CN116254064A - Polymer film - Google Patents

Polymer film Download PDF

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CN116254064A
CN116254064A CN202111505156.1A CN202111505156A CN116254064A CN 116254064 A CN116254064 A CN 116254064A CN 202111505156 A CN202111505156 A CN 202111505156A CN 116254064 A CN116254064 A CN 116254064A
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polymer film
mol
acetal resin
polyvinyl acetal
layer
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黄子荣
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Chang Chun Petrochemical Co Ltd
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Chang Chun Petrochemical Co Ltd
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Priority to US17/853,604 priority patent/US20230182449A1/en
Priority to JP2022187685A priority patent/JP7522171B2/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/10Adhesives in the form of films or foils without carriers
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J129/00Adhesives 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
    • C09J129/14Homopolymers or copolymers of acetals or ketals obtained by polymerisation of unsaturated acetals or ketals or by after-treatment of polymers of unsaturated alcohols
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/30Adhesives in the form of films or foils characterised by the adhesive composition
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00Additional features of adhesives in the form of films or foils
    • C09J2301/20Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive itself
    • C09J2301/208Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive itself the adhesive layer being constituted by at least two or more adjacent or superposed adhesive layers, e.g. multilayer adhesive

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Abstract

本发明涉及一种聚合物膜,其包含聚乙烯醇缩醛树脂及可塑剂;其中,该聚合物膜为一层或多层,且该聚合物膜的损耗因子最低值出现的温度为40℃至60℃。本发明所提供的聚合物膜具有良好的流动性及加工性。

Figure 202111505156

The present invention relates to a polymer film, which comprises polyvinyl acetal resin and a plasticizer; wherein, the polymer film is one or more layers, and the temperature at which the minimum value of the loss factor of the polymer film appears is 40°C to 60°C. The polymer film provided by the invention has good fluidity and processability.

Figure 202111505156

Description

聚合物膜polymer film

【技术领域】【Technical field】

本发明主要关于一种聚合物膜体;本发明尤其是关于一种适用于夹层玻璃的中间膜的聚合物膜。The present invention mainly relates to a polymer film body; in particular, the present invention relates to a polymer film suitable for an interlayer film of laminated glass.

【背景技术】【Background technique】

聚合物膜在现今社会中的应用相当广泛,且其制成材料相当多元,聚合物膜具有良好的造膜性,依原料或制程调整可具有高透明性、弹性、韧性、耐强碱、耐油性、可挠性、耐候性与低温耐冲击性等优越的特性。聚合物膜常见的材料如聚乙烯醇缩醛树脂,其具有特殊的化学结构,故其对玻璃、金属、陶瓷粉、塑料、皮革及木材等都有优良的接着性;除此之外,聚乙烯醇缩醛树脂对颜料与染料有良好的分散性,与多种树脂亦具有优异的兼容性。Polymer films are widely used in today's society, and their materials are quite diverse. Polymer films have good film-forming properties, and can be adjusted according to raw materials or manufacturing processes to have high transparency, elasticity, toughness, strong alkali resistance, and oil resistance. Excellent properties such as flexibility, flexibility, weather resistance and low temperature impact resistance. Polyvinyl acetal resin, a common material for polymer film, has a special chemical structure, so it has excellent adhesion to glass, metal, ceramic powder, plastic, leather and wood; in addition, polyvinyl acetal resin Vinyl acetal resin has good dispersibility for pigments and dyes, and has excellent compatibility with various resins.

在应用层面上,聚乙烯醇缩醛树脂所制成的聚合物膜可以是单层膜、多层膜或是夹设于玻璃间的中间膜等多种形式存在。然而在制成终端产品之前,聚乙烯醇缩醛树脂膜片需要经过不少的加工步骤,例如展膜或裁切等涉及形变的过程。据此,聚乙烯醇缩醛树脂膜片是否具备优异的加工性变成为一项重要的指标。At the application level, the polymer film made of polyvinyl acetal resin can exist in various forms such as a single-layer film, a multi-layer film, or an interlayer film sandwiched between glasses. However, before being made into a final product, polyvinyl acetal resin films need to go through a lot of processing steps, such as stretching or cutting and other processes involving deformation. Accordingly, whether the polyvinyl acetal resin film has excellent processability becomes an important index.

具体而言,聚合物的加工性与其黏弹性质具高度关联性;而所谓黏弹性质是指材料在发生形变时,可逆及不可逆的形变模量。进一步地,与黏弹性质相关的参数包括损耗因子(tanδ)值以及与其对应的玻璃转移温度(glass transition temperature,Tg),所谓tanδ又称指损耗因子、阻尼因子或损耗角正切,用以表达材料黏弹性质中的阻尼特性,并且可对等为材料的损耗模量(loss modulus,G”)与储存模量(storage modulus,G’)的比值;相对地,所述损耗因子对应温度的波峰值即为玻璃转移温度,其可视为物质在玻璃态(系指材料处于流动性低的状态)以及高弹性态(系指材料处于流动性高且柔软的状态)之间可逆转化的温度。Specifically, the processability of a polymer is highly correlated with its viscoelastic properties; the so-called viscoelastic properties refer to the reversible and irreversible modulus of deformation when a material is deformed. Further, the parameters related to viscoelastic properties include loss factor (tanδ) value and corresponding glass transition temperature (glass transition temperature, Tg). The so-called tanδ also refers to loss factor, damping factor or loss tangent, which is used to express The damping characteristic in the viscoelastic properties of a material, and can be equivalent to the ratio of the loss modulus (loss modulus, G") of the material to the storage modulus (storage modulus, G'); relatively, the loss factor corresponds to the temperature The peak value of the wave is the glass transition temperature, which can be regarded as the temperature at which a substance can reversibly change between the glass state (meaning that the material is in a state of low fluidity) and the high elastic state (meaning that the material is in a state of high fluidity and softness) .

【发明内容】【Content of invention】

发明内容旨在提供本发明的简化摘要,以令阅读者对本发明具备基本的理解。此发明内容并非本发明的完整概述,且其用意并非指出本发明实施例的重要或关键组件或界定本发明的范围。The Summary of the Invention is intended to provide a simplified summary of the invention to enable readers to have a basic understanding of the invention. This summary is not an extensive overview of the invention, and it is not intended to identify key or critical elements of the embodiments of the invention or to delineate the scope of the invention.

本发明人发现,聚合物膜于其加工时的温度条件下所展现的黏弹性质与其加工性具有更进一步的关联性,且应能透过调控所述温度条件下的黏弹性质而获得具备较佳加工性的聚合物膜。作为夹层玻璃用中间膜,聚乙烯醇缩醛薄膜会经过展膜的过程,此过程会将膜进行拉伸成为所要的形状。若薄膜太硬,则会因为较难拉伸使得后端展膜不易;太软则会在展膜过程中造成纹路溃散,因此,薄膜在40至60℃时的黏弹性质便是加工是否顺畅的关键。据此,本发明藉由界定聚合物膜产生损耗因子(tanδ)最低值的温度范围而改良其流动性及加工性。The present inventors have found that the viscoelastic properties exhibited by the polymer film under the temperature conditions during its processing have a further correlation with its processability, and should be able to be obtained by controlling the viscoelastic properties under the temperature conditions. Polymer film with better processability. As an interlayer film for laminated glass, polyvinyl acetal film will go through the process of film stretching, which will stretch the film into the desired shape. If the film is too hard, it will be difficult to stretch the film at the rear end because it is difficult to stretch; if it is too soft, the texture will collapse during the film stretching process. Therefore, the viscoelastic properties of the film at 40 to 60°C are the key to whether the processing is smooth key. Accordingly, the present invention improves the flowability and processability of polymer films by defining the temperature range in which their loss tangent (tan δ) minima occurs.

具体而言,本发明一方面提供一种聚合物膜,其包含聚乙烯醇缩醛树脂及可塑剂,且该聚合物膜为一层或多层,该聚合物膜的损耗因子最低值出现的温度为40℃至60℃。Specifically, the present invention provides a polymer film, which includes polyvinyl acetal resin and a plasticizer, and the polymer film is one or more layers, and the minimum value of the loss factor of the polymer film appears The temperature is 40°C to 60°C.

根据本发明的一实施例,该损耗因子最低值为0.13至0.19。According to an embodiment of the present invention, the minimum value of the loss factor is 0.13 to 0.19.

