CN112703112A - 多孔层结构体及其制造方法 - Google Patents
多孔层结构体及其制造方法 Download PDFInfo
- Publication number
- CN112703112A CN112703112A CN201980062237.3A CN201980062237A CN112703112A CN 112703112 A CN112703112 A CN 112703112A CN 201980062237 A CN201980062237 A CN 201980062237A CN 112703112 A CN112703112 A CN 112703112A
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- CN
- China
- Prior art keywords
- substrate
- polyol component
- polyurethane prepolymer
- polyurethane
- mass
- 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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- 229920005830 Polyurethane Foam Polymers 0.000 claims abstract description 39
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- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 claims abstract description 18
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Images
Classifications
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
- D06N3/14—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
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- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
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- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
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- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
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- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/18—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by features of a layer of foamed material
- B32B5/20—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by features of a layer of foamed material foamed in situ
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- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
- B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
- B32B5/245—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it being a foam layer
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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Abstract
多孔层结构体,其是包含基材A、设置在该基材A上的聚氨酯发泡层的多孔层结构体,前述聚氨酯发泡层为将具有异氰酸酯基的聚氨酯预聚物发泡而成的发泡层,前述聚氨酯发泡层的密度为0.10~0.60g/cm3,前述聚氨酯预聚物实质上不含挥发成分,满足规定的组成。
Description
技术领域
本发明涉及多孔层结构体及其制造方法。
背景技术
聚氨酯预聚物用于粘合剂、涂料、密封材料等,特别是湿气固化型的聚氨酯预聚物因空气中的水分而固化,因此有能够以单组份使用的优点。这样的聚氨酯预聚物在分子内具有能够与空气中、涂布其的基材中存在的水(湿气)反应而形成交联结构的官能团(例如异氰酸酯基)。并且,根据用途开发了未固化、在常温下为液体或者固体状的、多种多样的聚氨酯预聚物。
另外,由于与水(湿气)反应而发泡,因此有时用作聚氨酯发泡体片材。聚氨酯发泡体片材由于具有优异的柔软性、伸缩性、缓冲性,因此与各种布料组合用于服装、靴子、护具等的用途中。以往,该聚氨酯发泡体片材的制造中使用有机溶剂,但是近年来由于对人体的有害性、环境问题其使用受到限制或禁止,当务之急是转变为不使用有机溶剂制造聚氨酯发泡体片材的方法。
例如,专利文献1中公开了不使用有害的有机溶剂,不需要有机溶剂的干燥步骤、提取步骤、减少了溶剂的蒸发除去所需要的能量消耗量的制造方法。
现有技术文献
专利文献
专利文献1 : 日本特许第3776428号公报。
发明内容
发明要解决的课题
专利文献1记载的方法的特征在于,使片状的液态混合物与水蒸气接触从而使液态混合物水发泡,但该方法中在发泡后与基材片贴合,因此与基材片的密合性降低。在要求良好的柔软性的聚氨酯用途中,从耐久性的角度考虑发泡层与基材层的良好的密合性也是必要的,专利文献1中得到的片材难以满足该要求。
由于上述情况,本发明的目的在于提供不使用有机溶剂制造、可发挥良好的柔软性和耐久性的多孔层结构体及其制造方法。
解决课题的手段
为了解决上述课题进行了深入研究,结果本发明人发现,通过包含将特定的聚氨酯预聚物发泡而成的聚氨酯发泡层的多孔层结构体可解决该课题,从而想到了本发明。即,本发明如下所述。
[1] 多孔层结构体,其是包含基材A、设置在该基材A上的聚氨酯发泡层的多孔层结构体,
前述聚氨酯发泡层为将具有异氰酸酯基的聚氨酯预聚物发泡而成的发泡层,
前述聚氨酯发泡层的密度为0.10~0.60g/cm3,
前述聚氨酯预聚物实质上不含挥发成分,满足下述(A)~(C)中的至少任一组成,
(A) 含有全部多元醇成分中的50质量%以上的凝胶点为20ml以上且小于30ml的多元醇成分(a)的组成,
(B) 含有全部多元醇成分中的30质量%以上的凝胶点为30ml以上且小于50ml的多元醇成分(b)的组成,
(C) 含有全部多元醇成分中的10质量%以上的凝胶点为50ml以上的多元醇成分(c)的组成。
[2] [1]所述的多孔层结构体,其中,设置前述聚氨酯发泡层前的前述基材A为含水基材A。
[3] [1]或[2]所述的多孔层结构体,其中,前述基材A为聚酯基布,聚氨酯发泡层的厚度为200μm时的用于由基材A剥离聚氨酯发泡层的剥离力为1.5kgf/inch以上。
[4] [1]~[3]中任一项所述的多孔层结构体,其中,前述聚氨酯预聚物含有全部多元醇成分中的50质量%以上的聚碳酸酯多元醇成分。
[5] [1]~[4]中任一项所述的多孔层结构体,其中,前述聚氨酯预聚物中,多异氰酸酯成分的异氰酸酯基当量相对于前述全部多元醇成分的羟基当量之比为1.33~5.0。
[6] [1]~[5]中任一项所述的多孔层结构体的制造方法,其包含:
对基材A实施含水处理,制成含水基材A的基材含水处理步骤、
将具有异氰酸酯基的聚氨酯预聚物涂布在基材B上形成聚氨酯预聚物涂膜的聚氨酯预聚物涂布步骤、
将前述含水基材A和在前述基材B上形成的前述聚氨酯预聚物涂膜贴合,制作涂膜结构体的涂膜结构体制作步骤、
对前述涂膜结构体实施陈化处理的陈化处理步骤,
前述聚氨酯预聚物实质上不含挥发成分,满足下述(A)~(C)中的至少任一组成,
(A) 含有全部多元醇成分中的50质量%以上的凝胶点为20ml以上且小于30ml的多元醇成分(a)的组成,
