CN117487122B - 聚氨酯发泡体系、可热回收聚氨酯泡沫及其制备方法 - Google Patents
聚氨酯发泡体系、可热回收聚氨酯泡沫及其制备方法 Download PDFInfo
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- CN117487122B CN117487122B CN202311841302.7A CN202311841302A CN117487122B CN 117487122 B CN117487122 B CN 117487122B CN 202311841302 A CN202311841302 A CN 202311841302A CN 117487122 B CN117487122 B CN 117487122B
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- isocyanate
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Classifications
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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
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
- C08J11/18—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material
- C08J11/22—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material by treatment with organic oxygen-containing compounds
- C08J11/24—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material by treatment with organic oxygen-containing compounds containing hydroxyl groups
-
- 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
- C08G18/08—Processes
- C08G18/16—Catalysts
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Abstract
本发明属聚氨酯泡沫领域,涉及聚氨酯发泡体系、可热回收聚氨酯泡沫及其制备方法。聚氨酯发泡体系含:平均官能度为1.7‑2.4的异氰酸酯反应性组分,其含分子量高于500 g/mol的多元醇;选自基于胺的催化剂和基于有机金属化合物的催化剂中的一种或多种催化剂;硅氧烷基表面活性剂;水;任选的官能度为2的扩链剂和/或官能度为3或以上的交联剂;和任选的添加剂;与平均官能度为1.9‑2.4的异氰酸酯组分,其含多异氰酸酯和/或异氰酸酯基团封端的预聚物,预聚物由多异氰酸酯与含两个或更多个羟基的化合物反应制备,三环聚亚甲基多苯基异氰酸酯重量与多异氰酸酯总重量的比不高于5.00%。聚氨酯泡沫可通过热处理方式回收。
Description
技术领域
本发明属于聚氨酯泡沫领域,涉及聚氨酯发泡体系、可热回收聚氨酯泡沫及其制备方法。
背景技术
在自然条件下,目前使用的绝大多数塑料等高分子材料均不可降解,对环境造成巨大破坏。随着温室效应、污染等环境危机的日益恶化,环境保护刻不容缓,许多国家已立法限制使用一次性非降解塑料,提倡使用可降解聚合物或回收聚合物制作的产品。
聚氨酯因其独特的结构和优异的性能,以泡沫、弹性体、胶黏剂等形式广泛应用于建筑材料、交通运输与消费品等领域。通常,聚氨酯泡沫由于结构中存在较高程度的交联呈热固性。
目前回收聚氨酯的方法有物理回收、焚烧回收和化学回收。包含发泡热塑性聚氨酯在内的热塑性聚氨酯适合物理回收方法。通常的非热塑性聚氨酯泡沫由于其热固性难以通过热熔融等物理回收方式被回收。焚烧回收又会产生大量二氧化碳。同时,聚氨酯泡沫内大量存在的化学交联导致其化学降解耗能耗时。
WO 2022194985 A1公开了一种两步法工艺以生成部分交联的含聚氨酯泡沫。
WO 2022096599 A1公开了一种包含聚氨酯-聚脲的水发泡泡沫,其按ISO 845测量的表观密度为30-700 kg/m3和拉伸强度(按DIN 53504测量)与表观密度的比为至少10 kPam3/kg。
US 20220363858 A1公开了一种用于制备热塑性聚氨酯软质泡沫的反应性混合物和方法,该泡沫具有主要为开孔的结构(基于泡沫的总体积计算并根据ASTM D6226-10测量的开孔含量≥50体积%)和低于200 kg/m3的表观密度。