根据本发明的一实施例,于一层的情况时,该损耗因子最低值出现的温度大于其玻璃转移温度;或于多层的情况时,该损耗因子最低值出现的温度大于其最大玻璃转移温度。According to an embodiment of the present invention, in the case of one layer, the temperature at which the minimum value of the loss factor occurs is greater than its glass transition temperature; or in the case of multiple layers, the temperature at which the minimum value of the loss factor occurs is greater than its maximum glass transition temperature temperature.

根据本发明的一实施例,该聚乙烯醇缩醛树脂为聚乙烯醇缩丁醛 (PolyvinylButyral,PVB)。According to an embodiment of the present invention, the polyvinyl acetal resin is polyvinyl butyral (PolyvinylButyral, PVB).

根据本发明的一实施例,该聚合物膜的厚度为0.2mm至2mm。According to an embodiment of the present invention, the polymer film has a thickness of 0.2 mm to 2 mm.

根据本发明的一实施例,该聚合物膜于50℃热处理1小时下的热收缩率(%)((加热前长度-加热后长度)/加热前长度X100)为2%至5%。According to an embodiment of the present invention, the thermal shrinkage (%) ((length before heating−length after heating)/length before heating×100) of the polymer film after heat treatment at 50° C. for 1 hour is 2% to 5%.

根据本发明的一实施例,该聚合物膜依据ASTM D412量测的伸长率为220%至300%。According to an embodiment of the present invention, the elongation of the polymer film measured according to ASTM D412 is 220% to 300%.

根据本发明的一实施例,于一层的情况时,该聚合物膜的该聚乙烯醇缩醛树脂的羟基含量比为27mol%至31mol%,及/或该聚乙烯醇缩醛树脂的缩醛度为68mol%至72mol%。According to an embodiment of the present invention, in the case of one layer, the hydroxyl content ratio of the polyvinyl acetal resin of the polymer film is 27mol% to 31mol%, and/or the polyvinyl acetal resin The degree of aldehyde is 68 mol% to 72 mol%.

根据本发明的一实施例,于一层的情况时,其中该聚合物膜的该聚乙烯醇缩醛树脂以100重量份计,该可塑剂为30至60重量份。According to an embodiment of the present invention, in the case of one layer, wherein the polyvinyl acetal resin of the polymer film is 100 parts by weight, the plasticizer is 30 to 60 parts by weight.

根据本发明的一实施例,于一层的情况时,该聚合物膜系为平视显示器用(head-up display,HUD,抬头显示器)膜。According to an embodiment of the present invention, in the case of one layer, the polymer film is a head-up display (HUD, head-up display) film.

根据本发明的一实施例,该聚合物膜具一厚端,及一厚度较该厚端为薄的薄端。According to an embodiment of the present invention, the polymer film has a thick end and a thin end that is thinner than the thick end.

根据本发明的一实施例,于多层的情况时,该聚合物膜系为三层结构,上下两层为保护层并夹一中间层。According to an embodiment of the present invention, in the case of multiple layers, the polymer film has a three-layer structure, the upper and lower layers are protective layers and an intermediate layer is sandwiched.

根据本发明的一实施例,该保护层的该聚乙烯醇缩醛树脂,具有羟基含量比为27mol%至31mol%,及/或缩醛度为68mol%至72mol%。According to an embodiment of the present invention, the polyvinyl acetal resin of the protective layer has a hydroxyl content ratio of 27 mol% to 31 mol%, and/or an acetalization degree of 68 mol% to 72 mol%.

根据本发明的一实施例,该保护层的该聚乙烯醇缩醛树脂以100 重量份计,该可塑剂为30至60重量份。According to an embodiment of the present invention, based on 100 parts by weight of the polyvinyl acetal resin of the protective layer, the amount of the plasticizer is 30 to 60 parts by weight.

根据本发明的一实施例,该中间层的该聚乙烯醇缩醛树脂,具有羟基含量比为22mol%至27mol%,及/或缩醛度为62mol%至68mol%。According to an embodiment of the present invention, the polyvinyl acetal resin of the intermediate layer has a hydroxyl content ratio of 22 mol% to 27 mol%, and/or an acetalization degree of 62 mol% to 68 mol%.

根据本发明的一实施例,该中间层的该聚乙烯醇缩醛树脂以100 重量份计,该可塑剂为60至90重量份。According to an embodiment of the present invention, based on 100 parts by weight of the polyvinyl acetal resin of the middle layer, the amount of the plasticizer is 60 to 90 parts by weight.

根据本发明的一实施例,该聚合物膜系作为夹层玻璃用的中间膜,其厚度为0.5至2mm。According to an embodiment of the present invention, the polymer film is used as an interlayer film for laminated glass, and its thickness is 0.5 to 2 mm.

根据本发明的一实施例,该聚合物膜的厚度为0.8mm,且该保护层/中间层/保护层的厚度为0.335mm/0.13mm/0.335mm。According to an embodiment of the present invention, the thickness of the polymer film is 0.8mm, and the thickness of the protective layer/intermediate layer/protective layer is 0.335mm/0.13mm/0.335mm.

本发明所提供的的优势在于:本发明所提供的聚合物膜奠基于上述特征的界定,进而具备更优异的加工性以及流动性。The advantages provided by the present invention are: based on the definition of the above-mentioned features, the polymer film provided by the present invention has better processability and fluidity.

【附图说明】【Description of drawings】

为让本发明的上述与其他目的、特征、优点与实施例能更浅显易懂,所附图式的说明如下:In order to make the above and other objects, features, advantages and embodiments of the present invention more understandable, the accompanying drawings are described as follows:

图1至图3是依据本发明不同实施例所绘示的聚合物膜剖面图;1 to 3 are cross-sectional views of polymer films according to different embodiments of the present invention;

图4至图5是依据本发明不同实施例所绘示的聚合物膜制造流程图。FIG. 4 to FIG. 5 are flow charts illustrating the fabrication of polymer films according to different embodiments of the present invention.

根据惯常的作业方式,图中各种特征与组件并未依实际比例绘制,其绘制方式是为了以最佳的方式呈现与本发明相关的具体特征与组件。此外,在不同图式间,以相同或相似的组件符号指称相似的组件及部件。In accordance with common practice, the various features and components in the drawings are not drawn to scale, but are drawn in order to best represent the specific features and components relevant to the invention. In addition, the same or similar component symbols refer to similar components and components in different drawings.

【具体实施方式】【Detailed ways】

为了使本发明的叙述更加详尽与完备,下文针对了本发明的实施态样与具体实施例提出了说明性的描述,但这并非实施或运用本发明具体实施例的唯一形式。在本说明书及后附的申请专利范围中,除非上下文另外载明,否则“一”及“该”亦可解释为复数。此外,在本说明书及后附的申请专利范围中,除非另外载明,否则“设置于某物之上”可视为直接或间接以贴附或其他形式与某物的表面接触,该表面的界定应视说明书内容的前后/段落语意以及本说明所属领域的通常知识予以判断。In order to make the description of the present invention more detailed and complete, the following provides an illustrative description of the implementation and specific embodiments of the present invention, but this is not the only form for implementing or using the specific embodiments of the present invention. In this specification and the appended claims, unless the context specifies otherwise, "a" and "the" can also be interpreted as plural. In addition, in this specification and the scope of the appended patent application, unless otherwise specified, "set on something" can be regarded as directly or indirectly contacting the surface of something by sticking or other forms, and the surface of the The definition should be judged according to the context/paragraph semantics of the content of the description and the common knowledge in the field to which this description belongs.

虽然用以界定本发明的数值范围与参数皆是约略的数值,此处已尽可能精确地呈现具体实施例中的相关数值。然而,任何数值本质上不可避免地含有因个别测试方法所致的标准偏差。在此处,“约”通常系指实际数值在一特定数值或一范围的正负10%、5%、1%或0.5%之内。或者是,“约”一词代表实际数值落在平均值的可接受标准误差之内,是本发明所属领域中具有通常知识者的考虑而定。因此,除非另有相反的说明,本说明书与附随申请专利范围所揭示的数值参数皆为约略的数值,且可视需求而更动。至少应将这些数值参数理解为所指出的有效位数与套用一般进位法所得到的数值。Although the numerical ranges and parameters used to define the present invention are approximate numerical values, the relevant numerical values in the specific examples are presented here as precisely as possible. Any numerical value, however, inherently inherently contain standard deviations resulting from their individual testing methodology. As used herein, "about" generally means that the actual value is within plus or minus 10%, 5%, 1%, or 0.5% of a particular value or range. Alternatively, the term "about" means that the actual value falls within an acceptable standard error of the mean, as considered by one of ordinary skill in the art to which this invention pertains. Therefore, unless otherwise stated to the contrary, the numerical parameters disclosed in this specification and the appended patent claims are approximate values, and may be changed as required. At least these numerical parameters should be understood as the value obtained by applying the normal rounding method to the indicated effective digits.