(B) 含有全部多元醇成分中的30质量%以上的凝胶点为30ml以上且小于50ml的多元醇成分(b)的组成,
(C) 含有全部多元醇成分中的10质量%以上的凝胶点为50ml以上的多元醇成分(c)的组成。
[7] [6]所述的多孔层结构体的制造方法,其中,在前述涂膜结构体制作步骤与前述陈化处理步骤之间,包含使水蒸气与前述涂膜结构体接触的水蒸气接触步骤。
发明效果
根据本发明,可提供不使用有机溶剂而制造、可发挥良好的柔软性和耐久性的多孔层结构体及其制造方法。
附图说明
[图1] 显示本实施方式的多孔层结构体的截面示意图。
[图2] 显示以往的多孔层结构体的截面示意图。
具体实施方式
以下,详细说明本发明的实施方式(本实施方式),但本发明不限于该实施方式。
[1.多孔层结构体]
本实施方式的多孔层结构体包含基材A、设置在该基材A上的聚氨酯发泡层。聚氨酯发泡层是将具有异氰酸酯基的聚氨酯预聚物发泡而成的发泡层。即,该聚氨酯发泡层是由具有异氰酸酯基的聚氨酯预聚物的发泡物形成的发泡层。
上述聚氨酯发泡层的一部分以侵入基材A的内部的方式存在。结果,基材A与聚氨酯发泡层的密合性提高,它们不剥离,发挥优异的耐久性。另外,由于发泡了,因此在维持优异的耐久性的同时具有良好的柔软性。
为了兼顾向基材A内部的侵入和良好的柔软性,本发明中,使聚氨酯发泡层的密度为0.10~0.60g/cm3,且作为用于形成该聚氨酯发泡层的聚氨酯预聚物,使用具有异氰酸酯基的特定的聚氨酯预聚物。
聚氨酯发泡层的密度与发泡层的发泡倍率相关,密度越低发泡倍率越高。并且,通过使聚氨酯发泡层的密度为0.10~0.60g/cm 3,在维持与基材A等的密合性的同时,得到良好的柔软性。
另外,本实施方式的聚氨酯预聚物实质上不含挥发成分。即,由于不使用有机溶剂制造多层结构体,因此不产生有害性的问题、环境问题。
在此,本发明中,“实质上不含挥发成分”是指不有意地含有有机溶剂等挥发成分,更具体地是指不存在有机溶剂。
本发明的具有异氰酸酯基的聚氨酯预聚物满足下述(A)~(C)中的至少任一组成。
(A) 含有全部多元醇成分中的50质量%以上的凝胶点为20ml以上且小于30ml的多元醇成分(a)的组成,
(B) 含有全部多元醇成分中的30质量%以上的凝胶点为30ml以上且小于50ml的多元醇成分(b)的组成,
(C) 含有全部多元醇成分中的10质量%以上的凝胶点为50ml以上的多元醇成分(c)的组成。
在此,凝胶点可如下所述地求出。
首先,准备含有多元醇成分1质量%的N,N’-二甲基甲酰胺(DMF)溶液。然后,用螺旋浆搅拌器充分搅拌使其均匀,同时在该溶液中滴加蒸馏水,在25±1℃的温度条件下求出多元醇开始凝固、微微白浊时的水滴加量(ml)。
要说明的是,测定中使用的DMF需要使用水分为0.03质量%以下的DMF,DMF溶液预先微微白浊的情况下,可将凝固开始、白浊程度变化时的水滴加量作为凝胶点。
多元醇成分(a)~(c)的凝胶点表示亲水性的程度,凝胶点为20ml以上且小于30ml的多元醇成分(a)在多元醇成分(a)~(c)中亲水性程度最低,因此,为了得到可形成具有良好的柔软性、特别是柔软的手感的合成人造革的发泡层,优选含有全部多元醇成分中的50质量%以上。
成为多元醇成分(a)的多元醇,是满足上述凝胶点范围的聚酯多元醇,具体而言,作为聚酯多元醇的醇成分,可列举乙二醇、二乙二醇、三乙二醇、丙二醇、1、2-丙二醇、正丙二醇、1,3-丁二醇、1,4-丁二醇、1,3-戊二醇、1,5-戊二醇、1,6-己二醇、己二醇、3-甲基-1,5-戊二醇、2-乙基-1,3-己二醇、1,9-壬二醇、新戊二醇等,作为酸成分,可列举对苯二甲酸、间苯二甲酸、丙二酸、戊二酸、庚二酸、辛二酸、琥珀酸、己二酸、壬二酸、癸二酸、十二烷二酸等的二元酸。对于这些二元醇成分和二元酸的组合,可列举单独使用,或将各成分使用2种以上得到的聚酯二元醇等,作为醇成分,含有乙二醇、二乙二醇、1、2-丙二醇、正丙二醇中的至少1种以上,或者作为酸成分含有琥珀酸等是优选的。关于上述多元醇的数均分子量,没有特别限定,优选为500~3000。
另外,凝胶点为30ml以上且小于50ml的多元醇成分(b)在多元醇成分(a)~(c)中亲水性程度为中等程度,因此为了得到可形成具有良好的柔软性、特别是柔软的手感的合成人造革的发泡层,优选含有全部多元醇成分中的30质量%以上。