因此,需要开发一种聚氨酯泡沫,其可通过热处理方式回收。
发明内容
为此,本发明提供了一种聚氨酯发泡体系,包含:
a) 平均官能度为1.7-2.4的异氰酸酯反应性组分,其包含,
分子量高于500 g/mol的一种或多种多元醇;
催化剂,其选自基于胺的催化剂和基于有机金属化合物的催化剂中的一种或多种;
硅氧烷基表面活性剂;
水;
任选存在的官能度为2的扩链剂和/或官能度为3或以上的交联剂;
和
任选存在的添加剂;与
b) 平均官能度为1.9-2.4的异氰酸酯组分,其包含多异氰酸酯和/或异氰酸酯基团封端的预聚物,预聚物由多异氰酸酯与含两个或更多个羟基的化合物反应制备,异氰酸酯组分中三环聚亚甲基多苯基异氰酸酯重量与所述多异氰酸酯总重量的比不高于5.00%。
可选的,所述异氰酸酯反应性组分与所述异氰酸酯组分具有70-120的异氰酸酯指数。
可选的,所述异氰酸酯组分具有1.95-2.30的平均官能度。
可选的,所述异氰酸酯组分具有20重量%至48.2重量%的NCO含量。
可选的,所述异氰酸酯组分中三环聚亚甲基多苯基异氰酸酯与四环聚亚甲基多苯基异氰酸酯的重量比为(2-4):1。
可选的,所述异氰酸酯反应性组分中官能度为4或以上的多元醇含量不高于80重量%,基于所述异氰酸酯反应性组分的总重量。
可选的,所述水占所述异氰酸酯反应性组分的1重量%至5重量%。
可选的,所述交联剂占所述异氰酸酯反应性组分0.5重量%至10重量%。
可选的,所述添加剂选自物理发泡剂、链调节剂、润滑剂、防腐剂、颜料或染料、增韧剂或抗冲改性剂、抗静电剂、流平剂、增塑剂、阻燃剂、成膜剂、抗氧化剂、蜡、抗紫外线添加剂、稳定剂、增稠剂、润湿剂、填料中的一种或多种。
本发明还提供了一种可热回收聚氨酯泡沫,其由上述聚氨酯发泡体系制备。
可选的,所述可热回收聚氨酯泡沫具有低于250 °C的熔融温度。
可选的,所述可热回收聚氨酯泡沫具有30-300 g/L的自由上升密度。
可选的,所述可热回收聚氨酯泡沫具有不低于50%的球回弹率。
可选的,所述可热回收聚氨酯泡沫具有1-30 s的恢复时间与在25%挠度时30-150N的压陷硬度。
本发明还提供了一种可热回收聚氨酯泡沫的制备方法,其包括,
a) 提供聚氨酯发泡体系;与
b) 让所述聚氨酯发泡体系聚合并发泡。
本发明提供的聚氨酯发泡体系可选择多种不同的多元醇和多异氰酸酯,采用水作为发泡剂,配方简单。聚氨酯泡沫制备方法为一步法,无需额外的发泡步骤或复杂的高压设备。聚氨酯发泡体系的异氰酸酯组分中三环聚亚甲基多苯基异氰酸酯重量与所述多异氰酸酯总重量的比不高于5.00%,由聚氨酯发泡体系制备的泡沫能够在200℃下熔融,因此可以通过热处理回收。
具体实施方式
下面对本发明进行详细描述。应当理解,本发明可以以许多不同的方式来实施,并且不应被解释为限于本文所阐述的实施方式。
除非另外说明,本文中使用的所有技术和科学术语具有本发明所属领域技术人员通常理解的含义。除非另有说明,本文所使用的下列术语具有下面赋予它们的含义。
如本文所使用的,冠词“一个”和“一种”是指物品或组件的一个或多于一个(即,至少一个)的语法宾语。
如本文所使用的,术语“包括”与“包含”等可以互换使用,并且应当以非限制性、开放的方式解释。也就是说,例如可以存在另外的部件或元件。表述“由……组成”或“基本上由……组成”或同源词可以包含在“包括”或同源词内。
除非另有说明,所有百分比(%)均为“重量百分比”。
除非另有说明,各组分或聚合物的分子量是指数均分子量(Mn)。
在本发明中,各组分的分子量按照GB/T 21863-2008采用凝胶渗透色谱(GPC)测定。
术语“聚氨酯体系”与“聚氨酯发泡体系”是指用于制备聚氨酯如聚氨酯泡沫的反应性化合物的组合,其中异氰酸酯组分通常保存在与异氰酸酯反应性组分不同的一个或多个容器中。
术语“聚氨酯”不限于仅包含氨基甲酸酯的那些聚合物。聚氨酯领域的技术人员充分理解,聚氨酯还可包含脲键、脲基甲酸酯、碳二亚胺、尿丁啶二酮和除氨基甲酸酯键之外的其它键。聚氨酯也包括聚氨酯-脲。
术语“热塑性(thermoplastic)”被定义为聚合物的一种性质,热塑性聚合物可以在较高的温度下熔化或软化而在多次加热-冷却的工艺中被加工为不同形状的制品而不发生明显的降解或化学反应。
术语“热固性(thermosetting)”被定义为聚合物的一种性质,当加热时,热固性聚合物发生化学反应,如降解或变质。这一特点使它们几乎不能在熔融温度下再加工。
术语“熔融乳化(melt-emulsifiable)”定义如下:分散的另一种方式,熔化预形成的聚合物,然后将熔融聚合物与多元醇在剪切下混合。剪切作用将熔融聚合物破裂成分散于多元醇相中的小液滴。
本发明中,异氰酸酯反应性组分的“表观官能度”是指组分中每个分子的平均官能度,即每个分子异氰酸酯反应性基团(如羟基)的平均数量。
本发明中,异氰酸酯组分的“表观官能度”是指组分中每个分子的平均官能度,即每个分子异氰酸酯基团的平均数量。
“NCO含量”或“异氰酸酯基团含量”,以重量百分比计,指异氰酸酯组分中以异氰酸酯基团(NCO)计的重量占异氰酸酯组分的总重量。NCO含量可以通过滴定等方法按照DIN ENISO 14896测量。