本发明提供一种聚合物膜,其包含聚乙烯醇缩醛树脂及可塑剂。具体而言,本文所述的聚乙烯醇缩醛树脂是指聚乙烯醇与醛缩合而成的树脂组合物;其中,上述聚乙烯醇可藉由将聚乙烯酯皂化而得,而其聚乙烯醇的皂化度通常为70摩尔%至99.9摩尔%的范围内,例如:70摩尔%、75摩尔%、80摩尔%、 85摩尔%、90摩尔%、95摩尔%、99摩尔%或99.9摩尔%。上述醛通常可采用碳数为1至10的醛,例如:甲醛、乙醛、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、正癸醛及苯甲醛等;较佳地,所述醛为丙醛、正丁醛、异丁醛、正己醛或正戊醛;更佳为丙醛、正丁醛或异丁醛。根据本发明的一实施例,该聚乙烯醇缩醛为聚乙烯醇缩丁醛(Polyvinyl Butyral,PVB)。The invention provides a polymer film comprising polyvinyl acetal resin and a plasticizer. Specifically, the polyvinyl acetal resin described herein refers to a resin composition formed by condensation of polyvinyl alcohol and aldehyde; wherein, the above-mentioned polyvinyl alcohol can be obtained by saponifying polyvinyl ester, and its polyethylene The saponification degree of the alcohol is usually in the range of 70 mole % to 99.9 mole %, for example: 70 mole %, 75 mole %, 80 mole %, 85 mole %, 90 mole %, 95 mole %, 99 mole % or 99.9 mole % . The above-mentioned aldehydes usually can be aldehydes with a carbon number of 1 to 10, such as: formaldehyde, acetaldehyde, propionaldehyde, n-butyraldehyde, isobutyraldehyde, n-valeraldehyde, 2-ethylbutyraldehyde, n-hexanal, n-octylaldehyde, N-nonanal, n-decylaldehyde and benzaldehyde, etc.; preferably, the aldehyde is propionaldehyde, n-butyraldehyde, isobutyraldehyde, n-hexanal or n-valeraldehyde; more preferably propionaldehyde, n-butyraldehyde or isobutyraldehyde aldehyde. According to an embodiment of the present invention, the polyvinyl acetal is polyvinyl butyral (Polyvinyl Butyral, PVB).

另一方面,所述可塑剂又称塑化剂,其通常与聚乙烯醇缩醛树脂合并使用而影响材料的黏弹性质。具体而言,所述可塑剂非限制性地选自由一元酸酯、多元酸酯、有机磷酸以及有机亚磷酸所组成的群组;所述可塑剂更具体地选自由三乙二醇双(2-乙基己酸酯)(triethylene glycol bis(2-ethylhexanoate), 3GO)、四乙二醇双(2-乙基己酸酯)、三乙二醇双(2-乙基丁酸酯)、四乙二醇双(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、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、己二酸双[2-(2-丁氧基乙氧基)乙酯]、聚己二酸酯、丙二醇二苯甲酸酯、二丙二醇二苯甲酸酯、三丙二醇二苯甲酸酯、聚丙二醇二苯甲酸酯、2,2,4- 三甲基-1,3-戊二醇二苯甲酸酯、苯甲酸异癸酯、苯甲酸-2-乙基己酯、邻苯二甲酸二异壬酯、对苯二甲酸二丁氧基乙酯、蓖麻油、蓖麻油酸甲酯、大豆油、以及环氧化大豆油所组成的群组。On the other hand, the plasticizer is also called plasticizer, which is usually used in combination with polyvinyl acetal resin to affect the viscoelastic properties of the material. Specifically, the plasticizer is non-limitingly selected from the group consisting of monobasic acid esters, polybasic acid esters, organic phosphoric acid, and organic phosphorous acid; more specifically, the plasticizer is selected from triethylene glycol bis(2 -Ethylhexanoate) (triethylene glycol bis(2-ethylhexanoate), 3GO), tetraethylene glycol bis(2-ethylhexanoate), triethylene glycol bis(2-ethylbutyrate), Tetraethylene glycol bis(2-ethylbutyrate), triethylene glycol diheptanoate, tetraethylene glycol diheptanoate, dihexyl adipate, dioctyl adipate, adipic acid Hexylcyclohexyl ester, diisononyl adipate, heptylnonyl adipate, dibutyl sebacate, bis[2-(2-butoxyethoxy)ethyl adipate], Polyadipate, Propylene Glycol Dibenzoate, Dipropylene Glycol Dibenzoate, Tripropylene Glycol Dibenzoate, Polypropylene Glycol Dibenzoate, 2,2,4-Trimethyl-1,3 -Pentylene glycol dibenzoate, isodecyl benzoate, 2-ethylhexyl benzoate, diisononyl phthalate, dibutoxyethyl terephthalate, castor oil, castor The group consisting of methyl sesoleate, soybean oil, and epoxidized soybean oil.

本发明所提供的聚合物膜为一层或多层的结构,其损耗因子最低值出现的温度为40℃至60℃,例如但不限于:42.28℃、48.29℃、49.77℃、51.43℃、 52.23℃、54.21℃、56.18℃、58.27℃或者59.14℃。The polymer film provided by the present invention has a one-layer or multi-layer structure, and the temperature at which the minimum value of the loss factor appears is 40°C to 60°C, such as but not limited to: 42.28°C, 48.29°C, 49.77°C, 51.43°C, 52.23°C °C, 54.21 °C, 56.18 °C, 58.27 °C, or 59.14 °C.

所谓损耗因子即为tanδ(或称损耗因子、阻尼因子、损耗角正切),用以表达材料黏弹性质中的阻尼特性,并且可对等为材料的损耗模量(或称损失模量、黏性模量,lossmodulus,G”)与储存模量(或称弹性模量,storage modulus,G’) 的比值。在不受特定理论限制之下,损耗因子会有最低值出现,此低点代表能量主要被储存;但过了此低点的温度后,能量渐渐转为消耗,此时黏性开始提高。因此,可藉由调整此低点来满足加工制程的要求,例如:倘若此低点小于加工温度,会因为膜太软导致断膜;反之,若此低点大于加工温度,会因为膜太有韧性使得展膜不易。The so-called loss factor is tanδ (or loss factor, damping factor, loss tangent), which is used to express the damping characteristics in the viscoelastic properties of materials, and can be equivalent to the loss modulus of materials (or loss modulus, viscoelasticity modulus, lossmodulus, G") to the ratio of the storage modulus (or elastic modulus, storage modulus, G'). Without being limited by a specific theory, the loss factor will have the lowest value, and this low point represents Energy is mainly stored; but after the temperature of this low point, the energy is gradually turned into consumption, and the viscosity begins to increase at this time. Therefore, this low point can be adjusted to meet the requirements of the processing process, for example: if this low point If it is lower than the processing temperature, the film will be broken because the film is too soft; on the contrary, if the low point is greater than the processing temperature, it will be difficult to expand the film because the film is too tough.

依据本发明的一些实施例,其损耗因子最低值为0.13至0.19,例如但不限于:0.138、0.141、0.144、0.149、0.151、0.174、0.177、0.179或者0.181。依据本发明的一些实施例,所述聚合物膜系一单层膜体的结构并具有一Tg,而其损耗因子最低值出现的温度大于该Tg;根据本发明的另一些实施例,所述聚合物膜系一多层膜体的结构并具有一最大Tg,而其损耗因子最低值出现的温度大于该最大Tg。如本文所用,所谓Tg系指玻璃转移温度,其系指物质在玻璃态(系指材料处于流动性低的状态)以及高弹性态(系指材料处于流动性高且柔软的状态)之间可逆转化的温度;进一步地,损耗因子产生波峰值的温度即为玻璃转移温度。According to some embodiments of the present invention, the minimum value of the loss factor is 0.13 to 0.19, such as but not limited to: 0.138, 0.141, 0.144, 0.149, 0.151, 0.174, 0.177, 0.179 or 0.181. According to some embodiments of the present invention, the polymer film is a single-layer film structure and has a Tg, and the temperature at which the minimum value of the loss factor occurs is greater than the Tg; according to other embodiments of the present invention, the The polymer film has a structure of a multi-layer film body and has a maximum Tg, and the temperature at which the minimum value of the dissipation factor occurs is greater than the maximum Tg. As used herein, the so-called Tg refers to the glass transition temperature, which refers to the reversibility of a substance between the glassy state (meaning that the material is in a low fluidity state) and the high elastic state (meaning that the material is in a high fluidity and soft state) The transformation temperature; further, the temperature at which the loss factor produces a peak value is the glass transition temperature.

