CN103562282B - 聚氨酯泡沫及其制备方法 - Google Patents
聚氨酯泡沫及其制备方法 Download PDFInfo
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- CN103562282B CN103562282B CN201280020955.2A CN201280020955A CN103562282B CN 103562282 B CN103562282 B CN 103562282B CN 201280020955 A CN201280020955 A CN 201280020955A CN 103562282 B CN103562282 B CN 103562282B
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Classifications
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- B29C44/46—Feeding the material to be shaped into an open space or onto moving surfaces, i.e. to make articles of indefinite length
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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Abstract
本发明涉及制备聚氨酯泡沫的方法,其中通过排出管线从混合头中排出一种包含A)、B)、C)和D)的混合物:A)对异氰酸酯呈反应活性的组分;B)表面活性剂组分;C)选自如下的发泡剂组分:直链、支化的或环状的C1-C6烃,直链、支化的或环状C1-C6碳氟氢化合物,N2,O2,氩和/或CO2,其中所述发泡剂C)处于超临界或接近临界状态;和D)多异氰酸酯组分。所述组分A)具有≥100 mg KOH/g至≤1000mg KOH/g的羟基值,所述发泡剂组分C)至少部分地以乳液形式存在,和在排出管线中设置具有一个或多个开孔的部件,以在包含A)、B)、C)和D)的混合物的排出步骤中提高流阻,其中开孔的横截面积或所有开孔的横截面积总和总计为排出管线内部横截面积的≥0.1%至≤99.9%。
Description
本发明涉及制备聚氨酯泡沫的方法,其中从混合头通过排出管线排出混合物,所述混合物包含A)对异氰酸酯呈反应活性的组分;B)表面活性剂组分;C)选自如下的发泡剂组分:直链、支化的或环状的C1-C6烃,直链、支化的或环状C1-C6碳氟氢化合物,N2,O2,氩和/或CO2,其中所述发泡剂C)处于超临界或接近临界状态;和D)多异氰酸酯组分。本发明进一步涉及通过此方法可获得的聚氨酯泡沫。
聚氨酯泡沫通过多元醇组分(其中也可含有发泡剂)与异氰酸酯反应制备。异氰酸酯与水反应产生二氧化碳,二氧化碳也可充当发泡剂。
对于泡沫形成来说并因此对于后来的固化泡沫的泡孔尺寸来说的决定性步骤是由发泡剂提供的成核作用,因为泡沫中的每一个泡孔均由气泡产生。在此有关的观察结果是成核后通常没有新的气泡产生,而是发泡剂扩散进入已经存在的气泡中。
加入稳定剂促进了不同组分的乳化作用,影响成核并抑制成长的气泡聚结。它们也影响泡孔打开。在开孔泡沫中,成长的孔的膜打开,留下孔的支撑(Stege)。