术语“异氰酸酯反应性氢原子”是指存在于异氰酸酯反应性组分中的羟基和胺基中的活性氢原子的总数。作为示例,一个羟基被认为包含一个反应性氢原子,一个伯胺基被认为包含一个反应性氢原子,一个水分子被认为包含两个活性氢原子。
本发明中,聚氨酯体系的“异氰酸酯指数”定义为反应中使用的异氰酸酯组分的异氰酸酯基团总数与异氰酸酯反应性组分中异氰酸酯反应性氢原子总数的比值,以百分比表示。异氰酸酯指数为100意味着对于异氰酸酯组分的每个异氰酸酯基团,在具有至少两个异氰酸酯反应性含氢基团的化合物和扩链剂中存在有一个活性氢原子,即存在一个对异氰酸酯具有反应性的官能团。异氰酸酯指数高于100意味着异氰酸酯基团多于异氰酸酯反应性基团。
除非另有说明,术语“平均”是指数均。
聚氨酯发泡体系
本发明的聚氨酯发泡体系是一种多组分反应性体系,其包含异氰酸酯组分与异氰酸酯反应性组分,在一些情况下,可进一步包含第三组分。在使用前,聚氨酯发泡体系的组分被分别储存在不同的容器如液罐、液槽或罐车内。需要制备聚氨酯泡沫时,各组分被混合以反应生成聚氨酯。
聚氨酯发泡体系中,异氰酸酯反应性组分与异氰酸酯组分优选具有70-120的异氰酸酯指数,例如75、80、85、90、95、100、105、110与115等;更优选具有80-110的异氰酸酯指数,例如85、90、95、100与105。
异氰酸酯组分
在本发明中,用于形成聚氨酯的组分可以包含异氰酸酯组分,其平均官能度为1.9-2.4。异氰酸酯组分包含多异氰酸酯和/或异氰酸酯基团封端的预聚物,该预聚物由多异氰酸酯与含活性氢原子化合物反应制备。异氰酸酯组分中三环聚亚甲基多苯基异氰酸酯重量与多异氰酸酯总重量的比不高于5.00%,优选不高于3.75%,更优选不高于2.50%。当异氰酸酯组分含有由多异氰酸酯与含活性氢原子化合物反应制备的预聚物时,多异氰酸酯总重量应仅仅由含异氰酸酯基团的起始原料重量计算得到,而不考虑含活性氢原子化合物的重量。
异氰酸酯可以包括已知用于生产聚氨酯的所有异氰酸酯。这些异氰酸酯包括脂族、脂环族、芳脂族和/或芳族异氰酸酯,例如三-、四-、五-、六-、七-和/或八亚甲基二异氰酸酯、2-甲基五亚甲基1,5-二异氰酸酯、2-乙基亚丁基1,4-二异氰酸酯、1,5-五亚甲基二异氰酸酯、1,4-亚丁基二异氰酸酯、1-异氰酸基-3,3,5-三甲基-5-异氰酸酯基甲基环己烷(异佛尔酮二异氰酸酯,IPDI)、1,4-和/或1,3-双(异氰酸酯基甲基)环己烷(HXDI)、1,4-环己烷二异氰酸酯、1-甲基环己烷2,4-和/或2,6-二异氰酸酯和/或二环己基甲烷4,4’-、2,4’-和2,2’-二异氰酸酯、包括二苯基甲烷2,2’-、2,4’-和/或4,4’-二异氰酸酯的二苯基甲烷二异氰酸酯(MDI)、包括三环/四环聚亚甲基多苯基异氰酸酯(三环聚MDI与四环聚MDI)在内的聚亚甲基多苯基异氰酸酯(聚合MDI)、1,5-萘二异氰酸酯(NDI)、2,4-和/或2,6-甲苯二异氰酸酯(TDI)、3,3’-二甲基二苯基二异氰酸酯、1,2-二苯基乙烷二异氰酸酯和/或苯二异氰酸酯、或其混合物。
优选地,异氰酸酯组分具有1.95-2.30的平均官能度,更优选具有2.02-2.23的平均官能度。
优选地,异氰酸酯组分具有20重量%至48.2重量%的NCO含量。
聚亚甲基多苯基异氰酸酯的结构如式I,其中,亚甲基CH2在其所连接的苯环上相对异氰酸酯基团NCO的位置可为邻位或对位,n为不小于1的整数。当n为1时对应三环聚亚甲基多苯基异氰酸酯;n为2时对应四环聚亚甲基多苯基异氰酸酯。三环和四环聚亚甲基多苯基异氰酸酯的含量可以通过高效液相色谱(HPLC)方法测定。
式I
聚合二异氰酸酯通常具有较高的表观官能度,其会导致聚氨酯中形成较高程度的交联。
优选地,异氰酸酯组分中三环聚亚甲基多苯基异氰酸酯与四环聚亚甲基多苯基异氰酸酯的重量比为(2-4):1。
异氰酸酯反应性组分
异氰酸酯反应性组分的平均官能度为1.7-2.4,其包含,
分子量高于500 g/mol的一种或多种多元醇;
催化剂;
表面活性剂;
水;
任选存在的官能度为2的扩链剂;
任选存在的官能度为3或以上的交联剂;与
任选存在的添加剂。
异氰酸酯反应性组分中,官能度为4或以上的多元醇含量优选不高于80重量%,更优选不高于60重量%,进一步优选不高于40重量%,基于异氰酸酯反应性组分的总重量。
优选地,水占异氰酸酯反应性组分的1重量%至5重量%,例如1.0重量%、1.5重量%、2.0重量%、2.5重量%、3.0重量%、3.5重量%、4.0重量%、4.5重量%与5.0重量%;更优选地,水占异氰酸酯反应性组分的2重量%至4重量%。
多元醇
在本发明中,异氰酸酯反应性组分包含多元醇。多元醇可具有500至20,000 g/mol、优选600至15,000 g/mol、更优选1,000至10,000 g/mol的数均分子量(Mn)。多元醇具有大于1的表观官能度。