本文所述的聚乙烯醇缩醛树脂的羟基含量比是指以百分率表示与羟基键结的伸乙基量除以主链的总伸乙基量而求出的摩尔分率。本文所述的聚乙烯醇缩醛树脂的缩醛度(或称缩醛化度)是指以百分率表示与缩醛基键结的伸乙基量除以主链的总伸乙基量而求出的摩尔分率。本文所述的聚乙烯醇缩醛树脂的乙酰度(或称乙酰化度)是以百分率表示的值,其是从主链的总伸乙基量减去与羟基键结的伸乙基量及与缩醛基键结的伸乙基量,再将所得之值除以主链的总伸乙基量而求出的摩尔分率。The hydroxyl group content ratio of the polyvinyl acetal resin herein refers to a mole fraction obtained by dividing the amount of ethylidene groups bonded to hydroxyl groups by the total amount of ethylidene groups in the main chain in percentage. The degree of acetalization (or called the degree of acetalization) of the polyvinyl acetal resin described herein refers to the amount expressed as a percentage of the ethylenic group bonded to the acetal group divided by the total ethylenic group amount of the main chain. out the mole fraction. The degree of acetylation (or the degree of acetylation) of the polyvinyl acetal resin described herein is a value expressed as a percentage, which is the amount of ethylidene groups bonded to hydroxyl groups and The mole fraction obtained by dividing the amount of ethylenyl groups bonded to the acetal group by the total amount of ethylenyl groups in the main chain.

上述羟基含量比、缩醛度及乙酰度是依据JIS K6728的“莫耳聚乙烯醇缩丁醛试验方法”测定的结果算出。The above-mentioned hydroxyl group content ratio, degree of acetalization, and degree of acetylation are calculated based on the measurement results of "Molar polyvinyl butyral test method" of JIS K6728.

图1至图3是依据本发明不同实施例所呈现的聚合物膜剖面图。所述不同实施例系分别表达本发明聚合物膜不同的结构态样;具体而言,本发明所提供的聚合物膜可为单层膜结构(如图1所示)、三层膜结构(如图2所示)以及楔形膜结构(如图3所示)。然而,在不违背本发明中心思想的情况下,本领域具有通常知识者可依需求调整或修改所述结构态样的内容。1 to 3 are cross-sectional views of polymer films according to different embodiments of the present invention. The different embodiments respectively express the different structural aspects of the polymer film of the present invention; specifically, the polymer film provided by the present invention can be a single-layer film structure (as shown in Figure 1), a three-layer film structure ( As shown in Figure 2) and wedge-shaped membrane structure (as shown in Figure 3). However, those skilled in the art can adjust or modify the contents of the structural aspects as required without departing from the central idea of the present invention.

单层膜Monolayer film

请参阅图1,本发明于此提供一聚合物膜100A,其具有一层体 101。该层体101的厚度较佳为0.2至2mm,更佳地为0.38至1.52mm,例如但不限于:0.38、0.76或1.52mm。该层体101的玻璃转移温度可为10至35℃,较佳地为 25至35℃,更佳地为28至33℃,但本发明并不为此所限定。Referring to FIG. 1 , the present invention provides a polymer film 100A, which has a layer 101. The thickness of the layer body 101 is preferably 0.2 to 2 mm, more preferably 0.38 to 1.52 mm, such as but not limited to: 0.38, 0.76 or 1.52 mm. The glass transition temperature of the layer 101 may be 10 to 35°C, preferably 25 to 35°C, more preferably 28 to 33°C, but the present invention is not limited thereto.

在本发明所提供的聚合物膜100A中,该层体101所含的聚乙烯醇缩醛树脂的羟基含量比为26至31mol%,较佳地为27.1至29.6mol%,例如但不限于:27.1、27.4、27.5或者29.6mol%。该层体101所含的聚乙烯醇缩醛树脂的缩醛度为68至73mol%,较佳地为69.4至71.9mol%,例如但不限于:69.4、71.5、 71.6或者71.9mol%。该层体101所含的聚乙烯醇缩醛树脂的乙酰度为0.1至3.0 mol%,较佳地为1.0mol%,但本发明并不为此所限定。In the polymer film 100A provided by the present invention, the polyvinyl acetal resin contained in the layer body 101 has a hydroxyl content ratio of 26 to 31 mol%, preferably 27.1 to 29.6 mol%, such as but not limited to: 27.1, 27.4, 27.5 or 29.6 mol%. The acetalization degree of the polyvinyl acetal resin contained in the layer body 101 is 68 to 73 mol%, preferably 69.4 to 71.9 mol%, such as but not limited to: 69.4, 71.5, 71.6 or 71.9 mol%. The acetylation degree of the polyvinyl acetal resin contained in the layer body 101 is 0.1 to 3.0 mol%, preferably 1.0 mol%, but the present invention is not limited thereto.

在本发明所提供的聚合物膜100A中,该层体101所含的聚乙烯醇缩醛树脂的假比重可为0.200至0.300,较佳地为0.240至0.260,更佳地为0.249至 0.258,但本发明并不为此所限定。本文所述的假比重是依据JIS K6720进行测定。In the polymer film 100A provided by the present invention, the pseudo specific gravity of the polyvinyl acetal resin contained in the layer body 101 may be 0.200 to 0.300, preferably 0.240 to 0.260, more preferably 0.249 to 0.258, But the present invention is not limited thereto. The pseudo specific gravity described here is measured based on JIS K6720.

在本发明所提供的聚合物膜100A中,该层体101所含的聚乙烯醇缩醛树脂的数量平均分子量(Mn)可为90,000至125,000,较佳地为105,000至 120,000,更佳地为106,250至115,200,但本发明并不为此所限定。In the polymer film 100A provided by the present invention, the number average molecular weight (Mn) of the polyvinyl acetal resin contained in the layer body 101 may be 90,000 to 125,000, preferably 105,000 to 120,000, more preferably 106,250 to 115,200, but the present invention is not limited thereto.

三层膜Three-layer film

请参阅图2,本发明于此提供一聚合物膜100B,其结构是呈现一中间层102夹设于上下两层保护层104之间的态样;然而,除此三层结构之外,本领域具有通常知识者可依据需求增设第四、第五或第六层等;且较佳地是同样以中间层及保护层交错层迭形成。具体而言,该中间层102的厚度较佳为0.11 至0.15mm,更佳地为0.13mm;该保护层104的厚度较佳为0.32至0.35mm,更佳地为0.335mm;而该聚合物膜100B的厚度较佳为0.5至2mm,更佳为0.75 至0.85mm,例如:0.75、0.76、0.77、0.78、0.8、0.82或0.85mm。于一较佳实施态样中,该聚合物膜系三层结构,上下两层为保护层并夹一中间层,其是作为夹层玻璃用的中间膜。Please refer to Fig. 2, the present invention provides a polymer film 100B here, and its structure is to present an intermediate layer 102 to be sandwiched between the aspect between two upper and lower protective layers 104; Yet, except this three-layer structure, this A person with ordinary knowledge in the field can add a fourth, fifth or sixth layer according to requirements; and preferably, the intermediate layer and the protective layer are also interleaved and laminated. Specifically, the thickness of the intermediate layer 102 is preferably 0.11 to 0.15mm, more preferably 0.13mm; the thickness of the protective layer 104 is preferably 0.32 to 0.35mm, more preferably 0.335mm; and the polymer The thickness of the film 100B is preferably 0.5 to 2 mm, more preferably 0.75 to 0.85 mm, for example: 0.75, 0.76, 0.77, 0.78, 0.8, 0.82 or 0.85 mm. In a preferred embodiment, the polymer film has a three-layer structure, the upper and lower layers are protective layers and an intermediate layer is sandwiched, which is used as an intermediate film for laminated glass.

在本发明所提供的聚合物膜100B中,该中间层102的玻璃转移温度可为-10至6℃,较佳地为-8至0℃,更佳地为-7至-2℃,但本发明并不为此所限定;该保护层104的玻璃转移温度可为10至35℃,较佳地为25至35℃,更佳地为28至33℃,但本发明并不为此所限定。In the polymer film 100B provided by the present invention, the glass transition temperature of the intermediate layer 102 may be -10 to 6°C, preferably -8 to 0°C, more preferably -7 to -2°C, but The present invention is not limited thereto; the glass transition temperature of the protective layer 104 may be 10 to 35°C, preferably 25 to 35°C, more preferably 28 to 33°C, but the present invention is not limited thereto. limited.