WO 2001/98389 A1中描述了含CO2的反应混合物的突然降压。此专利申请涉及制备聚氨酯块状(Block)泡沫的方法,其中将包含二氧化碳的反应性聚氨酯混合物突然由二氧化碳的平衡溶解压力以上的压力减压至常压。溶解的二氧化碳逸出,反应性液体聚氨酯混合物发泡;将发泡的混合物施加到基底上,然后固化形成块状泡沫。在显著高于平衡溶解压力的压力下首先将二氧化碳完全溶解在反应混合物中,或者溶解在组分多元醇和异氰酸酯中的至少一种中。然后将压力降至接近平衡溶解压力的压力,其中瞬时下降到平衡溶解压力以下,以放出少量二氧化碳和形成气泡微分散体,任选地将各组分混合,压力突然减至大气压之后将释放出的二氧化碳再完全溶解。 然而,在此并没有纳米孔的泡沫或发泡剂的超临界条件的指示。
US 2004/0054022 A1公开了硬质聚氨酯泡沫的制备方法,该泡沫具有20-40 kg/m3的密度和泡孔的纵向直径与横向直径之比的平均值为1.0-1.4。使用的发泡剂是水与多异氰酸酯反应中产生的CO2以及超临界、亚临界或液体CO2。在与多异氰酸酯混合之前,将水和液态的CO2 加入到多元醇中。优选的CO2 含量为0.5%-3%。由于在更大量的CO2时将会有突然汽化的风险,这是不言而喻的。
已知在软质聚氨酯泡沫的制造中用CO2作为物理发泡剂,例如Hennecke的名称为Novaflex? 的发泡剂。
在此需要繁琐的减压技术且CO2的量受限。在此方面FAPU (the European Polyurethane Journal) 59 (2010) 2,第33-35页,写道:“然而,迄今为止机器和原料生产者的测试表明溶解的CO2发泡剂的最大含量在多元醇组分中保持限制在大约2重量%,因为否则在高压混合中泡沫的膨胀即使在混合头中也会失去控制,使得不可能达到均匀的泡孔结构”。
DE 4442 254 A1描述了由双组份反应性塑料制备发泡材料的方法,其中使用二氧化碳作为发泡剂,将至少一种反应性组分与二氧化碳在压力下混合,混合各组分,其中至少一种组分含有在压力下的二氧化碳,将通过混合得到的反应混合物(其含有二氧化碳)减压,并固化。通过产生高剪切速率突然进行减压。因为二氧化碳为溶解状态,所以受控诱导产生气泡核必须“发生在液体反应性混合物由在溶解的二氧化碳中亚饱和的状态过渡为用二氧化碳过饱和的状态的瞬间,即在由溶解的二氧化碳的饱和压力以上的压力减压到溶解的二氧化碳的饱和压力以下的压力的瞬间”。槽缝前后的压力差一般为5-20bar,这显然在74bar的二氧化碳超临界压力以下。
WO 96/02376 A1描述了用在压力下溶解的二氧化碳用于泡沫制备的方法和装置。因为二氧化碳为溶解态,所以其中也必须产生气泡核。这一点通过使用至少一种具有窄的槽缝宽度的槽缝格栅得以实现。
WO 01/10623 A1描述了用于制备聚氨酯泡沫的方法和装置。在此将二氧化碳通过压力保持在溶解状态。成核作用通过产生湍流实现。
所希望的是制备硬质聚氨酯泡沫的进一步改善的方法。本发明的目的是详细说明这种类型的方法,该方法允许尤其是以受控的方式使用更高含量的发泡剂CO2并且形成均匀的泡孔结构。
已经发现,此目的根据本发明通过包含如下步骤的制备聚氨酯泡沫的方法得以实现:
- 在混合头中提供混合物,所述混合物包含:
A) 对异氰酸酯呈反应活性的组分;
B) 表面活性剂组分;
C) 选自如下的发泡剂组分:直链、支化的或环状的C1-C6烃,直链、支化的或环状C1-C6碳氟氢化合物,N2,O2,氩和/或CO2,其中所述发泡剂C)处于超临界或接近临界状态;和
D) 多异氰酸酯组分;
- 通过排出管线从混合头中排出包含 A)、B)、C)和D)的混合物。
该方法特征在于所述对异氰酸酯呈反应活性的组分A)具有 ≥ 100 mg KOH/g至 ≤ 1000 mg KOH/g的羟基值, 所述发泡剂组分C)至少部分地以乳液形式存在,以及具有一个或多个开孔(Mittel)的部件设置在排出管线中以在包含A)、B)、C)和D)的混合物的排放步骤过程中提高流阻, 其中开孔的横截面积或所有开孔的横截面积总和总计为排出管线的内部横截面积的 ≥ 0.1%至≤ 99.9%。