成为多元醇成分(b)的多元醇,为满足上述凝胶点范围的聚酯多元醇,具体而言,作为聚酯多元醇的醇成分,可列举乙二醇、二乙二醇、三乙二醇、丙二醇、1、2-丙二醇、正丙二醇、1,3-丁二醇、1,4-丁二醇、1,3-戊二醇、1,5-戊二醇、1,6-己二醇、己二醇、3-甲基-1,5-戊二醇、2-乙基-1,3-己二醇、1,9-壬二醇、新戊二醇等,作为酸成分,可列举对苯二甲酸、间苯二甲酸、丙二酸、戊二酸、庚二酸、辛二酸、琥珀酸、己二酸、壬二酸、癸二酸、十二烷二酸等二元酸。对于这些二元醇成分和二元酸的组合,可列举单独使用,或将各成分使用2种以上得到的聚酯二元醇等,作为醇成分,含有乙二醇、二乙二醇、1、2-丙二醇、正丙二醇中的至少1种以上,或者作为酸成分含有琥珀酸等是优选的。关于上述多元醇的数均分子量,没有特别限定,优选为500~小于2000。
而且,凝胶点为50ml以上的多元醇成分(c)在多元醇成分(a)~(c)中亲水性程度最高,因此为了得到可形成具有良好的柔软性、特别是柔软的手感的合成人造革的发泡层,优选含有全部多元醇成分中的10质量%以上。
成为多元醇成分(c)的多元醇,具体而言,为满足上述凝胶点范围的聚醚多元醇,具体可列举聚乙二醇(PEG)、EO/PO共聚物、EO/THF共聚物等。关于上述多元醇的数均分子量,没有特别限定,优选为500~6000。
以下对本实施方式的聚氨酯预聚物、基材、聚氨酯发泡层等进行更详细的说明。
<聚氨酯预聚物>
聚氨酯预聚物如已经说明的,由满足(A)~(C)的至少任一组成的多元醇成分、异氰酸酯成分和适当的其它成分构成。即,本实施方式的具有异氰酸酯基的聚氨酯预聚物是由多元醇成分和多异氰酸酯成分得到的聚氨酯预聚物。特别是,该聚氨酯预聚物是湿气固化型聚氨酯预聚物,利用湿气固化时发泡而得到本发明的多孔层结构体。
(多元醇成分)
聚氨酯预聚物如果满足已经说明的(A)~(C)的至少任一组成,则可以含有多元醇成分(a)~(c)以外的多元醇成分。
例如,可以将多元醇成分(a)~(c)的各自与在凝胶点测定中小于20ml的多元醇成分(x)组合。如果是这样的组合,则例如可确保发泡性的同时,提高初期粘合强度、提高弯曲性、赋予耐化学药品性、耐久性、调整粘度等。
成为多元醇成分(x)的多元醇,具体地,作为聚醚多元醇,可列举聚氧四亚甲基二醇(PTMG)、聚氧亚丙基二醇(PPG)、凝胶点小于20ml的聚酯多元醇、己内酯系多元醇、聚碳酸酯系多元醇等。
特别是为了提高耐水解性而得到更良好的耐久性,可以含有聚碳酸酯多元醇成分。含有聚碳酸酯多元醇成分时,优选含有全部多元醇成分中的50质量%以上,更优选含有70~90质量%。
作为成为聚碳酸酯多元醇成分的聚碳酸酯多元醇,如果是烷烃二醇与碳酸二烷基酯、碳酸亚烷基酯、碳酸二苯酯等碳酸酯化合物反应得到的以往公知的聚碳酸酯多元醇,则没有特别限定。
(异氰酸酯成分)
作为本实施方式的聚氨酯预聚物的合成成分使用的异氰酸酯没有特别限定,优选脂肪族二异氰酸酯、脂环族二异氰酸酯、芳香族二异氰酸酯等2官能的多异氰酸酯。
作为成为异氰酸酯成分的多异氰酸酯的具体例子,为甲苯二异氰酸酯、4-甲氧基-1,3-苯二异氰酸酯、4-异丙基-1,3-苯二异氰酸酯、4-氯-1,3-苯二异氰酸酯、4-丁氧基-1,3-苯二异氰酸酯、2,4-二异氰酸酯-二苯基醚、均三甲苯二异氰酸酯、4,4’-二苯基甲烷二异氰酸酯、亚杜基二异氰酸酯、1,5-萘二异氰酸酯、联苯胺二异氰酸酯、o-硝基联苯胺二异氰酸酯、4,4-二异氰酸二苄基酯、1,4-四亚甲基二异氰酸酯、1,5-五亚甲基二异氰酸酯、1,6-六亚甲基二异氰酸酯、1,10-十亚甲基二异氰酸酯、1,4-亚环己基二异氰酸酯、二甲苯二异氰酸酯、4,4’-亚甲基双(环己基异氰酸酯)、1,5-四氢萘二异氰酸酯、异佛尔酮二异氰酸酯、二环己基甲烷4,4’-二异氰酸酯等。其中,优选至少含有4,4’-二苯基甲烷二异氰酸酯(MDI)。
在汽车用途、淡色系用途等需要耐光性的情况下,优选将4,4’-二苯基甲烷二异氰酸酯与脂肪族二异氰酸酯、脂环族二异氰酸酯并用。
另外,作为多异氰酸酯,为碳原子数4~10的直链型脂肪族二异氰酸酯,优选含有该碳原子数4~10的直链型脂肪族二异氰酸酯10~50摩尔%,更优选含有20~40摩尔%。通过含有碳原子数4~10的直链型脂肪族二异氰酸酯10~50摩尔%,可发挥更良好的固化性。作为碳原子数4~10的直链型脂肪族二异氰酸酯,优选1,5-五亚甲基二异氰酸酯、1,6-六亚甲基二异氰酸酯。