在本发明所提供的聚合物膜100B中,该中间层102所含的聚乙烯醇缩醛树脂的羟基含量比为22至27mol%,较佳地为23.8至26.2mol%,例如但不限于:23.8、24.9或者26.2mol%。该中间层102所含的聚乙烯醇缩醛树脂的缩醛度为62至68mol%,较佳地为63.3至67.6mol%,例如但不限于:63.3、 63.7或者67.6mol%。该中间层102所含的聚乙烯醇缩醛树脂的乙酰度为7至13 mol%,例如但不限于:8.6、10.5或者11.4mol%,但本发明并不为此所限定。另一方面,该保护层104所含的聚乙烯醇缩醛树脂的羟基含量比为26至31mol%,较佳地为27.4至30.1mol%,例如但不限于:27.4、27.8或者30.1mol%。该保护层104所含的聚乙烯醇缩醛树脂的缩醛度为68至73mol%,较佳地为68.9至 71.6mol%,例如但不限于:68.9、71.2、或者71.6mol%。该保护层104所含的聚乙烯醇缩醛树脂的乙酰度为0.1至3.0mol%,较佳地为1.0mol%,但本发明并不为此所限定。In the polymer film 100B provided by the present invention, the polyvinyl acetal resin contained in the intermediate layer 102 has a hydroxyl content ratio of 22 to 27 mol%, preferably 23.8 to 26.2 mol%, such as but not limited to: 23.8, 24.9 or 26.2 mol%. The acetalization degree of the polyvinyl acetal resin contained in the intermediate layer 102 is 62 to 68 mol%, preferably 63.3 to 67.6 mol%, such as but not limited to: 63.3, 63.7 or 67.6 mol%. The acetylation degree of the polyvinyl acetal resin contained in the middle layer 102 is 7 to 13 mol%, such as but not limited to: 8.6, 10.5 or 11.4 mol%, but the present invention is not limited thereto. On the other hand, the polyvinyl acetal resin contained in the protective layer 104 has a hydroxyl content ratio of 26 to 31 mol%, preferably 27.4 to 30.1 mol%, such as but not limited to: 27.4, 27.8 or 30.1 mol%. The acetalization degree of the polyvinyl acetal resin contained in the protective layer 104 is 68 to 73 mol%, preferably 68.9 to 71.6 mol%, such as but not limited to: 68.9, 71.2, or 71.6 mol%. The acetylation degree of the polyvinyl acetal resin contained in the protective layer 104 is 0.1 to 3.0 mol%, preferably 1.0 mol%, but the present invention is not limited thereto.

在本发明所提供的聚合物膜100B中,该中间层102所含的聚乙烯醇缩醛树脂的假比重可为0.200至0.300,较佳地为0.240至0.260,更佳地为 0.247至0.258,但本发明并不为此所限定;该保护层104所含的聚乙烯醇缩醛树脂的假比重可为0.200至0.300,较佳地为0.240至0.260,更佳地为0.251至0.257,但本发明并不为此所限定。In the polymer film 100B provided by the present invention, the polyvinyl acetal resin contained in the intermediate layer 102 may have a pseudo specific gravity of 0.200 to 0.300, preferably 0.240 to 0.260, more preferably 0.247 to 0.258, But the present invention is not limited thereto; the pseudo specific gravity of the polyvinyl acetal resin contained in the protective layer 104 can be 0.200 to 0.300, preferably 0.240 to 0.260, more preferably 0.251 to 0.257, but this The invention is not limited thereto.

在本发明所提供的聚合物膜100A中,该中间层102所含的聚乙烯醇缩醛树脂的数量平均分子量(Mn)可为100,000至280,000,较佳地为120,000 至250,000,更佳地为150,000至225,000,但本发明并不为此所限定;该保护层 104所含的聚乙烯醇缩醛树脂的数量平均分子量(Mn)可为90,000至125,000,较佳地为105,000至120,000,更佳地为107,950至112,000,但本发明并不为此所限定。In the polymer film 100A provided by the present invention, the number average molecular weight (Mn) of the polyvinyl acetal resin contained in the intermediate layer 102 may be 100,000 to 280,000, preferably 120,000 to 250,000, more preferably 150,000 to 225,000, but the present invention is not limited thereto; the number average molecular weight (Mn) of the polyvinyl acetal resin contained in the protective layer 104 can be 90,000 to 125,000, preferably 105,000 to 120,000, more preferably The range is 107,950 to 112,000, but the present invention is not limited thereto.

楔形膜wedge membrane

请参阅图3,本发明于此提供一聚合物膜100C。根据本发明一些实施例,该聚合物膜100C可以作为平视显示器用(head-up display,HUD)膜。具体而言,该聚合物膜100C为避免作为HUD膜时投影影像有重迭的状况,于膜体的两端分别设有一厚端以及厚度较该厚端为薄的薄端。该薄端具一厚度T1,而该厚端具一厚度T2;该厚度T1为0.7至0.8mm,较佳地为0.76mm;而该厚度T2为1.4至1.5mm,较佳地为1.45mm。更进一步地,该聚合物膜100C系说明一整体皆呈现楔形的膜体结构,且其宽度W1为1200mm。Please refer to FIG. 3 , where the present invention provides a polymer film 100C. According to some embodiments of the present invention, the polymer film 100C may be used as a head-up display (HUD) film. Specifically, in order to avoid overlapping projected images when the polymer film 100C is used as a HUD film, two ends of the film body are respectively provided with a thick end and a thin end that is thinner than the thick end. The thin end has a thickness T 1 , and the thick end has a thickness T 2 ; the thickness T 1 is 0.7 to 0.8 mm, preferably 0.76 mm; and the thickness T 2 is 1.4 to 1.5 mm, preferably is 1.45mm. Furthermore, the polymer film 100C illustrates a wedge-shaped film structure as a whole, and its width W 1 is 1200 mm.

在本发明所提供的聚合物膜100C中,聚合物膜100C所含的聚乙烯醇缩醛树脂的范围与上述单层膜的实施例内容相似,该聚合物膜100C所含的聚乙烯醇缩醛树脂的羟基含量比为26至31mol%,较佳地为28.3至28.7mol%,例如但不限于:28.3或者28.7mol%;该聚合物膜100C所含的聚乙烯醇缩醛树脂的缩醛度(mol%)为68至73mol%,较佳地为70.3至70.7mol%,例如但不限于:70.3或者70.7mol%;而该聚合物膜100C所含的聚乙烯醇缩醛树脂的乙酰度(mol%)为0.1至3.0mol%,较佳地为1.0mol%,但本发明并不为此所限定。In the polymer film 100C provided by the present invention, the scope of the polyvinyl acetal resin contained in the polymer film 100C is similar to the content of the above-mentioned embodiment of the single-layer film, and the polyvinyl acetal resin contained in the polymer film 100C The hydroxyl content ratio of the aldehyde resin is 26 to 31 mol%, preferably 28.3 to 28.7 mol%, such as but not limited to: 28.3 or 28.7 mol%; the acetal of the polyvinyl acetal resin contained in the polymer film 100C The acetylation degree (mol%) is 68 to 73mol%, preferably 70.3 to 70.7mol%, such as but not limited to: 70.3 or 70.7mol%; and the acetylation degree of the polyvinyl acetal resin contained in the polymer film 100C (mol%) is 0.1 to 3.0 mol%, preferably 1.0 mol%, but the present invention is not limited thereto.

聚合物膜的制造流程Polymer film manufacturing process

图4至图5是分别呈现本发明不同实施例的聚合物膜制造流程图。请先参阅图4,于此所提供的聚合物膜制造流程是用以制成如上述的单层膜以及楔形膜态样;其流程至少包含步骤S100至S102。4 to 5 are flow charts showing different embodiments of the polymer film fabrication of the present invention. Please refer to FIG. 4 first. The polymer film manufacturing process provided here is used to manufacture the above-mentioned single-layer film and wedge-shaped film; the process at least includes steps S100 to S102.

具体而言,在步骤S100中,将一聚乙烯醇缩醛树脂以及一可塑剂混练形成一树脂组合物。其中,该聚乙烯醇缩醛树脂以100重量份计,该可塑剂较佳为30至60重量份;更佳地,该可塑剂为35至45重量份,例如:35、 36、37、38、39、40、41、42、43、44或45重量份。另一方面,混练时的操作温度以及转速可依据习用方法及需求所调整,其细部条件不为本案所限制。Specifically, in step S100, a polyvinyl acetal resin and a plasticizer are kneaded to form a resin composition. Wherein, the polyvinyl acetal resin is based on 100 parts by weight, the plasticizer is preferably 30 to 60 parts by weight; more preferably, the plasticizer is 35 to 45 parts by weight, for example: 35, 36, 37, 38 , 39, 40, 41, 42, 43, 44 or 45 parts by weight. On the other hand, the operating temperature and rotation speed during kneading can be adjusted according to conventional methods and requirements, and the detailed conditions are not limited by this case.