所述多元醇可以是聚氨酯制备中常用的多元醇,例如聚醚多元醇、聚酯多元醇如聚己内酯多元醇、聚碳酸酯多元醇及其组合,优选聚醚多元醇。
本发明中的多元醇可以通过本领域已知的方法制备或者可以商购获得。
在本发明的一个实施方案中,所述多元醇可以选自衍生自包含2至6个碳原子,例如3、4、5或6个碳原子的含氧杂环化合物的聚醚多元醇,优选烷基环氧乙烷。优选地,所述多元醇通过将环氧乙烷和甲基环氧乙烷作为重复单元聚合来制备,优选用仲羟基封端。
在本发明的一个优选实施方案中,所述多元醇选自衍生自环氧化物、优选环氧乙烷、环氧丙烷或其混合物的聚醚多元醇。
在本发明的一个实施方案中,所述多元醇可以选自聚酯多元醇,包括例如由具有2至12个碳原子、优选4至6个碳原子的二羧酸和多元醇获得的聚酯多元醇。合适的二羧酸包括但不限于:脂族二羧酸,例如琥珀酸、戊二酸、己二酸、辛二酸、壬二酸和癸二酸;或者芳香族二羧酸,例如邻苯二甲酸、间苯二甲酸和对苯二甲酸。所述二羧酸可以单独使用或作为混合物使用,例如作为琥珀酸、戊二酸和己二酸的混合物使用。为了制备聚酯多元醇,还可以任选地使用相应的二羧酸衍生物,例如醇残基中具有1至4个碳原子的羧酸二酯、酸酐或酰基氯来代替二羧酸。合适的多元醇的实例包括具有2至10个碳原子、优选2至6个碳原子的二醇,例如乙二醇、二乙二醇、1,4-丁二醇、1,5-戊二醇、1,6-己二醇、1,10-己二醇、2,2-二甲基-1,3-丙二醇、1,3-丙二醇或二丙二醇。根据所需的性能,所述聚酯多元醇可以单独使用或作为混合物使用。优选的聚酯多元醇包括聚(乙二醇己二酸酯)、聚(1,4-丁二醇己二酸酯)、聚(乙二醇/1,4-丁二醇己二酸酯)、聚(1,6-己二醇/新戊二醇己二酸酯)、聚(1,6-己二醇/1,4-丁二醇己二酸酯)和聚己内酯、ω-羟基羧酸例如ω-羟基己酸的缩合产物或内酯例如任选取代的ω-己内酯的聚合产物。
在本发明的一个实施方案中,所述多元醇可以选自衍生自碳酸和二醇的聚碳酸酯多元醇,尤其是具有4至6个碳原子的二醇,例如1,4-丁二醇或1,6-己二醇。
扩链剂
在本发明中,任选地,异氰酸酯反应性组分包含官能度为2的扩链剂。
可以使用的扩链剂是分子量优选小于500 g/mol、特别优选在60至400 g/mol范围内的物质,其具有2个对异氰酸酯有反应性的氢原子。这些扩链剂可以单独使用或以混合物的形式使用。优选使用分子量小于500 g/mol、特别是60至400 g/mol、尤其特别是60至350g/mol的二醇。可以使用的实例为具有2至14个、优选2至10个碳原子的脂族、环脂族和/或芳脂族二醇,例如乙二醇、1,3-丙二醇、1,4-丁二醇、1,6-己二醇、1,10-癸二醇、1,2-、1,3-和1,4-二羟基环己烷、二甘醇、二丙二醇、三丙二醇、乙二胺或1,3-丙二胺。优选使用乙二醇、1,3-丙二醇或1,4-丁二醇,尤其是1,4-丁二醇。
如存在,扩链剂的用量优选为1重量%至20重量%,更优选3重量%至15重量%,例如3重量%、4重量%、5重量%、6重量%、7重量%、8重量%、9重量%、10重量%、11重量%、12重量%、13重量%、14重量%或15重量%,以异氰酸酯反应性组分的总重量计。
交联剂
在本发明中,任选地,异氰酸酯反应性组分包含官能度为3或以上的交联剂。
可以使用的交联剂是分子量小于500 g/mol的物质,其具有3个或更多个(例如4个)对异氰酸酯有反应性的氢原子。这些交联剂可以单独使用或以混合物的形式使用。优选使用分子量小于500 g/mol、特别是80至400 g/mol、尤其特别是80至350 g/mol的三醇、四醇、三胺、四胺或烷醇胺。可以使用的实例为具有2至14个、优选2至10个碳原子的脂族、环脂族和/或芳脂族三醇、四醇或烷醇胺,例如甘油、二乙醇胺、三乙醇胺、三羟甲基丙烷与季戊四醇。优选使用甘油、二乙醇胺或三羟甲基丙烷,尤其是甘油。
如存在,交联剂的用量优选为0.5重量%至10重量%,更优选1重量%至5重量%,例如1.0重量%、1.5重量%、2.0重量%、2.5重量%、3.0重量%、3.5重量%、4.0重量%、4.5重量%或5.0重量%,以异氰酸酯反应性组分的总重量计。
催化剂
在本发明中,异氰酸酯反应性组分包含催化剂。
对于催化剂,可以使用所有能够加速异氰酸酯和多元醇之间反应的化合物。这些催化剂包括基于胺的催化剂和基于有机金属化合物的催化剂,或它们的混合物。
对于胺基催化剂,可以使用,例如,强碱性胺,诸如N,N,N-三乙基氨基乙氧基乙醇、双(N,N-二甲基氨基乙基)醚、二甲基环己胺、三甲基羟乙基乙二胺、二甲基苄胺、三乙胺、N,N-二甲基-1,3-丙二胺、三亚乙基二胺、五甲基二亚丙基三胺、二甲基乙醇胺、N-甲基咪唑、N-乙基咪唑、四甲基六亚甲基二胺、三(二甲基氨基丙基)六氢三嗪、二甲基氨基丙胺、N-乙基吗啉、二氮杂双环十一碳烯、二氮杂双环壬烯、二氮杂双环辛烷。
对于基于有机金属化合物的催化剂,可以使用,例如,有机锡化合物,诸如有机羧酸的锡(II)盐,如乙酸锡(II)、辛酸锡(II)、乙基己酸锡(II)和月桂酸锡(II),和有机羧酸的二烷基锡(IV)盐,如二乙酸二丁基锡、二月桂酸二丁基锡、马来酸二丁基锡和二乙酸二辛基锡;锌盐或铋盐,如辛酸锌、新癸酸铋、2-乙基己酸铋和辛酸铋;或羧酸的碱金属盐,如乙酸钾或甲酸钾。