令人惊讶地发现,使用非单相的多元醇发泡剂混合物与混合头的流出系统中用于维持反压和/或压力增加并随后减压至环境压力的装置相结合可以克服现有技术的缺点并可以提供低密度的细孔硬质聚氨酯泡沫。
在混合物的排放步骤中,在排出管线中的流阻提升部件下游在混合物中所处的压力最后降低至大气压。本文中大气压特别是指 ≥ 0.9 bar至 ≤ 1.1 bar的压力。发泡剂过渡为亚临界状态和优选变为气态。例如,反应混合物可以简单地被引入到开放模具中或以连续的方式用于制备片材,例如通过开发发泡装置或双输送机装置进行。
设置于排出管线中(并优选在其端部)用于在包含组分A)、B)、C)和D)的混合物的排放步骤中提高流阻的部件可以是例如从流动方向看安置在混合头的混合室下游的孔板、格栅、槽缝格栅和/或滤网。流阻升高有目的地影响反应混合物从混合头排出之前的压力。如此设定的压力可以低于反应混合物各组分混合过程中的压力。这使得可以影响发泡剂微滴或发泡剂小泡的形成和膨胀。例如WO 2001/98389 A1中描述了这类部件。
所述一个或多个开孔各自具有横截面积。这是指垂直于流出管纵向并由此垂直于反应混合物流动方向的开孔的面积。所以此横截面积最终表明了在反应混合物排放到外部的过程中流动通过的面积。
类似地,排出管线具有内径并由此也具有内部横截面积,其与反应混合物的流动方向呈直角。
在最简单的情况下,从混合头起的排出管线是具有 ≥ 5 mm至≤ 15 mm内径的、任选地呈夹角的圆筒状管且在其一端装有带有直径 ≥ 0.5 mm至≤ 1.5 mm的圆孔的孔板。
组分A)的OH值在加入的单个多元醇的情况下是其OH值。在混合物的情况下规定为平均OH值。在本发明中此值通常可以根据DIN 53240测定。OH值越高,特别是发泡剂CO2在多元醇混合物中的溶解度越差。这与本发明的目的保持一致,因为要寻求发泡剂乳液。关于组分A)的OH值的优选值是 ≥ 200 mg KOH/g至 ≤ 600 mg KOH/g并更优选 ≥ 300 mg KOH/g至 ≤ 550 mg KOH/g。
对本发明方法适合的表面活性剂B)在它们的选择方面最初并不受任何限制。表面活性剂理想地能够使发泡剂在对异氰酸酯呈反应活性的相中形成乳液或微乳液。表面活性剂例如为烷氧基化的链烷醇如具有 ≥ 6至 ≤ 30个碳原子的直链或支化的链烷醇与具有 ≥ 5至≤ 100个氧化烯单元的聚烷撑二醇的醚、烷氧基化的烷基酚、烷氧基化的脂肪酸、烷氧基化的失水山梨糖醇的羧酸酯(尤其是Polysorbate 80)、脂肪酸酯、聚亚烷基胺、硫酸烷基酯、磷脂酰肌醇、氟化的表面活性剂、包含聚硅氧烷基团的表面活性剂、和/或磺基琥珀酸双(2-乙基-1-己基)酯。氟化的表面活性剂可以是全氟化或部分氟化的。其例如为部分氟化的乙氧基化链烷醇或羧酸。
还可以想到发泡剂组分C)至少部分地以乳液形式存在。
使用超临界或接近临界的发泡剂C)制备聚氨酯泡沫。在本发明中当满足下面的条件时,出现接近临界的条件:(Tc–T)/T≤0.4和/或(pc-p)/p≤0.4,其中T是该过程中所处的温度,Tc是发泡剂或发泡剂混合物的临界温度,p是该过程中所处的压力和pc是发泡剂或发泡剂混合物的临界压力。当(Tc–T)/T≤0.3 和/或(pc-p)/p≤0.3和更优选(Tc–T)/T≤0.2 和/或(pc-p)/p≤0.2时,优选出现接近临界的条件。不愿意局限于任一种理论的束缚,据认为通过适合的表面活性剂组分的选择,在包含对异氰酸酯呈反应活性的组分的相中形成超临界或接近临界的发泡剂的乳液或微乳液。