在步骤S102中,将树脂组合物制成聚合物膜。其中,制成方法可采用习用薄膜制备方式进行,例如:挤出成型或热压成型等方法。进一步地,在此步骤中可依据制成的聚合物膜态样而进行细部调整;例如:可细部调整以制成几何参数上不同的单层膜或是楔形膜。In step S102, the resin composition is made into a polymer film. Wherein, the manufacturing method can be carried out by conventional film preparation methods, such as extrusion molding or thermocompression molding and other methods. Further, in this step, detailed adjustments can be made according to the shape of the fabricated polymer film; for example, a single-layer film or a wedge-shaped film with different geometric parameters can be produced through detailed adjustments.

复请参阅图5,于此所提供的聚合物膜制造流程是用以制成如上述的三层膜态样;其流程至少包含步骤S200至S206。Referring again to FIG. 5 , the polymer film manufacturing process provided here is used to make the above-mentioned three-layer film; the process at least includes steps S200 to S206 .

具体而言,在步骤S200中,将第一聚乙烯醇缩醛树脂以及可塑剂混练形成第一树脂组合物。其中,该第一聚乙烯醇缩醛树脂以100重量份计时,该可塑剂较佳为60至90重量份;更佳地,该可塑剂为60至70重量份,例如:60、61、62、63、64、65、66、67、68、69或70重量份。另一方面,混练时的操作温度以及转速可依据习用方法及需求所调整,其细部条件不为本案所限制。Specifically, in step S200, the first polyvinyl acetal resin and the plasticizer are kneaded to form a first resin composition. Wherein, the first polyvinyl acetal resin is calculated as 100 parts by weight, the plasticizer is preferably 60 to 90 parts by weight; more preferably, the plasticizer is 60 to 70 parts by weight, for example: 60, 61, 62 , 63, 64, 65, 66, 67, 68, 69 or 70 parts by weight. On the other hand, the operating temperature and rotation speed during kneading can be adjusted according to conventional methods and requirements, and the detailed conditions are not limited by this case.

在步骤S202中,将第二聚乙烯醇缩醛树脂以及可塑剂混练形成第二树脂组合物;其中,该聚乙烯醇缩醛树脂以100重量份计,该可塑剂较佳为30至60重量份;更佳地,该可塑剂为35至45重量份,例如:35、36、37、 38、39、40、41、42、43、44或45重量份。另一方面,混练时的操作温度以及转速亦可依据习用方法及所调整,其细部条件不为本案所限制。In step S202, the second polyvinyl acetal resin and plasticizer are kneaded to form a second resin composition; wherein, based on 100 parts by weight of the polyvinyl acetal resin, the plasticizer is preferably 30 to 60 parts by weight; more preferably, the plasticizer is 35 to 45 parts by weight, for example: 35, 36, 37, 38, 39, 40, 41, 42, 43, 44 or 45 parts by weight. On the other hand, the operating temperature and rotation speed during kneading can also be adjusted according to conventional methods, and the detailed conditions are not limited by this case.

在步骤S204中,将第一树脂组合物及第二树脂组合物分别制成第一层及第二层;其中,制成方法可采用习用薄膜制备方式进行,例如:挤出成型或热压成型等方法。在步骤S206中,结合第一层及第二层以形成聚合物膜;其中,该第一层作为一中间层,而该第二层作为一保护层。另一方面,制成方法同样可采用习用薄膜制备方式,例如:挤出成型或热压成型等方法。根据至少一实施例,步骤S204及步骤S206可以是将第二树脂组合物(作为一保护层) 与第一树脂组合物(作为一中间层),以T-型模头共挤出的方式挤出具有三层结构的中间膜,其中该中间膜的结构为保护层/中间层/保护层。In step S204, the first resin composition and the second resin composition are respectively made into the first layer and the second layer; wherein, the manufacturing method can be carried out by conventional film preparation methods, such as extrusion molding or thermocompression molding and other methods. In step S206, the first layer and the second layer are combined to form a polymer film; wherein, the first layer serves as an intermediate layer, and the second layer serves as a protective layer. On the other hand, the manufacturing method can also adopt conventional film preparation methods, such as extrusion molding or thermocompression molding and other methods. According to at least one embodiment, step S204 and step S206 can be to extrude the second resin composition (as a protective layer) and the first resin composition (as an intermediate layer) with a T-type die head co-extrusion An intermediate film with a three-layer structure is produced, wherein the structure of the intermediate film is protective layer/intermediate layer/protective layer.

聚乙烯醇缩醛树脂的分子量的测定Determination of molecular weight of polyvinyl acetal resin

利用胶体渗透层析法(gel permeation chromatography,GPC) 来测量聚乙烯醇缩醛树脂的分子量分布,其中是将聚乙烯醇缩醛树脂溶解于四氢呋喃(tetrahydrofuran,THF)中,在以下条件下进行GPC分析,并以对应聚苯乙烯标准品(Waters PS STD)面积的比率计算其分子量。The molecular weight distribution of the polyvinyl acetal resin was measured by gel permeation chromatography (GPC), wherein the polyvinyl acetal resin was dissolved in tetrahydrofuran (tetrahydrofuran, THF), and GPC was carried out under the following conditions Analyze and calculate its molecular weight as the ratio of the area of the corresponding polystyrene standard (Waters PS STD).

装置:Waters 1515PUMP systemDevice: Waters 1515PUMP system

探测器:Waters 2414RIDetector: Waters 2414RI

冲提条件:1.0毫升/分钟(mL/min),THFEluting condition: 1.0 milliliter/minute (mL/min), THF

管柱:Waters Styragel HR5 THF、Waters Styragel HR4 THF、Waters StyragelHR3 THF、Waters Styragel HR1 THFColumns: Waters Styragel HR5 THF, Waters Styragel HR4 THF, Waters Styragel HR3 THF, Waters Styragel HR1 THF

经由以上流程所制造而成的聚合物膜可作为一待测膜片进行以下各式特性测定。The polymer film manufactured through the above process can be used as a film to be tested for the following various characteristic measurements.

黏弹性质的测定Determination of viscoelastic properties

本文用以测定黏弹性质的方法至少包括下列步骤:首先,将待测膜片裁切为一圆形,其直径为8mm,并将所述待测膜片放置于一恒温恒湿箱中 24小时,进一步调控其温度以及相对湿度分别保持在23℃以及55%。其中特别需要注意的是,所述裁切为一圆形的步骤中,系依待测膜片的宽度方向的中间处进行裁切。The method for measuring viscoelastic properties in this paper at least includes the following steps: First, cut the membrane to be tested into a circle with a diameter of 8mm, and place the membrane to be tested in a constant temperature and humidity box 24 Hours, the temperature and relative humidity were further adjusted and maintained at 23°C and 55%, respectively. It should be particularly noted that in the step of cutting into a circle, the cutting is carried out at the middle of the width direction of the film to be tested.

接续,将待测膜片放置于一旋转剪切流变仪(Discovery Hybrid Rheometer II,DHR)(TA Instrument制造)中以振荡法进行黏弹性质的分析,分析条件如下:测试温度由100℃降至-20℃,且其降温速率为3℃/min;振荡频率设定为1Hz;将待测膜片维持在1%的应变;夹具压力设定为1N。藉由上述方法自分析结果中获得待测膜片的损耗因子及玻璃转移温度。Next, place the membrane to be tested in a rotational shear rheometer (Discovery Hybrid Rheometer II, DHR) (manufactured by TA Instrument) to analyze the viscoelastic properties by the oscillation method. The analysis conditions are as follows: the test temperature decreases from 100 ° C to to -20°C, and the cooling rate is 3°C/min; the oscillation frequency is set to 1Hz; the strain of the diaphragm to be tested is maintained at 1%; the clamp pressure is set to 1N. The dissipation factor and glass transition temperature of the membrane to be tested are obtained from the analysis results by the above method.

