIS R 3211(1988)的可见光透射率(A光Y值、A-Y(380~780nm))为88%(使用Hitachi High-Tech Technology Co.,Ltd.制、“U4100”)的单层膜构成的夹层玻璃的光学变形值为1.14,无玻璃的状态的光学变形值为1.30的方式调节光源的照度、投影光学变形图像的屏幕的角度、相机的角度来评价光学变形值。光学变形的评价在夹层玻璃温度为25℃的条件下进行。作为光学变形值,虽然可算出纵和横的值,但采用数值低者。需要说明的是,使用接触式温度计作为温度计。测定结果示于表1和表2。
需要说明的是,若光学变形值为1.24以下,则在将夹层玻璃作为车辆用挡风玻璃使用时,不会发生信号、人行横道的闪变。
[表1]
[表2]
产业上的可利用性
根据本发明,可提供能够得到光学变形的发生得到了抑制的夹层玻璃的夹层玻璃用中间膜、该夹层玻璃用中间膜的制造方法、以及使用该夹层玻璃用中间膜而成的夹层玻璃。
符号说明
1 夹层玻璃用中间膜的表面的凹凸
11 凸部
12 凹部
21 任意选择的一个凹部
22 与任意选择的一个凹部相邻的凹部
23 与任意选择的一个凹部相邻的凹部
A 凹部21与凹部22的间隔
B 凹部21与凹部23的间隔
Claims (6)
1.一种夹层玻璃用中间膜,其特征在于,是通过利用熔体破裂的挤压唇压花法制造的、由层叠有2层以上树脂层的层叠体构成且在至少一个表面具有多个凹凸的夹层玻璃用中间膜,其中,
在所述具有凹凸的表面,根据JIS B 0601(1994)测定的最大高度Ry与所述凹凸的平均间隔Sm满足下述式(1),其中,Ry与Sm的单位均为μm,
(Ry×Sm)/2≤3500 (1)。
2.根据权利要求1所述的夹层玻璃用中间膜,其特征在于,在具有凹凸的表面,根据JISB 0601(1994)测定的最大高度Ry与凹凸的平均间隔Sm满足下述式(2),其中,Ry与Sm的单位均为μm,
(Ry×Sm)/2≤2700 (2)。
3.根据权利要求1或2所述的夹层玻璃用中间膜,其特征在于,将夹层玻璃用中间膜浸渍于50℃的温水中10分钟后的流动方向的收缩率为4%以下。
4.根据权利要求1、2或3所述的夹层玻璃用中间膜,其特征在于,在至少一个表面包含具有底部连续的沟形状的多个凹部。
5.一种夹层玻璃,其特征在于,包含:一对玻璃板、和层叠于该一对玻璃板之间的权利要求1、2、3或4所述的夹层玻璃用中间膜。
6.一种夹层玻璃用中间膜的制造方法,其特征在于,是制造权利要求1、2、3或4所述的夹层玻璃用中间膜的方法,
所述制造方法包括通过利用熔体破裂的挤压唇压花法对夹层玻璃用中间膜的至少一个表面赋予多个凹凸的工序,
在该工序中,在使用共挤出机对各树脂进行共挤出时,设为以下条件;
将模具入口的树脂压力设为40~150kgf/cm2,将树脂的温度设为160~250℃,将模具的温度设为100~270℃,将模具出口的宽度设为700~3500mm,将每模具出口的宽度的挤出量设为130~1700kg/hr·m,将刚从模具出口排出后的膜表面温度设为170~250℃,将从模具出口至冷却水槽的距离设为10~400mm,冷却水槽内的水温设为10~70℃。
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