关于制成本实施方式的聚氨酯预聚物时的多元醇与多异氰酸酯的比率,优选多异氰酸酯成分的异氰酸酯基当量相对于全部多元醇成分的羟基当量之比为1.33~5.0,更优选为1.5~3.0。如果NCO/OH为1.33~5.0,则柔软性和与基材A的剥离强度均更良好。
本实施方式的聚氨酯预聚物作为配混成分可以配混官能团数为3~5的具有末端异氰酸酯基的多异氰酸酯交联剂。从固化性和与基材的密合性的角度考虑,优选相对于聚氨酯预聚物100质量份含有该多异氰酸酯交联剂30质量%以下,更优选含有2~20质量%。
本实施方式的聚氨酯预聚物的制造方法没有特别限定。例如,在上述的多元醇中混合多异氰酸酯,使NCO/OH为1.33~5.0,在80~120℃下反应60~120分钟左右可制造。
要说明的是,聚氨酯预聚物中根据需要可以适量配混多官能基多异氰酸酯、热塑性聚合物、增粘树脂、催化剂、颜料、抗氧化剂、紫外线吸收剂、表面活性剂、阻燃剂、填充剂、发泡剂等。
(基材)
作为基材A,可使用以往公知的合成人造革的基材,例如可列举包含斜纹组织、平纹组织等的织物、将该织物的棉布进行机械起毛得到的起毛布、人造丝布、尼龙布、聚酯布、凯夫拉布、无纺布(聚酯、尼龙、各种胶乳)、各种膜、片等。
设置聚氨酯发泡层前的基材A优选为含水基材A。即,基材A预先含水,由此聚氨酯发泡层的形成变得容易,同时容易控制聚氨酯发泡层向基材的侵入程度,它们的密合性进一步提高。
含水基材A的含水率优选为10~70质量%,更优选为15~50质量%。通过含水率为10~70质量%,可控制发泡速度和发泡密度,可制作柔软性良好且具有与基材的优异的密合性的合成人造革。
基材A是厚度为1000μm的聚酯基布、聚氨酯发泡层的厚度为200μm时的用于由基材A剥离聚氨酯发泡层的剥离力优选为1.5kgf/inch以上,更优选为2.0kgf/inch以上。通过为1.5kgf/inch以上,例如可得到作为发泡合成人造革超过在实用上没有问题的水准的与基材A的密合性(剥离强度)。剥离力的测定可通过实施例的“剥离强度试验”中记载的方法测定。
另外,多孔结构体的聚氨酯发泡层中,优选在没有形成基材A的一侧设置基材B。此时的基材B例如相当于表皮层,可列举溶剂系聚氨酯、水系聚氨酯、TPU等表皮层形成用涂料所形成的物质,没有特别限定。
基材A为由可进行含水处理的材料形成即可,对厚度没有特别限定。另外,对基材B的厚度也没有特别限定,作为不损害所制作的合成人造革的手感的厚度,优选为0.01~0.2mm,更优选为0.02~0.1mm。
(聚氨酯发泡层)
将上述具有异氰酸酯基的聚氨酯预聚物发泡而成的聚氨酯发泡层的密度从兼顾良好的柔软性和大的剥离强度的角度考虑,为0.10g/cm3~0.60g/cm3,优选为0.2g/cm3~0.5g/cm3。发泡层的密度可通过实施例中记载的方法测定。
聚氨酯发泡层的厚度优选为0.05~1.0mm,更优选为0.1~0.8mm。
如上所述,具有本实施方式的聚氨酯预聚物(湿气固化型聚氨酯预聚物)在湿气固化时发泡所形成的聚氨酯发泡层的本实施方式的多孔层结构体适用于鞋、服装、包、家具、汽车内装材料(例如仪表板、门、控制台、座椅垫)、隔热材料、吸声材料、冲击吸收材料等。
[2.多孔层结构体的制造方法]
本实施方式的多孔层结构体的制造方法包含:对基材A实施含水处理,制成含水基材A的基材含水处理步骤、将具有异氰酸酯基的聚氨酯预聚物涂布在基材B上形成聚氨酯预聚物涂膜的聚氨酯预聚物涂布步骤、将前述含水基材A和在前述基材B上形成的聚氨酯预聚物涂膜贴合,制作涂膜结构体的涂膜结构体制作步骤、对涂膜结构体实施陈化处理的陈化处理步骤。
以下对各步骤进行说明。
(基材含水处理步骤)
例如,以卷对卷方式制作多孔层结构体时,作为含水处理步骤一边将卷状的基材A抽出,一边使其通过装有水的浸渗槽的水中。由此,使基材A中浸渗水。在浸渗槽中浸渗的时间因基材A的材质而不同,作为使该基材中充分吸收水分的时间,例如优选为5~60秒左右。然后,使其在2个辊间通过,由此除去不需要的水,作为含水基材A。此时,通过调节2个辊间的间隙可调节含水率。然后,为了与涂布了聚氨酯预聚物的基材B贴合,将含水基材A向位于下游的例如层压辊侧抽出。
要说明的是,对于含水处理步骤,除了使基材A通过装有水的浸渗槽的水中的方法以外,与蒸汽、雾气接触的方法也可以。
(聚氨酯预聚物涂布步骤)