如果使用的话,催化剂的用量优选为0.1重量%至2.0重量%,更优选0.5重量%至1.5重量%,以异氰酸酯反应性组分的总重量计。
表面活性剂
本领域中已知的多种表面活性剂都可以用于本发明中。
合适的表面活性剂为例如乳化剂,例如蓖麻油硫酸的钠盐或脂肪酸的钠盐以及脂肪酸与胺的盐,例如油酸二乙胺、硬脂酸二乙醇胺、蓖麻油酸二乙醇胺,磺酸盐,例如十二烷基苯磺酸或二萘基甲二磺酸和蓖麻油酸的碱金属或铵盐;泡沫稳定剂,例如硅氧烷-环氧烷共聚物和其他有机硅氧烷、乙氧基化烷基酚、乙氧基化脂肪醇、石蜡油、蓖麻油酯或蓖麻油酸酯、土耳其红油和花生油,以及泡孔调节剂,例如石蜡、脂肪醇和二甲基聚硅氧烷。具有聚环氧烷和氟代烷烃基作为侧基的低聚聚丙烯酸酯也适合改善乳化作用、泡孔结构和/或其稳定性。基于聚氨酯发泡体系的总重量计,表面活性剂的用量通常为0.01重量%至5重量%。
根据一些实施例,聚氨酯发泡体系中的表面活性剂优选为硅氧烷基表面活性剂。硅氧烷基表面活性剂选自可水解的聚醚-聚硅氧烷嵌段共聚物、不可水解的聚醚-聚硅氧烷嵌段共聚物、氰基烷基聚硅氧烷、聚醚硅氧烷、聚二甲基硅氧烷和聚醚改性二甲基聚硅氧烷。
水
在本发明中,异氰酸酯反应性组分含水。
水在聚氨酯体系中起到化学发泡剂的作用,即与异氰酸酯基团反应,释放二氧化碳以发泡形成聚氨酯泡沫。同时,水可以与异氰酸酯反应生成脲键。
根据一些实施例,水占异氰酸酯反应性组分的1重量%至5重量%,优选2重量%至4重量%。
添加剂
在本发明中,异氰酸酯反应性组分任选地包含添加剂。
可用于本发明的添加剂选自物理发泡剂、链调节剂、润滑剂、防腐剂、颜料或染料、增韧剂或抗冲改性剂、抗静电剂、流平剂、增塑剂、阻燃剂、成膜剂、抗氧化剂、蜡、抗紫外线添加剂、稳定剂、增稠剂、润湿剂、填料中的一种或多种。在制备聚氨酯时,优选使用上述添加剂之一或其混合物。
如存在,所述添加剂的用量通常为聚氨酯发泡体系总重量的0.1至10重量%,例如0.1重量%、0.4重量%、0.7重量%、1.0重量%、1.3重量%、1.6重量%、1.9重量%、2.2重量%、2.5重量%、2.8重量%、3.1重量%、3.4重量%、3.7重量%、4.0重量%、4.3重量%、4.6重量%、4.9重量%、5.2重量%、5.5重量%、5.8重量%、6.1重量%、6.4重量%、6.7重量%、7.0重量%、7.3重量%、7.6重量%、7.9重量%、8.2重量%、8.5重量%、8.8重量%、9.1重量%、9.4重量%、9.7重量%与10.0重量%。
物理发泡剂是指在聚氨酯制备的原料中分散(如溶解、乳化或悬浮)并在聚氨酯形成的条件下释放或蒸发的化合物。它们为烃、卤代烃和其他化合物,例如全氟烷烃如全氟己烷,氢氯氟烃,以及醚、酯、酮和/或缩醛,例如具有4至8个碳原子的脂族烃或脂族环烃,氢氟烯烃(HFO),或气体例如二氧化碳、氮气或其混合物。根据一些实施例,聚氨酯体系的异氰酸酯反应性组分不含物理发泡剂。
对于链调节剂,其包括具有一个羟基的烷基醇,例如,该烷基醇的碳原子数可以为2-30,优选4-26,更优选10-22。优选具有10-20个碳原子、优选14-18个碳原子的具有一个端羟基的烷基醇,特别优选1-十四醇。如果存在的话,所述链调节剂的量优选为0.1重量%至1.0重量%,例如0.1重量%、0.2重量%、0.3重量%、0.4重量%、0.5重量%、0.6重量%、0.7重量%、0.8重量%、0.9重量%或1.0重量%,以聚氨酯发泡体系的总重量计。
对于抗氧化剂,可以使用所有常用于制备聚氨酯的化合物,例如茶多酚(TP)、生育酚、黄酮类、丁基羟基苯甲醚(BHA)、二丁基羟基甲苯(BHT)、叔丁基氢醌(TBHQ)等。如果存在的话,所述抗氧化剂的量优选为0.1重量%至1.5重量%,例如0.1重量%、0.2重量%、0.3重量%、0.4重量%、0.5重量%、0.6重量%、0.7重量%、0.8重量%、0.9重量%、1.0重量%、1.2重量%、1.3重量%、1.4重量%或1.5重量%,以聚氨酯发泡体系的总重量计。
对于润滑剂,可以使用所有常用于制备聚氨酯的化合物,例如烷氧基化脂肪酸酯、烷氧基化脂肪醇、脂肪胺盐等。如果存在的话,所述润滑剂的量优选为0.1重量%至1.0重量%,例如0.1重量%、0.2重量%、0.3重量%、0.4重量%、0.5重量%、0.6重量%、0.7重量%、0.8重量%、0.9重量%或1.0重量%,以聚氨酯发泡体系的总重量计。
对于抗紫外线添加剂,可以使用所有适合制备聚氨酯的化合物,例如水杨酸酯、苯基酮、苯并三唑、取代的丙烯腈、三嗪等。如果存在的话,所述抗紫外线添加剂的量优选为0.1重量%至1.0重量%,例如0.1重量%、0.2重量%、0.3重量%、0.4重量%、0.5重量%、0.6重量%、0.7重量%、0.8重量%、0.9重量%或1.0重量%,以聚氨酯发泡体系的总重量计。