发泡剂优选可以在反应混合物中形成自己的相。例如可以使用超临界二氧化碳。二氧化碳可以在形成聚氨酯泡沫的反应过程中形成,例如通过异氰酸酯与水或与酸反应。其它发泡剂的实例是直链C1-C6-烃、支化的C4-C6-烃和环状C3-C6-烃。发泡剂的具体实例有甲烷、乙烷、丙烷、正丁烷、异丁烷、正戊烷、异戊烷、环戊烷、异己烷和/或环己烷。另外例如为甲烷、乙烷、丙烷、正丁烷、异丁烷、正戊烷、异戊烷、环戊烷、己烷、异己烷、2,3-二甲基丁烷和/或环己烷的部分或全氟化的衍生物。优选使用二氧化碳或具有的二氧化碳含量大于30重量%、优选大于50重量%和更优选大于70重量%的发泡剂混合物。
发泡剂在包含A)、B)和C),但不包含D)的反应混合物中的比例可以为例如≥ 5重量%至≤ 40重量%。
组分D)是多异氰酸酯,即具有 ≥ 2的NCO官能度的异氰酸酯。因此,反应混合物可以反应得到聚氨酯泡沫或多异氰尿酸酯泡沫。此反应混合物可以直接在混合头中制备。
合适的多异氰酸酯的实例是1,4-丁二异氰酸酯、1,5-戊二异氰酸酯、1,6-己二异氰酸酯(HDI)、异佛尔酮二异氰酸酯(IPDI)、2,2,4-和/或2,4,4-三甲基-己二异氰酸酯、异构双(4,4'-异氰酸根合环己基)甲烷或具有任何异构体含量的其混合物、1,4-环己二异氰酸酯、1,4-苯二异氰酸酯、2,4-和/或2,6-甲苯二异氰酸酯(TDI)、1,5-萘二异氰酸酯、2,2'-和/或2,4'-和/或4,4'-二苯甲烷二异氰酸酯(MDI)和/或更高级同系物(聚合MDI)、1,3-和/或l,4-双(2-异氰酸根合丙-2-基)-苯(TMXDI)、l,3-双(异氰酸根合甲基)苯(XDI)和含有C1至C6烷基的2,6-二异氰酸根合己酸烷基酯(赖氨酸二异氰酸酯)。优选来自二苯甲烷二异氰酸酯系列的异氰酸酯。
除上述多异氰酸酯外,还可以以合适的比例使用具有脲二酮、异氰脲酸酯、氨基甲酸酯、碳二亚胺、脲酮亚胺、脲基甲酸酯、缩二脲、酰胺、亚氨基噁二嗪二酮和/或噁二嗪三酮结构的改性二异氰酸酯以及每分子含有多于2个NCO基团的未改性多异氰酸酯,例如4-异氰酸根合甲基-1,8-辛烷二异氰酸酯(壬烷三异氰酸酯)或三苯甲烷-4,4',4"-三异氰酸酯。
异氰酸酯可以是通过具有 ≥ 2的NCO官能度的异氰酸酯与具有 ≥ 62 g/mol至 ≤ 8000 g/mol的分子量和 ≥ 1.5至 ≤ 6的OH官能度的多元醇反应可获得的预聚物。
当然还可以使用另外的常规助剂和添加剂诸如催化剂、阻燃剂、脱模剂、填料等以制备聚氨酯泡沫。
多异氰酸酯组分D)中的NCO基团数和组分A)的对异氰酸酯呈反应活性的基团数的数值比可以例如互相为≥50:100至≤500:100。该指数也可以处于范围 ≥160:100至≤ 330:100或≥80:100至≤140:100。
包含组分A)、B)、C)和D)的混合物例如通过在对于发泡剂来说超临界或接近临界的条件下首先将除了多异氰酸酯组分之外的所有组分装入高压混合头中并接着将它们与多异氰酸酯D)混合可获得。
用于制备聚氨酯泡沫的混合头中和/或排出管线中(在包含A)、B)、C)和D)的混合物的排放步骤中用于提高流阻的单开孔或多开孔部件的上游)的适合的压力可以例如为≥ 40 bar至≤ 300 bar并且可以优选为≥ 60 bar至≤ 250 bar。适合的温度例如为 ≥ 10℃至 ≤ 80℃ , 优选 ≥ 25℃至 ≤ 60℃。特别优选CO2的临界点以上的压力和温度,即 ≥ 73.7 bar和≥ 31℃。
适合的对NCO呈反应活性的组分A)尤其是多元醇、多胺、聚氨基醇和多硫醇。