热收缩率的测定Determination of heat shrinkage

本文用以测定热收缩率的方法是基于以下仪器进行测定:The method used in this paper to determine thermal shrinkage is based on the following instruments:

加热烘箱(型号:Binder FD-115W)Heating Oven (Model: Binder FD-115W)

热循环烘箱thermal cycle oven

计尺器(精度为1mm)Ruler (accuracy is 1mm)

本文用以测定热收缩率的方法至少包括下列步骤:将待测膜片裁切为一正方形,其边长为17cm,并于该待测膜片内画记15cm的正方形标线;接续,将该待测膜片悬吊于温度设定为50℃的烘箱内1小时后,取出并置于室温环境下1小时;最后对该待测膜片的热收缩率进行测定。The method for determining thermal shrinkage rate in this paper at least includes the following steps: cutting the film to be tested into a square with a side length of 17 cm, and marking a 15 cm square marking line in the film to be tested; After the film to be tested was suspended in an oven set at 50°C for 1 hour, it was taken out and placed at room temperature for 1 hour; finally, the thermal shrinkage of the film to be tested was measured.

针对热收缩率的计算方法为:热收缩率(%)=(加热前长度-加热后长度)/加热前长度*100。在不受特定理论限制之下,经计算而得的热收缩率数值结果越高则该待测膜片越偏向流动性高且柔软的状态;而热收缩率数值结果越低则该待测膜片越偏向流动性低且坚硬的状态。根据至少一实施例,于50℃热处理1小时下,待测膜片所表现的热收缩率数值若在2-5%的范围内,则其待测膜片可被视为具备良好的加工性。The calculation method for thermal shrinkage rate is: thermal shrinkage rate (%)=(length before heating−length after heating)/length before heating*100. Without being bound by a specific theory, the higher the calculated heat shrinkage value, the more the film to be tested tends to be in a state of high fluidity and softness; and the lower the heat shrinkage value, the more the film to be tested is The sheet tends to be in a hard state with low fluidity. According to at least one embodiment, under heat treatment at 50°C for 1 hour, if the thermal shrinkage value of the film to be tested is in the range of 2-5%, then the film to be tested can be considered to have good processability .

伸长率的测定Determination of elongation

本文用以测定伸长率的方法系依循ASTM D412测试规范,而其所采用的仪器为GOTECH制的AI-7000M拉力试验机。具体而言,所述方法至少包括下列步骤:将待测膜片放置于相对湿度23%而温度为23℃的环境下2小时。The method used to measure elongation in this paper follows the ASTM D412 test specification, and the instrument used is the AI-7000M tensile testing machine manufactured by GOTECH. Specifically, the method at least includes the following steps: placing the film to be tested in an environment with a relative humidity of 23% and a temperature of 23° C. for 2 hours.

针对伸长率的计算方法为:伸长率(%)=(拉伸后长度-拉伸前长度)/拉伸前长度*100。根据至少一实施例,待测膜片所表现的伸长率数值若在220%至300%的范围内,则其待测膜片可被视为具备良好的加工性。若伸长率大于300%时,则在展膜过程容易变形;若伸长率小于220%时,则在使用上因较难拉伸,而导致展膜不易。The calculation method for elongation is: elongation (%)=(length after stretching−length before stretching)/length before stretching*100. According to at least one embodiment, if the elongation value of the film to be tested is in the range of 220% to 300%, the film to be tested can be considered to have good processability. If the elongation is greater than 300%, it will be easily deformed during the stretching process; if the elongation is less than 220%, it will be difficult to stretch in use, resulting in difficult stretching.

实施例1至9Examples 1 to 9

于此,本发明依据上述内容提供实施例1至9的聚合物膜,不同实施例之间调整以不同参数制成而产生不同特性;进一步地,针对聚合物膜的黏弹性质、热收缩率以及伸长率的特性进行分析。实施例1至9的详细参数界定以及特性分析结果如表1所示。Here, the present invention provides the polymer films of Examples 1 to 9 according to the above content. Different examples are adjusted and made with different parameters to produce different characteristics; further, for the viscoelastic properties and thermal shrinkage of the polymer films And the characteristics of elongation were analyzed. The detailed parameter definitions and characteristic analysis results of Examples 1 to 9 are shown in Table 1.

实施例1至9的聚合物膜的制备方法简述如下:The preparation method of the polymer film of embodiment 1 to 9 is briefly described as follows:

制备保护层用树脂组成物:使用混练机将100重量份的第一聚乙烯醇缩醛树脂(示例性使用PVB树脂)与35至45重量份的可塑剂(示例性使用 3GO)充分混练,得到保护层用树脂组成物。Prepare the resin composition for the protective layer: use a kneader to fully knead 100 parts by weight of the first polyvinyl acetal resin (exemplarily use PVB resin) and 35 to 45 parts by weight of plasticizer (exemplarily use 3GO) , to obtain a resin composition for a protective layer.

制备中间层用树脂组成物:使用混练机将100重量份的第二聚乙烯醇缩醛树脂(示例性使用PVB树脂)与60至70重量份的可塑剂(示例性使用 3GO)充分混练,得到中间层用树脂组成物。Prepare the resin composition for the middle layer: use a kneader to fully knead 100 parts by weight of the second polyvinyl acetal resin (exemplary use of PVB resin) and 60 to 70 parts by weight of plasticizer (exemplary use of 3GO) , to obtain a resin composition for an intermediate layer.

制备膜体:实施例1至4使用挤出机将保护层用树脂组成物挤出成单层膜的形式,厚度为0.38至1.52mm;实施例5及6则系采用楔形膜(即HUD 膜)的形式,使用挤出机将前述树脂组成物挤出成一端厚一端薄,其中厚端及薄端的厚度分别为1.45mm及0.76mm,而HUD膜的宽度约为1200mm;而实施例7至9系将保护层用树脂组成物与中间层用树脂组成物,以T型模头共挤出的方式挤出形成三层膜的形式,厚度为0.8mm,其结构为保护层/中间层/保护层(厚度:0.335mm/0.13mm/0.335mm)。Preparation of film body: Examples 1 to 4 use an extruder to extrude the resin composition for the protective layer into a single-layer film with a thickness of 0.38 to 1.52 mm; ) form, using an extruder to extrude the above-mentioned resin composition into one end thick and one end thin, wherein the thickness of the thick end and the thin end are respectively 1.45mm and 0.76mm, and the width of the HUD film is about 1200mm; and the embodiment 7 to Series 9 extrudes the resin composition for the protective layer and the resin composition for the intermediate layer through a T-die to form a three-layer film with a thickness of 0.8mm, and its structure is protective layer/intermediate layer/ Protective layer (thickness: 0.335mm/0.13mm/0.335mm).

比较例1至8Comparative Examples 1 to 8

以相似于实施例1至9的制备方法比较例1至9的聚合物膜,差异之处如表2所示;进一步地,针对聚合物膜的黏弹性质、热收缩率以及伸长率的特性进行分析,分析与评定方法与实施例1至9相同。The polymer films of Examples 1 to 9 were compared in a preparation method similar to that of Examples 1 to 9, and the differences are shown in Table 2; further, for the viscoelastic properties, thermal shrinkage and elongation of the polymer films Characteristic is analyzed, and analysis and evaluation method are identical with embodiment 1 to 9.

需要阐明的是,比较例1至4是采用单层膜的形式;比较例5及 6则系采用楔形膜(即HUD膜)的形式;而比较例7至8系采用三层膜(以一中间层夹设于上下两层保护层的间)的形式。比较例1至8的详细参数界定以及特性分析结果如表2所示。It should be clarified that Comparative Examples 1 to 4 are in the form of a single-layer film; Comparative Examples 5 and 6 are in the form of a wedge-shaped film (i.e. a HUD film); and Comparative Examples 7 to 8 are in the form of a three-layer film (with a The middle layer is sandwiched between the upper and lower protective layers). The detailed parameter definitions and characteristic analysis results of Comparative Examples 1 to 8 are shown in Table 2.