例如,在抽出作为表皮的辊状的基材B的同时,将收纳于熔化器等的聚氨酯预聚物涂布于该基材B,形成聚氨酯预聚物涂膜。在此,由于聚氨酯预聚物不含水分,因此在涂膜形成后几乎不发泡。另外,从贮存期的角度考虑也是有效的。
要说明的是,聚氨酯预聚物如已经说明的,具有异氰酸酯基、实质上不含挥发成分、满足已经说明的(a)~(c)的至少任一组成。该聚氨酯预聚物收纳于熔化器等,为聚氨酯预聚物涂布步骤中的涂布所准备。
聚氨酯预聚物涂膜的厚度因聚氨酯预聚物的粘度、组成而不同,优选为50~500μm,更优选为100~300μm。
形成聚氨酯预聚物涂膜的基材B为了与含水基材A贴合,例如向层压辊侧抽出。
(涂膜结构体制作步骤)
为了将形成在基材B上的聚氨酯预聚物涂膜贴合于基材A,例如向包含1对辊的层压辊抽出含水基材A与基材B,在此层压,由此制作涂膜结构体。然后,卷成卷状,送至用于进行发泡处理的陈化处理步骤。
(陈化处理步骤)
陈化处理步骤中,卷状的涂膜结构体在15~80℃、40~95%RH的状态下保持48~120小时,进行陈化处理。通过该陈化处理,发生发泡,制作本实施方式的多孔层结构体。
(水蒸气接触步骤)
另外,本制造方法中,在涂膜结构体制作步骤与陈化处理步骤之间,优选含有使水蒸气与涂膜结构体接触的水蒸气接触步骤。水蒸气接触步骤中,使气氛为30~60℃(优选35~55℃)、80%RH以上(优选85%RH以上),在该气氛中的时间因温度条件、湿度条件而不同,优选为20秒以上(优选25~60秒)。
通过水蒸气接触步骤,可提高涂膜结构体的含水率,因此其后的陈化处理步骤中容易得到良好的发泡倍率。即,可良好地控制发泡程度。
在以上那样的步骤中,在形成聚氨酯预聚物的涂膜后不发泡。因此,在没有发泡(即泡)的状态下进行其后的贴合。结果,可在基材与聚氨酯发泡层之间达成高的密合性。并且,在陈化处理步骤中进行了充分的发泡,因此在维持高密合性的同时形成柔软性良好的聚氨酯发泡层。
本实施方式的多孔层结构体如上所述可发挥良好的柔软性和与基材A的密合性(剥离力),认为这是由于下述的结构导致的。
即,首先,不通过本发明的制造方法制作的以往的多孔层结构体20如图2所示,处于基材A22与基材B26之间的聚氨酯发泡层24的下表面24A几乎没有侵入基材A22侧。这是由于在以往的方法中涂布发泡了的聚氨酯预聚物后,与没有进行特别事前处理(例如含水处理)的基布贴合,因此聚氨酯发泡层24与基材A22的密合性没有本发明大。
另一方面,通过本发明的制造方法制作的多孔层结构体10如图1所示,位于基材A12和基材B16之间的聚氨酯发泡层14的下表面14A适当地侵入基材A12侧,因此由于锚固效果聚氨酯发泡层14和基材A12的密合性非常大。
从利用锚固效果得到的良好的密合性的角度考虑,作为发泡层向基材A侵入的程度,优选相对于基材A的厚度从表面至少侵渗大概10%以上发泡层。如果侵入程度小于10%,则不充分表现密合性。但是,以发泡层占基材A的厚度的大半的程度侵渗的情况下,产生有损柔软性或者不充分表现密合性等的不良情况。适当的侵渗程度因基材A的种类而不同,这通过贴合步骤前的基材A的含水处理来控制。
要说明的是,多孔层结构体可直接用作合成人造革,但是也可以适当进行例如表面处理剂的涂布、与其它基材的贴合等处理。
实施例
下面,通过实施例和比较例进一步详细说明本发明。但是本发明不受实施例等的限定。要说明的是,数均分子量通过GPC(聚苯乙烯换算)测定。
[实施例1~41、比较例1~34]
(聚氨酯预聚物的合成)
在带有搅拌器、温度计、气体导入口等的500毫升的玻璃制反应容器中以下表2~10所示的各配混量加入下表1所示的多元醇,加热・减压进行脱水处理后,封入氮气,在内温100℃下搅拌后,加入MDI规定量(NCO/OH=1.3~5.0),搅拌反应120分钟,得到聚氨酯预聚物。
[表1]
要说明的是,凝胶点如下所述测定。
首先,确认样品(多元醇)的不挥发成分后,用DMF(水分0.03质量%以下)调节至10质量%溶液,用螺旋浆搅拌器搅拌,得到均匀的DMF溶液。
将10g该DMF采取到300ml的三角烧瓶中,进一步加入DMF 90g,用磁力搅拌器搅拌均匀,得到1质量%DMF溶液100g。将该溶液在25±1℃的温度条件下持续搅拌的同时用滴定管滴加蒸馏水,将白浊消失的滴加量(微微白浊时的水滴加量:ml)作为凝胶点。
要说明的是,DMF使用以不吸收水分的方式保存的试剂1级品。
(表皮的制作)