多胺的实例是乙二胺、1,2-二氨基丙烷、1,3-二氨基丙烷、1,4-二氨基丁烷、1,6-二氨基己烷、异佛尔酮二胺、2,2,4-和2,4,4-三甲基六亚甲基二胺的异构混合物、2-甲基五亚甲基二胺、二亚乙基三胺、1,3-苯二甲基二胺、1,4-苯二甲基二胺、 α,α,α’,α’-四甲基-1,3-苯二甲基二胺、 α,α,α’,α’-四甲基-1,4-苯二甲基二胺、4,4’-二氨基二环己基甲烷、二乙基甲基苯二胺(DETDA)、4,4’-二氨基-3,3’-二氯二苯甲烷(MOCA)、二甲基亚乙基二胺、1,4-双(氨基甲基)环己烷、4,4'-二氨基-3,3’-二甲基二环己基甲烷和 4,4'-二氨基-3,5-二乙基-3’,5’-二异丙基二环己基甲烷。聚合的多胺如聚亚氧烷基胺也是适合的。
氨基醇例如为N-氨基乙基乙醇胺、乙醇胺、3-氨基丙醇、新戊醇胺和二乙醇胺。
多硫醇例如为二(2-巯基乙基)醚、季戊四醇四硫基乙醇酸酯、季戊四醇四(3-巯基丙酸酯) 和1,2-双((2-巯基乙基)硫代)-3-巯基丙烷。
多元醇例如可以具有 ≥ 62 g/mol至 ≤ 8000 g/mol,优选 ≥ 90 g/mol至 ≤ 5000 g/mol和更优选 ≥ 92 g/mol至 ≤ 1000 g/mol的数均分子量Mn。
所述多元醇的平均OH官能度例如≥2,例如为≥2至≤6,优选≥2.1至≤4,且更优选≥2.2至≤3。
可使用的聚醚多元醇的实例是可通过四氢呋喃经由阳离子开环聚合获得的聚丁二醇聚醚。
合适的聚醚多元醇进一步包括氧化苯乙烯、环氧乙烷、环氧丙烷、环氧丁烷和/或表氯醇加成到二-或多官能起始物分子上的产物。
合适的起始物分子是例如水、乙二醇、二甘醇、丁基二甘醇、甘油、二甘醇、三羟甲基丙烷、丙二醇、季戊四醇、山梨糖醇、蔗糖、乙二胺、甲苯二胺、三乙醇胺、1,4-丁二醇、1,6-己二醇和所述多元醇与二羧酸的低分子含羟基酯。
适合的聚酯多元醇包括二-以及三-和四醇与二-以及三-和四羧酸的缩聚物或羟基羧酸的或内酯的缩聚物。相应的多羧酸酐或低级醇的相应的多羧酸酯也可代替游离多羧酸用于制备聚酯。
合适的二醇的实例是乙二醇、丁二醇、二甘醇、三甘醇、聚烷撑二醇,如聚乙二醇,以及1,2-丙二醇、1,3-丙二醇、1,3-丁二醇、1,4-丁二醇、1,6-己二醇和异构体、新戊二醇或羟基特戊酸新戊二醇酯。此外,也可以使用多元醇,如三羟甲基丙烷、甘油、赤藻糖醇、季戊四醇、三羟甲基苯或异氰脲酸三羟乙酯。
可用的多羧酸例如是邻苯二甲酸、间苯二甲酸、对苯二甲酸、四氢邻苯二甲酸、六氢邻苯二甲酸、环己二甲酸、己二酸、壬二酸、癸二酸、戊二酸、四氯邻苯二甲酸、马来酸、富马酸、衣康酸、丙二酸、辛二酸、琥珀酸、2-甲基琥珀酸、3,3-二乙基戊二酸、2,2-二甲基琥珀酸、十二烷二酸、桥亚甲基四氢邻苯二甲酸、二聚脂肪酸、三聚脂肪酸、柠檬酸或偏苯三酸。也可以使用相应的酐作为酸源。
只要待酯化的多元醇的平均官能度≥2,还可以使用单羧酸,如苯甲酸和己烷甲酸。
在含有端羟基的聚酯多元醇的制备中可同时用作反应物的羟基羧酸的实例是羟基己酸、羟基丁酸、羟基癸酸、羟基硬脂酸等。合适的内酯尤其包括己内酯、丁内酯和同系物。
根据本发明可使用的聚碳酸酯多元醇是含羟基的聚碳酸酯,例如聚碳酸酯二醇。这些可通过碳酸衍生物,如碳酸二苯酯、碳酸二甲酯或光气与多元醇,优选二醇的反应获得,或可通过环氧烷如环氧丙烷与二氧化碳的共聚反应获得。
所述二醇的实例是乙二醇、1,2-和1,3-丙二醇、1,3-丁二醇、1,4-丁二醇、1,6-己二醇、1,8-辛二醇、新戊二醇、1,4-双羟甲基环己烷、2-甲基-1,3-丙二醇、2,2,4-三甲基-1,3-戊二醇、二丙二醇、聚丙二醇、二丁二醇、聚丁二醇、双酚A和上述类型的内酯改性二醇。
也可以用聚醚-聚碳酸酯二醇代替纯的聚碳酸酯二醇,或者除了纯的聚碳酸酯二醇还可以用聚醚-聚碳酸酯二醇。