表1Table 1

Figure BDA0003403987160000171
Figure BDA0003403987160000171

表2Table 2

Figure BDA0003403987160000181
Figure BDA0003403987160000181

由表1及表2可见,实施例1至9聚合物膜无论为单层膜或多层膜,藉由调控该聚合物膜的损耗因子最低值出现的温度为40℃至60℃,使实施例1至 9聚合物膜表现出相比比较例1至8聚合物膜更佳的流动性及加工性。由表2可进一步理解,如比较例1、3、5及7的损耗因子最低值出现的温度皆小于40℃,它们的热收缩率皆大于5%、伸长率皆大于300%,显示比较例1、3、5及7的聚合物膜太软,容易在展膜过程中变形或断膜;而比较例2、4、6及8的损耗因子最低值出现的温度皆大于60℃,其等的热收缩率皆小于2%、伸长率皆小于220%,显示比较例2、4、6及8的聚合物膜太有韧性,使得展膜不易。It can be seen from Table 1 and Table 2 that whether the polymer films in Examples 1 to 9 are single-layer films or multi-layer films, the temperature at which the lowest value of the loss factor of the polymer film appears is 40°C to 60°C, so that the implementation The polymer films of Examples 1 to 9 exhibited better fluidity and processability than the polymer films of Comparative Examples 1 to 8. It can be further understood from Table 2 that the temperature at which the lowest loss factor values of Comparative Examples 1, 3, 5, and 7 appear are all less than 40°C, and their thermal shrinkage rates are all greater than 5%, and their elongation rates are all greater than 300%, showing that comparative examples The polymer films of Examples 1, 3, 5, and 7 are too soft, and are easy to be deformed or broken during film stretching; while the lowest values of loss factors of Comparative Examples 2, 4, 6, and 8 all occur at temperatures greater than 60°C. The heat shrinkage ratios of the polymer films of Comparative Examples 2, 4, 6 and 8 are all less than 2%, and the elongation rates are all less than 220%, which shows that the polymer films of Comparative Examples 2, 4, 6 and 8 are too tough, making it difficult to stretch the film.

综上所述,本发明提供一种聚合物膜,其包含聚乙烯醇缩醛树脂及可塑剂;其中,该聚合物膜为一层或多层,且该聚合物膜的损耗因子最低值出现的温度为40℃至60℃。本发明所提供的聚合物膜具有良好的流动性及加工性。In summary, the present invention provides a polymer film comprising polyvinyl acetal resin and a plasticizer; wherein the polymer film is one or more layers, and the minimum value of the loss factor of the polymer film appears The temperature is 40°C to 60°C. The polymer film provided by the invention has good fluidity and processability.

除非本文另有定义,否则结合本申请所使用的科学及技术用语应具有本领域中具有通常知识者所理解的一般含义。此外,除非上下文另有要求,否则单数用语应包括复数,复数用语应包括单数。Unless otherwise defined herein, scientific and technical terms used in connection with this application shall have the ordinary meaning as understood by those of ordinary skill in the art. Further, unless otherwise required by context, words in the singular shall include pluralities and words in the plural shall include the singular.

以上已将本发明做一详细说明,惟以上所述者,仅是本发明的较佳实施例而已,当不能以此限定本发明实施的范围,即凡依本发明申请专利范围所作的均等变化与修饰,皆应仍属本发明的专利涵盖范围内。The present invention has been described in detail above, but the above is only a preferred embodiment of the present invention, and should not limit the scope of the present invention with this, that is, all equivalent changes made according to the patent scope of the present invention and modification, all should still belong to the scope of patent coverage of the present invention.

【符号说明】【Symbol Description】

100A~100C:聚合物膜100A~100C: polymer film

101:层体101: layer body

102:中间层102: middle layer

104:保护层104: protective layer

W1:宽度W 1 : width

T1,T2:厚度T 1 , T 2 : Thickness

S100~S102,S200~S206:步骤。S100~S102, S200~S206: steps.

Claims (18)

1.一种聚合物膜,其包含聚乙烯醇缩醛树脂及可塑剂,且所述聚合物膜为一层或多层,所述聚合物膜的损耗因子最低值出现的温度为40℃至60℃。1. A polymer film, which comprises polyvinyl acetal resin and a plasticizer, and the polymer film is one or more layers, and the temperature at which the minimum value of the loss factor of the polymer film occurs is from 40°C to 60°C. 2.如权利要求1的聚合物膜,其中所述损耗因子最低值为0.13至0.19。2. The polymer film of claim 1, wherein the loss factor minimum value is 0.13 to 0.19. 3.如权利要求2的聚合物膜,在一层的情况时,所述损耗因子最低值出现的温度大于其玻璃转移温度;或在多层的情况时,所述损耗因子最低值出现的温度大于其最大玻璃转移温度。3. The polymeric film of claim 2 , the temperature at which said dissipation factor minima occurs greater than its glass transition temperature in the case of a single layer; or the temperature at which said dissipation factor minima occurs in the case of a multilayer greater than its maximum glass transition temperature. 4.如权利要求1的聚合物膜,其中所述聚乙烯醇缩醛树脂为聚乙烯醇缩丁醛。4. The polymer film of claim 1, wherein the polyvinyl acetal resin is polyvinyl butyral. 5.如权利要求1的聚合物膜,其厚度为0.2mm至2mm。5. The polymer film according to claim 1, which has a thickness of 0.2 mm to 2 mm. 6.如权利要求1的聚合物膜,其于50℃热处理1小时下的热收缩率为2%至5%。6. The polymer film according to claim 1, which has a heat shrinkage rate of 2% to 5% upon heat treatment at 50°C for 1 hour. 7.如权利要求1的聚合物膜,其依据ASTM D412量测的伸长率为220%至300%。7. The polymer film of claim 1, which has an elongation measured according to ASTM D412 of 220% to 300%. 8.如权利要求1的聚合物膜,在一层的情况时,所述聚合物膜的所述聚乙烯醇缩醛树脂的羟基含量比为27mol%至31mol%,及/或所述聚乙烯醇缩醛树脂的缩醛度为68mol%至72mol%。8. The polymer film according to claim 1, wherein in the case of one layer, the hydroxyl content ratio of said polyvinyl acetal resin of said polymer film is 27 mol% to 31 mol%, and/or said polyethylene The degree of acetalization of the alcohol acetal resin is 68 mol% to 72 mol%. 9.如权利要求1的聚合物膜,在一层的情况时,其中所述聚合物膜的所述聚乙烯醇缩醛树脂以100重量份计,所述可塑剂为30至60重量份。9. The polymer film according to claim 1, wherein said plasticizer is 30 to 60 parts by weight based on 100 parts by weight of said polyvinyl acetal resin of said polymer film in the case of one layer. 10.如权利要求1至9任一项的聚合物膜,在一层的情况时,所述聚合物膜是平视显示器用膜。10. The polymer film according to any one of claims 1 to 9, which in the case of one layer is a film for a head-up display. 11.如权利要求10的聚合物膜,其具一厚端,及一厚度较所述厚端为薄的薄端。11. The polymer film of claim 10 having a thick end and a thin end having a thickness less than said thick end. 12.如权利要求1至7任一项的聚合物膜,在多层的情况时,其是三层结构,上下两层为保护层并夹一中间层。12. The polymer film according to any one of claims 1 to 7, in the case of multiple layers, it is a three-layer structure, the upper and lower layers are protective layers and an intermediate layer is sandwiched. 13.如权利要求12的聚合物膜,其中所述保护层的所述聚乙烯醇缩醛树脂,具有羟基含量比为27mol%至31mol%,及/或缩醛度为68mol%至72mol%。13. The polymer film according to claim 12, wherein said polyvinyl acetal resin of said protective layer has a hydroxyl content ratio of 27 mol% to 31 mol%, and/or a degree of acetalization of 68 mol% to 72 mol%. 14.如权利要求12的聚合物膜,其中所述保护层的所述聚乙烯醇缩醛树脂以100重量份计,所述可塑剂为30至60重量份。14. The polymer film according to claim 12, wherein said polyvinyl acetal resin of said protective layer is 30 to 60 parts by weight based on 100 parts by weight of said plasticizer. 15.如权利要求12的聚合物膜,其中所述中间层的所述聚乙烯醇缩醛树脂,具有羟基含量比为22至27mol%,及/或缩醛度为62mol%至68mol%。15. The polymer film according to claim 12, wherein said polyvinyl acetal resin of said intermediate layer has a hydroxyl content ratio of 22 to 27 mol%, and/or an acetalization degree of 62 to 68 mol%. 16.如权利要求12的聚合物膜,其中所述中间层的所述聚乙烯醇缩醛树脂以100重量份计,所述可塑剂为60至90重量份。16. The polymer film according to claim 12, wherein said polyvinyl acetal resin of said intermediate layer is 60 to 90 parts by weight based on 100 parts by weight of said plasticizer. 17.如权利要求12的聚合物膜,其是作为夹层玻璃用的中间膜,其厚度为0.5至2mm。17. The polymer film according to claim 12, which is an interlayer film for laminated glass and has a thickness of 0.5 to 2 mm. 18.如权利要求17的聚合物膜,其厚度为0.8mm,且所述保护层/中间层/保护层的厚度为0.335mm/0.13mm/0.335mm。18. The polymer film according to claim 17, having a thickness of 0.8mm, and the thickness of the protective layer/interlayer/protective layer is 0.335mm/0.13mm/0.335mm.
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