对于颜料或染料,可以使用所有适合制备聚氨酯的化合物,例如炭黑、苯胺黑、二氧化钛、氧化铁红、钛黄、异吲哚啉酮颜料、氧化镉、酞菁绿、铬红、吖啶嗪、蒽醌、吖啶、花青素、噁嗪、噻嗪等。优选地,颜料或染料以色浆的形式使用。如果存在的话,所述颜料或染料的量优选为0.1重量%至2.0重量%,例如0.1重量%、0.2重量%、0.3重量%、0.4重量%、0.5重量%、0.6重量%、0.7重量%、0.8重量%、0.9重量%、1.0重量%、1.1重量%、1.2重量%、1.3重量%、1.4重量%、1.5重量%、1.6重量%、1.7重量%、1.8重量%、1.9重量%或2.0重量%,以聚氨酯发泡体系的总重量计。
对于增韧剂或抗冲改性剂,可以使用所有适合制备聚氨酯的化合物,例如核壳橡胶、硅酸盐粉、粉状高岭土等。如果存在的话,所述增韧剂或抗冲改性剂的量优选为1重量%至2重量%,例如1.0重量%、1.1重量%、1.2重量%、1.3重量%、1.4重量%、1.5重量%、1.6重量%、1.7重量%、1.8重量%、1.9重量%或2.0重量%,以聚氨酯发泡体系的重量计。
可以使用的填料是有机和无机粉末或者纤维材料,或是其混合物。可以使用的有机填料的实例是木粉、淀粉、亚麻纤维、大麻纤维、苎麻纤维、黄麻纤维、剑麻纤维、棉纤维、纤维素纤维或芳族聚酰胺纤维。可以使用的无机填料的实例是硅酸盐、重晶石、玻璃珠、沸石、金属或金属氧化物。优选使用粉状无机物质,如滑石、白垩、高岭土(Al2(Si2O5)(OH)4)、氢氧化铝、氢氧化镁、亚硝酸铝、硅酸铝、硫酸钡、碳酸钙、硫酸钙、硫酸钡、硅石、粉状石英、气相二氧化硅、氧化铝、云母或硅灰石;或珠粒形式或纤维形式的无机物质,例如铁粉、玻璃珠、玻璃纤维或碳纤维。平均粒径或在纤维形式填料的情况时的长度应在孔尺寸或更小范围内。优选平均粒径在0.1至100 μm范围内,更优选在1至50 μm范围内。如果存在的话,所述填料的量优选为0.1重量%至1.0重量%,例如0.1重量%、0.2重量%、0.3重量%、0.4重量%、0.5重量%、0.6重量%、0.7重量%、0.8重量%、0.9重量%或1.0重量%,以聚氨酯发泡体系的总重量计。
对于成膜剂,可以使用所有适合制备聚氨酯的化合物,例如聚乙烯胺、聚酰胺等。如果存在,成膜剂的量优选0.1重量%至1.0重量%,例如0.1重量%、0.2重量%、0.3重量%、0.4重量%、0.5重量%、0.6重量%、0.7重量%、0.8重量%、0.9重量%或1.0重量%,以聚氨酯发泡体系的总重量计。
在本文描述的所有实施方案中,聚氨酯发泡体系中各组分的含量总和为100重量%,以聚氨酯发泡体系的总重量计。
本发明还提供了一种制备聚氨酯泡沫的方法,其包括,
a) 提供聚氨酯发泡体系;与
b) 让所述聚氨酯发泡体系聚合并发泡。
本发明聚氨酯各组分的混合可以通过常用于生产聚氨酯反应混合物的方式例如在高压或低压方法中进行。发泡可以通过模具发泡、间歇发泡或连续自由发泡等技术人员所熟知的工艺而实现。
聚氨酯泡沫
本发明所提供的可热回收聚氨酯泡沫可由上述聚氨酯发泡体系所制备。其具备好的高回弹率和/或粘弹性。
聚氨酯泡沫优选具有低于250℃的熔融温度,更优选具有低于220℃的熔融温度。
聚氨酯泡沫优选具有30-300 g/L的自由上升密度,更优选具有30-150 g/L的自由上升密度。
聚氨酯泡沫优选具有不低于50%的球回弹率,其根据ASTM D3574测定。
聚氨酯泡沫优选具有1-30 s的恢复时间与在25%挠度时30-150 N的压陷硬度,均通过ASTM D3574测定。
本公开的高回弹聚氨酯泡沫特别适用于运输、运动和家具。例如高回弹聚氨酯泡沫可用于各种车辆中的座椅应用,如轿车、越野车辆、卡车、拖拉机、军用车辆、火车与船只等。或者,高回弹聚氨酯泡沫可用于运动鞋、徒步鞋、靴子等鞋子的鞋底、中底或内底、沙发与床垫。高回弹聚氨酯泡沫提升了鞋子尤其是运动鞋的舒适度和跑步体验。
本公开的粘弹性聚氨酯泡沫体特别适用于运输,例如用于各种车辆或载具中的座椅,例如轿车、越野车辆、卡车、拖拉机、军用车辆、火车、船只等。一种典型的汽车座椅应用采用模制的或板材粘弹性聚氨酯泡沫体的薄(0.5-2.0 cm)层和底下的模制的高回弹性泡沫体。其它座椅泡沫体应用包括与高回弹性泡沫体层共模制,其中可以喷雾或倾倒粘弹性聚氨酯泡沫体组分。粘弹性聚氨酯泡沫体层改善了汽车座椅的舒适度和压力缓和能力。
然而,本公开的粘弹性聚氨酯泡沫体不限于用于运输。作为一个实例,该粘弹性聚氨酯泡沫体特别适用于经历家具例如沙发、床垫或枕头。
回收方法
本发明提供的聚氨酯泡沫可通过多种方法回收。
聚氨酯泡沫可以通过熔融乳化进行回收。在一些情况下,待回收的聚氨酯泡沫可以通过喂料漏斗、喂料螺杆等设备被送入加热的有机液相(如聚醚多元醇、聚酯多元醇、聚碳酸酯多元醇或任意两者或三者的混合体系)并被熔融分散。有机液相中可存在表面活性剂。熔融分散的过程可以伴随机械搅拌、离心等操作。熔融分散可以在转子-定子(rotor-stator)设备中进行以实现泡沫熔融形成的液滴尺寸减小并与液相均匀混合。聚氨酯泡沫熔融并充分乳化后,形成的分散体系可以被冷却以使液滴形式的聚氨酯重新固体化,形成聚氨酯颗粒分散在多元醇中的混合物。该混合物含回收成分(recycled content),可供后续合成聚氨酯之用。