可以使用的聚醚酯多元醇是含有醚基团、酯基团和OH基团的化合物。具有最多12个碳原子的有机二羧酸适用于制备聚醚酯多元醇,优选为具有≥4至≤6个碳原子的脂族二羧酸或芳族二羧酸,它们可以独立或混合使用。例如,可以提到辛二酸、壬二酸、癸烷二羧酸、马来酸、丙二酸、邻苯二甲酸、庚二酸和癸二酸,尤其是戊二酸、富马酸、琥珀酸、己二酸、邻苯二甲酸、对苯二甲酸和间苯二甲酸。可用的这些酸的衍生物是例如它们的酐和它们与具有≥1至≤4个碳原子的低分子量一元醇的酯和半酯。
用于制备聚醚酯多元醇的其它组分是通过起始物分子,如多元醇的烷氧基化获得的聚醚多元醇。该起始物分子是至少双官能的,但任选还可含有一定比例的更高官能,尤其是三官能的起始物分子。
起始物分子例如是具有优选≥18g/mol至≤400g/mol或≥62g/mol至≤200g/mol的数均分子量Mn的二醇,如1,2-乙二醇、1,3-丙二醇、1,2-丙二醇、1,4-丁二醇、1,5-戊烯二醇、1,5-戊二醇、新戊二醇、1,6-己二醇、1,7-庚二醇、1,8-辛二醇、1,10-癸二醇、2-甲基-1,3-丙二醇、2,2-二甲基-1,3-丙二醇、3-甲基-1,5-戊二醇、2-丁基-2-乙基-1,3-丙二醇、2-丁烯-1,4-二醇和2-丁炔-1,4-二醇,醚二醇类,如二甘醇、三甘醇、四甘醇、二丁二醇、三丁二醇、四丁二醇、二己二醇、三己二醇、四己二醇,和烷撑二醇如二甘醇的低聚混合物。
除二醇外,也可以使用数均官能度>2至≤8或≥3至≤4的多元醇,例如1,1,1-三羟甲基丙烷、三乙醇胺、甘油、失水山梨糖醇和季戊四醇以及具有平均分子量优选为≥62 g/mol至≤400g/mol或≥92 g/mol至≤200g/mol的在三醇或四醇上起始的聚环氧乙烷多元醇。
聚醚酯多元醇也可通过由有机二羧酸与二醇的反应得到的反应产物的烷氧基化作用而制备。可以使用的所述酸的衍生物的实例是它们的酸酐,例如邻苯二甲酸酐。
聚丙烯酸酯多元醇可通过含羟基的烯键式不饱和单体的自由基聚合或通过含羟基的烯键式不饱和单体任选与其它烯键式不饱和单体的自由基共聚获得。实例是丙烯酸乙酯、丙烯酸丁酯、丙烯酸2-乙基己酯、丙烯酸异冰片酯、甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸丁酯、甲基丙烯酸环己酯、甲基丙烯酸异冰片酯、苯乙烯、丙烯酸、丙烯腈和/或甲基丙烯腈。合适的含羟基的烯键式不饱和单体特别是丙烯酸2-羟乙酯、甲基丙烯酸2-羟乙酯、可通过环氧丙烷加成到丙烯酸上获得的丙烯酸羟丙酯异构体的混合物和可通过环氧丙烷加成到甲基丙烯酸上获得的甲基丙烯酸羟丙酯异构体的混合物。端羟基也可以以被保护形式存在。合适的自由基引发剂是选自偶氮化合物,例如偶氮二异丁腈(AIBN),或选自过氧化物例如二叔丁基过氧化物的那些。
在一个配方实例中,组分A)、B)、C)和D)以如下的量存在:
A) ≥ 25重量%至 ≤ 45重量%
B) ≥ 0.5重量%至 ≤ 15重量%
C) ≥ 4重量%至 ≤ 40重量%
D) ≥ 30重量%至 ≤ 70重量%。
重量%数值在此总计为 ≤ 100重量%。各组分优选的量为:
A) ≥ 30重量%至 ≤ 40重量%
B) ≥ 1重量%至 ≤ 5重量%
C) ≥ 6重量%至 ≤ 20重量%
D) ≥ 40重量%至 ≤ 60重量%。
现在将对根据本发明的方法借助优选的实施方案更详细地描述。它们可以以任何需要的方式结合,除非由上下文明显是相反的。
在另一个实施方案中,所述开孔的横截面积或所有开孔的横截面积总和总计为排出管线内部截面面积的≥ 0.5%至≤ 10%。一个开孔优选为出口喷嘴的形式。开孔横截面积或所有开孔横截面积总和的优选的范围为≥ 0.7%至 ≤ 2.5%。
在另一个实施方案中,存在超临界条件的混合头内部和/或外部的反应室的体积与开孔的横截面积或与所有开孔的横截面积总和之比为 ≥ 5 m至 ≤ 200 m。