将合成人造革用的溶剂型聚氨酯树脂レザミンNE-8875-30(大日精化工业株式会社)、作为合成人造革用着色剂的セイカセブンBS-780(大日精化工业株式会社)、作为稀释溶剂的甲基乙基酮和二甲基甲酰胺混合,用刮棒涂布机以250μm/wet的涂布量在脱模纸上均匀涂布后,在120℃干燥5分钟,得到膜厚40~50μm的带表皮的膜(基材B)。
(合成人造革的制作)
在形成于上述脱模纸上的表皮上涂布加热至100℃的聚氨酯预聚物,以形成涂布膜厚度为100μm的涂膜,将进行或未进行含水处理的基布(基材A)用层压辊加热压接,从而制作涂膜结构体。作为陈化处理步骤,在温度25℃、相对湿度65%的环境下保持120小时,将涂膜结构体熟化。剥离脱模纸,制成评价用合成人造革。对其进行下述评价。结果示于下表。
要说明的是,基布使用织物(聚酯的圆型针织聚氨酯基布、厚度10mm)。含水处理通过使水浸渗于基布后,用适当调节了辊间隔的轧液机进行均匀的挤压操作而进行。另外,通过调节轧液机的辊间隔得到所需的含水率。
(发泡程度评价:发泡层的密度)
用各聚氨酯预聚物制作评价用合成人造革后,将该合成人造革切成10cm×10cm见方,另外将含水处理前的基材A切成10cm×10cm、将在脱模纸上形成的表皮切成10cm×10cm,由脱模纸剥离,通过下式算出发泡层的密度。
(1)合成人造革的重量测定・计算:
由合成人造革整体的重量:a、基材A的重量:b、表皮层的重量:c通过下式算出发泡层的重量。
发泡层的重量:d=a-b-c
(2)合成人造革的厚度测定・计算:
由合成人造革整体的厚度:e、基材A的厚度:f、表皮层的厚度:g通过下式求出发泡层的厚度。
发泡层的厚度:h=e-f-g
(3)发泡层的密度计算:通过下式求出发泡层的密度。
发泡层的密度=d÷h×10×10(g/cm 3)
要说明的是,通过发泡层的密度为0.10g/cm 3~0.60g/cm 3,可兼顾良好的柔软性和大的剥离强度。
(剥离强度试验)
在评价用合成人造革上热压接宽度17mm的聚氨酯系HM带后,制作25mm宽的长条状测定样品,用AGS-J(岛津制作所)以200mm/min的速度拉伸,测定粘接强度,为1.5kgf/inch以上时判断为得到作为发泡合成人造革超过在实用上没有问题的水平的与基材A的密合性(剥离强度)。
(耐水解试验)
将聚氨酯预聚物涂布在脱模纸上,使膜厚为40~50μm,在25℃/60RH%的气氛中熟化120小时,作为耐水解试验中使用的膜。将剥离了脱模纸的膜置于70℃/95RH%的气氛中,每周进行耐久试验,进行7周,用AGS-J(岛津制作所)进行拉伸强度试验。评价指标如下:
维持断裂强度保持率50%以上的时间:1~4周 ×
维持断裂强度保持率50%以上的时间:5~6周 〇
维持断裂强度保持率50%以上的时间:7周以上 ◎
要说明的是,〇和◎为合格。
[是否合格的判定]
各表中,将发泡层的密度为0.1~0.6g/cm3、且符合剥离强度的基准(1.5kgf/inch以上)的作为〇、将发泡层的密度不是0.1~0.6g/cm 3或者不符合剥离强度的基准的作为×,显示判定结果。
[表2]
[表3]
[表4]
由表2~4可知,本实施例具有良好的发泡程度。
[表5]
[表6]
由表5、6可知,通过基材的含水率为15~50质量%,得到良好的发泡程度和剥离强度。
[表7]
[表8]
由表7、8可知,通过贴合后的水蒸气处理(水蒸气接触步骤)发泡程度提高。但是,即使是最容易发泡的亲水性强的级别中,如果基布不含水,则即使贴合后进行水蒸气处理,也未充分发泡。
[表9]
由表9可知,通过聚氨酯预聚物含有全部多元醇成分中50质量%以上的聚碳酸酯多元醇成分,耐水解性变得良好。
[表10]
由表10可知,即使基材的含水率相同,通过NCO/OH比为1.33~5,得到良好的发泡程度和剥离强度。
符号说明
10 多孔层结构体
12 基材A
14 聚氨酯发泡层
16 基材B。
Claims (7)
1.多孔层结构体,其是包含基材A、设置在该基材A上的聚氨酯发泡层的多孔层结构体,
前述聚氨酯发泡层为将具有异氰酸酯基的聚氨酯预聚物发泡而成的发泡层,
前述聚氨酯发泡层的密度为0.10~0.60g/cm3,
前述聚氨酯预聚物实质上不含挥发成分,满足下述(A)~(C)中的至少任一组成,
(A) 含有全部多元醇成分中的50质量%以上的凝胶点为20ml以上且小于30ml的多元醇成分(a)的组成,
(B) 含有全部多元醇成分中的30质量%以上的凝胶点为30ml以上且小于50ml的多元醇成分(b)的组成,