在另一些情况下,可以通过热压方式回收本发明提供的聚氨酯泡沫。在例如高于聚氨酯泡沫熔融温度的温度下,压缩发泡的聚氨酯制品(如软泡床垫或硬泡隔热材料),将发泡的聚氨酯转化为致密的聚氨酯。压缩聚发泡聚氨酯的压力可以超过1个大气压。例如,可以在0.7 MPa压力下使聚氨酯泡沫在180℃熔融。又或者,可以在1.0 MPa压力下使聚氨酯泡沫在160℃熔融。热压时间可以持续,例如,60秒、120秒、180秒、240秒或300秒。致密的聚氨酯可以用作合成革或其他要求更高密度聚氨酯产品的场合。
作为另一种可能,通过对聚氨酯泡沫切粒并与新合成的热塑性聚氨酯粒子混合,并通过成型工艺(如注塑成型、吹塑、压缩成型、挤出成型),可制作含回收成分的最终制品。
实施例
本发明通过实施例及对比例进一步进行说明,但这些实施例和对比例不旨在限制本发明。
使用以下原材料:
Lupranol® 2090,含伯羟基的聚醚多元醇,官能度为3,来自巴斯夫。
Lupranol® 2048,含伯羟基的聚醚多元醇,官能度为3,来自巴斯夫。
CHE 628,聚醚多元醇,是由含活性氢基团的化合物为起始剂在催化剂作用下与氧化乙烯和氧化丙烯开环聚合反应而成,表观官能度为6,来自长华化学。
CHP-H45,固含量41重量%,羟值为19-23 mgKOH/g,基于苯乙烯-丙烯腈(SAN)聚合物的聚合物多元醇,来自长华化学。
YD-310,官能度为3的聚醚多元醇,主要含仲羟基,来自亚东化工。
Lupranol® VP 9391,官能度为3的聚醚多元醇,来自巴斯夫。
二乙醇胺与甘油,用作交联剂,均来自巴斯夫。
Jeffcat® Z-130,凝胶催化剂,来自亨斯曼。
Dabco® NE300,胺类催化剂,来自赢创。
Dabco® NE1091,非挥发性凝胶催化剂,来自赢创。
Dabco® 33 LV,33.3重量%三亚乙基二胺溶于66.7重量%二丙二醇的溶液,用作催化剂,来自赢创。
Dabco® T-120,二月桂基硫醇二丁基锡催化剂,来自赢创。
Dabco® BL-11,叔胺催化剂,来自赢创。
Tegostab® B 8734,硅油型表面活性剂,来自赢创。
VORASURF™ DC 198,硅油型表面活性剂,来自陶氏。
Lupranat® MI,二苯基甲烷二异氰酸酯,其中2,4’-异构体的含量高于LupranatMS,官能度为2,来自巴斯夫。
Lupranat® MS,4,4’-二苯基甲烷二异氰酸酯,官能度为2,来自巴斯夫。
Lupranat® MM 103,碳化二亚胺改性的二苯基甲烷二异氰酸酯,平均官能度约为2.2,来自巴斯夫。
Lupranat® M 20 S,聚合二苯基甲烷二异氰酸酯(pMDI),平均官能度约为2.7,含三环聚亚甲基多苯基异氰酸酯及更高级聚亚甲基多苯基异氰酸酯,来自巴斯夫。
Lupranat T 80 A,2,4-甲苯二异氰酸酯与2,6-甲苯二异氰酸酯的80:20异构体混合物,来自巴斯夫。
Elastopan® CS 9600 C-B,来自巴斯夫。
Lupranat® MIPS,2,4’-二苯基甲烷二异氰酸酯与4,4’-二苯基甲烷二异氰酸酯的混合物,官能度为2,来自巴斯夫。
根据ASTM D3574测试柔性聚氨酯泡沫样品的拉伸强度、断裂伸长率和撕裂强度。拉伸强度、撕裂强度和断裂伸长率性质描绘柔性聚氨酯泡沫体承受制造和组装期间的处置的能力。
压缩强度、压缩模量、自由上升密度与泡沫密度根据ASTM D3574测定。
压陷硬度,根据ASTM D3574的压痕力挠度(IFD)测试指定挠度测定。在挠度25%、40%与65%时,记录力值作为压陷硬度,单位为N。
75%偏转下滞后损失,根据ASTM D3574测定。低的滞后值作为好的弹性泡沫性能的量度对于汽车座椅、沙发等舒适性是重要的。
根据ASTM D3574,对高回弹性聚氨酯泡沫测定了其压缩永久形变(CS)。压缩永久形变将柔性聚氨酯泡沫压缩至原始厚度的50%,并在该压缩下在70℃条件下保持22小时来测量,压缩永久形变表示为原始压缩率的百分比。
根据ASTM D3574,对粘弹性聚氨酯泡沫测定了其压缩永久形变。压缩永久形变将柔性聚氨酯泡沫分别压缩至原始厚度的25%与10%,并在该压缩下在70℃条件下保持22小时来测量,压缩永久形变表示为原始压缩率的百分比。
球回弹率根据ASTM D3574测定。将钢球从参比高度落至样品上,并测量球回弹的峰值高度。球回弹率的值以峰值高度占参比高度的百分比表示。
恢复时间根据ASTM D3574测定。
对聚氨酯泡沫加热直至200℃或240℃,观察其是否发生明显的熔融。
“成乳时间”被定义为从开始混合到反应混合物开始起发的时间间隔。
“凝胶时间”被定义为从开始混合到可通过插入和抽出木棍将长线或发粘材料从起发团块的内部拉出的时间。
“完全起发时间”被定义为从开始混合到发泡团块膨胀完成的时间。
“消粘时间”被定义为从开始混合到可以用手指或压舌板触摸泡沫表面而不粘着的时间。