反应室可以在混合头内由其混合室形成。在混合头外部,反应室可以由在包含A)、B)、C)和D)的混合物的排放步骤中用于升高流阻的部件的上游的那部分排出管线形成。因此,在最简单的情况下,孔板上游的排出管线的体积提供了反应室的体积。
利用所述比例,混合物的流动通过PU反应过程中粘度增加,而受到有利的影响。优选的比例是 ≥ 10 m至 ≤ 100 m。
在另一个实施方案中,从具有一个或多个开孔的流阻提升部件排出包含A)、B)、C)和D)的混合物时,排出的混合物的体积流与开孔的横截面积或与横截面积总和之比为 ≥ 5 m/s至 ≤ 400 m/s。
同样,利用所述比例,混合物的流动通过PU反应过程中粘度增加,而受到有利的影响。优选的比例是 ≥ 40 m/s至 ≤ 200 m/s。
在另一个实施方案中,在提供混合物之后在混合头中存在≥ 40 bar至≤ 150 bar的压力。在混合头中和混合头的下游特别存在此状态。压力也可以为 ≥ 80 bar至≤ 120 bar或 ≥ 60 bar至 ≤ 100 bar。所述压力将保持对使用的发泡剂为超临界或接近临界的条件。
在另一个实施方案中,混合头中的混合物在发泡剂的超临界或接近临界条件下具有 ≥ 0秒至 ≤ 20秒,优选 ≥ 0.1 秒至 ≤ 10秒并更优选 ≥ 0.5秒至 ≤ 5秒的停留时间。这确保了混合物可以在超临界或接近临界条件下聚合。停留时间可以通过其中所处为超临界或接近临界条件的反应室的体积(=带有直到孔板的流出管位置的混合室的总体积)除以每单位时间输送的混合物的体积来测定。
在另一个实施方案中,所述对异氰酸酯呈反应活性的组分A)包含具有 ≥ 200 mg KOH/g至≤ 600 mg KOH/g的羟基值的聚醚酯多元醇和具有 ≥ 800 mg KOH/g羟基值的短链多元醇。适合的聚醚酯多元醇尤其包括双官能聚醚酯多元醇,其通过环氧烷且尤其是环氧乙烷加成到邻苯二甲酸酐、二甘醇和乙二胺的混合物上得到并具有 ≥ 275 mg KOH/g至 ≤ 325 mg KOH/g的OH值。
此类产品由Bayer MaterialScience AG 以商品名Desmophen? VP.PU 1431可得。聚酯多元醇的OH值也可以为 ≥ 290 mg KOH/g 至 ≤ 320 mg KOH/g。短链多元醇特别是具有 ≥ 2至≤ 6 个碳原子的多元醇。甘油是优选的。其具有1827 mg KOH/g的OH值。通过加入短链多元醇可以有利地增加多元醇相的极性。
在另一个实施方案中,表面活性剂组分B)包含聚硅氧烷-聚氧化烯共聚物。聚硅氧烷-聚氧化烯共聚物(硅酮-二醇共聚物)优选涉及以CAS号87244-72-2登记的化合物。
在另一个实施方案中,所述发泡剂组分C)的比例基于混合物的总重量计为 ≥ 4重量%至≤ 12重量%。优选的比例是 ≥ 6重量%至 ≤ 10重量%和特别优选的比例为 ≥ 7重量%至 ≤ 9重量%。
在另一个实施方案中,所述多异氰酸酯组分D)包含单体的和/或聚合的二苯甲烷4,4’-二异氰酸酯。此类型的多异氰酸酯由Bayer MaterialScience作为二苯甲烷4,4’-二异氰酸酯(MDI)与异构体和更高官能的同系物的混合物以商品名Desmodur? 44V70L可得。
本发明进一步提供了通过本发明的方法获得的或可以获得的聚氨酯泡沫。
在一个实施方案中,聚氨酯泡沫具有 ≥ 20 kg/m3至≤ 160 kg/m3的表观密度。表观密度可以根据DIN EN 1602测定并且优选为≥ 30 kg/m3至≤ 120 kg/m3和更优选 ≥ 40 kg/m3 至≤ 80 kg/m3。对于本发明的泡沫来说绝热是其中优选的用途。