(C) 含有全部多元醇成分中的10质量%以上的凝胶点为50ml以上的多元醇成分(c)的组成。
2.根据权利要求1所述的多孔层结构体,其中,设置前述聚氨酯发泡层前的前述基材A为含水基材A。
3.根据权利要求1或2所述的多孔层结构体,其中,前述基材A为聚酯基布,聚氨酯发泡层的厚度为200μm时的用于由基材A剥离聚氨酯发泡层的剥离力为1.5kgf/inch以上。
4.根据权利要求1~3中任一项所述的多孔层结构体,其中,前述聚氨酯预聚物含有全部多元醇成分中的50质量%以上的聚碳酸酯多元醇成分。
5.根据权利要求1~4中任一项所述的多孔层结构体,其中,前述聚氨酯预聚物中,多异氰酸酯成分的异氰酸酯基当量相对于前述全部多元醇成分的羟基当量之比为1.33~5.0。
6. 权利要求1~5中任一项所述的多孔层结构体的制造方法,其包含:
对基材A实施含水处理,制成含水基材A的基材含水处理步骤、
将具有异氰酸酯基的聚氨酯预聚物涂布在基材B上形成聚氨酯预聚物涂膜的聚氨酯预聚物涂布步骤、
将前述含水基材A和在前述基材B上形成的前述聚氨酯预聚物涂膜贴合,制作涂膜结构体的涂膜结构体制作步骤、
对前述涂膜结构体实施陈化处理的陈化处理步骤,
前述聚氨酯预聚物实质上不含挥发成分,满足下述(A)~(C)中的至少任一组成,
(A) 含有全部多元醇成分中的50质量%以上的凝胶点为20ml以上且小于30ml的多元醇成分(a)的组成,
(B) 含有全部多元醇成分中的30质量%以上的凝胶点为30ml以上且小于50ml的多元醇成分(b)的组成,
(C) 含有全部多元醇成分中的10质量%以上的凝胶点为50ml以上的多元醇成分(c)的组成。
7.根据权利要求6所述的多孔层结构体的制造方法,其中,在前述涂膜结构体制作步骤与前述陈化处理步骤之间,包含使水蒸气与前述涂膜结构体接触的水蒸气接触步骤。
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CN1334832A (zh) * | 1998-12-29 | 2002-02-06 | 陶氏化学公司 | 由机械发泡聚氨酯分散体制备的聚氨酯泡沫材料 |
CN1406298A (zh) * | 2000-02-28 | 2003-03-26 | 松本油脂制药株式会社 | 多孔结构的制造方法 |
JP2003246830A (ja) * | 2002-02-25 | 2003-09-05 | Dainippon Ink & Chem Inc | 耐久性に優れた無溶剤型湿気硬化性ホットメルトウレタン樹脂組成物、発泡体、及びそれを用いたシート構造体 |
JP2003306526A (ja) * | 2002-04-15 | 2003-10-31 | Dainippon Ink & Chem Inc | 無溶剤型湿気硬化性ホットメルトウレタン樹脂組成物、発泡体及びそれを用いたシート構造体 |
CN1732082A (zh) * | 2002-12-27 | 2006-02-08 | 株式会社加平 | 聚氨酯发泡体薄片以及使用它的层叠体薄片的制造方法 |
CN103483529A (zh) * | 2012-06-11 | 2014-01-01 | 株式会社德成 | 聚氨酯发泡片材的制造方法以及使用其的皮革样片材状物 |
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EP3858614A4 (en) | 2022-06-08 |
US11840802B2 (en) | 2023-12-12 |
TWI801668B (zh) | 2023-05-11 |
US20220034027A1 (en) | 2022-02-03 |
JP7094849B2 (ja) | 2022-07-04 |
WO2020066920A1 (ja) | 2020-04-02 |
CN112703112B (zh) | 2022-12-27 |
MX2021003371A (es) | 2021-05-27 |
JP2020049732A (ja) | 2020-04-02 |
EP3858614A1 (en) | 2021-08-04 |
TW202023808A (zh) | 2020-07-01 |
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