异氰酸酯组分中的三环与四环聚MDI含量通过高效液相色谱(HPLC)方法测定。使用了搭配二极管阵列检测器的Agilent 1100高效液相色谱仪。其步骤如下:待测样品用四氢呋喃-甲醇50:50混合溶剂在60℃下衍生化1小时。反应后的混合物注射入高效液相色谱仪中。色谱仪使用C18色谱柱(15 cm × 4.6 mm,2 μm),流动相溶剂A为甲酸水溶液,溶剂B为乙腈,进样体积2 μL,流速0.3 mL/min,柱温箱温度30℃。分离后的移动相用紫外探测器在250 nm波长下检测。三环聚MDI与四环聚MDI含量依据外标法测量确定,使用Lupranat®M 20 S与Lupranat® MI作为外标物。
预聚物的制备
将根据表1所示的实施例1至3的异氰酸酯组分中除多元醇外的组分按照表中重量称量,加入至圆底烧瓶中并加热至60℃。在氮气存在下加入多元醇,随后将混合物在80℃下搅拌2小时,冷却并测定NCO、三环聚MDI与四环聚MDI的含量。
聚氨酯泡沫的制备
模具发泡:根据表1、表3、表5与表7所示的聚氨酯发泡体系配置多元醇组分与异氰酸酯组分。并分别进行搅拌,以充分混合各成分。将多元醇组分与异氰酸酯组分混合并剧烈搅拌后,将混合物倒入16 L模具中,并闭合模具。模具温度为55℃。
间歇发泡:根据表7所示的所示的聚氨酯发泡体系配置多元醇组分与异氰酸酯组分。并分别进行搅拌,以充分混合各成分。将多元醇组分与异氰酸酯组分混合并剧烈搅拌后,将混合物倒入边长为30 cm的上开口正方体木箱中自由发泡。
表2、4、6与8分别列出了表1、3、5与7所示配方所制作的泡沫性能。
表1
表2
表3
表4
表5
表6
表7
表8
与实施例1相比,实施例2异氰酸酯反应性组分含较多高官能度多元醇,但其反应得到的聚氨酯泡沫在200℃下仍能熔融。
与实施例2相比,含较多三环聚亚甲基多苯基异氰酸酯的对比例2所得到的聚氨酯泡沫在200℃甚至240℃下不能熔融。
表8中所示的实施例7、7#、8与8#在25%挠度时具有30-150 N的压陷硬度,这对于实现坐垫、床垫等产品的优良触感是有利的。
由以上实施例可知,本发明提供的聚氨酯发泡体系中异氰酸酯反应性组分可以包含较大量的三官能度甚至更高官能度多元醇。这对于聚氨酯配方设计是友好的,赋予聚氨酯体系开发人员更高的自由度。本发明制备聚氨酯泡沫采用一步法,可以采用间歇或连续自由发泡,不需要额外的发泡步骤,也不涉及压力设备如高压釜。
Claims (13)
1.一种聚氨酯发泡体系,包含:
a) 平均官能度为1.7-2.4的异氰酸酯反应性组分,其包含,
分子量高于500 g/mol的一种或多种多元醇;
催化剂,其选自基于胺的催化剂和基于有机金属化合物的催化剂中的一种或多种;
硅氧烷基表面活性剂;
水;
官能度为3或以上的交联剂,其中所述交联剂占所述异氰酸酯反应性组分0.5重量%至10重量%;
任选存在的官能度为2的扩链剂;
和
任选存在的添加剂;与
b) 平均官能度为2.02-2.23的异氰酸酯组分,其包含多异氰酸酯和/或异氰酸酯基团封端的预聚物,所述预聚物由多异氰酸酯与含两个或更多个羟基的化合物反应制备,所述异氰酸酯组分包含三环聚亚甲基多苯基异氰酸酯,其中所述三环聚亚甲基多苯基异氰酸酯重量与所述多异氰酸酯总重量的比不高于5.00%。
2.根据权利要求1所述的聚氨酯发泡体系,其中,所述异氰酸酯反应性组分与所述异氰酸酯组分具有70-120的异氰酸酯指数。
3.根据权利要求1所述的聚氨酯发泡体系,所述异氰酸酯组分具有20重量%至48.2重量%的NCO含量。
4.根据权利要求1所述的聚氨酯发泡体系,所述异氰酸酯组分中三环聚亚甲基多苯基异氰酸酯与四环聚亚甲基多苯基异氰酸酯的重量比为(2-4):1。
5.根据权利要求1所述的聚氨酯发泡体系,所述异氰酸酯反应性组分中官能度为4或以上的多元醇含量不高于80重量%,基于所述异氰酸酯反应性组分的总重量。
6.根据权利要求1所述的聚氨酯发泡体系,所述水占所述异氰酸酯反应性组分的1重量%至5重量%。
7.根据权利要求1所述的聚氨酯发泡体系,所述添加剂选自物理发泡剂、链调节剂、润滑剂、防腐剂、颜料或染料、增韧剂或抗冲改性剂、抗静电剂、流平剂、增塑剂、阻燃剂、成膜剂、抗氧化剂、抗紫外线添加剂、稳定剂、增稠剂、润湿剂、填料中的一种或多种。
8.一种可热回收聚氨酯泡沫,其由如权利要求1至7中任一项所述的聚氨酯发泡体系制备。
9.根据权利要求8所述的可热回收聚氨酯泡沫,其具有低于250℃的熔融温度。
10.根据权利要求8所述的可热回收聚氨酯泡沫,其具有30-300 g/L的自由上升密度。
11.根据权利要求8所述的可热回收聚氨酯泡沫,其具有不低于50%的球回弹率。
12.根据权利要求8所述的可热回收聚氨酯泡沫,其具有1-30 s的恢复时间与在25%挠度时30-150 N的压陷硬度。
13.一种可热回收聚氨酯泡沫的制备方法,其包括,
a) 提供如权利要求1至7中任一项所述的聚氨酯发泡体系;与
b) 让所述聚氨酯发泡体系聚合并发泡。
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