本发明借助下面的实施例进行阐述,而不是受其限制。
词汇表
Desmophen? VP.PU 1431:双官能聚醚酯多元醇,EO在邻苯二甲酸酐、二甘醇和乙二胺的混合物上的加合物,其中OH值为275-325 mg KOH/g和在25℃下粘度为6.5 ± 1.3 Pa s; Bayer MaterialScience AG。
DABCO? DC198:Air Products的产品;稳定剂/表面活性剂。DABCO? DC198是聚硅氧烷-聚氧化烯共聚物(硅酮-二醇共聚物)。这种类型的化合物登记为CAS号87244-72-2。
DBTL:二月桂酸二丁基锡。
Desmorapid? 726b:来自Bayer MaterialScience AG的催化剂。
Desmodur? 44V70L:二苯甲烷4,4’-二异氰酸酯(MDI)与异构体和更高官能度的同系物的混合物,来自Bayer MaterialScience AG。
实施例1至实施例4以及对比例1和2
根据下表1中所述的配方制备CO2-发泡的聚氨酯泡沫。除非另外说明,数量以重量份给出。对异氰酸酯呈反应活性的化合物A)的混合物与加入的组分如表面活性剂B)和催化剂混合。其在标准的高压混合装置中作为多元醇组分使用并在120 bar的压力下与发泡剂C)混合。在此过程中处于对发泡剂的超临界条件。将此混合物在高压混合头中与多异氰酸酯D)混合,后者在120 bar压力下进行输送。在混合头中所处的条件下发泡剂至少部分以乳液形式存在。
注射量(Schussmenge)为60g/s,相当于体积流为72ml/s(混合物密度为1.2g/ml)。混合头的流出管具有8.5mm的内径和大约50cm的长度。包括直到孔板位置的流出管在内的混合室总体积为36ml。在实施例中具有表中说明的孔尺寸的孔板被装配在混合头下游的流出管中。这使得可以以受控的方式设定混合头中的压力并实现反应混合物中压力的更缓慢降低。
与实施例1和4相反,特意地设定在低压的对比例1和2具有显然更高的表观密度。这表明这里发泡剂明显利用较差。
Claims (9)
1.制备聚氨酯泡沫的方法,包括如下步骤:
- 在混合头中提供混合物,其中所述混合物包括:
A) 对异氰酸酯呈反应活性的组分;
B) 表面活性剂组分;
C) 选自如下的发泡剂组分:直链、支化的或环状的C1-C6烃,直链、支化的或环状C1-C6碳氟氢化合物,N2,O2,氩和/或CO2,其中所述发泡剂C)处于超临界或接近临界状态;和
D) 多异氰酸酯组分;
- 通过排出管线从混合头中排出包含A)、B)、C)和D)的混合物,
其特征在于
所述对异氰酸酯呈反应活性的组分A)具有 ≥ 100 mg KOH/g 至 ≤ 1000 mg KOH/g的羟基值,
所述发泡剂组分C)至少部分地以乳液形式存在,和
在排出管线中设置具有一个或多个开孔的部件,以在包含A)、B)、C)和D)的混合物的排出步骤中提高流阻,其中开孔的横截面积或所有开孔的横截面积总和总计为排出管线内部横截面积的≥ 0.1%至≤ 99.9%,并且其中在混合头内部和/或外部的处于超临界条件的反应室的体积与开孔的横截面积或与所有开孔的横截面积总和之比为≥ 5 m至 ≤ 200 m。
2.如权利要求1所述的方法,其中所述开孔的横截面积或所有开孔的横截面积总和总计为排出管线内部截面面积的≥ 0.5%至≤ 10%。
3.如权利要求1所述的方法,其中在从具有一个或多个开孔的流阻提升部件排出包含A)、B)、C)和D)的混合物时,排出的混合物的体积流速与开孔的横截面积或与横截面积总和之比为≥ 5 m/s至 ≤ 400 m/s。
4.如权利要求1所述的方法,其中在提供混合物之后在混合头中存在≥ 40 bar至≤ 150 bar的压力。
5.如权利要求1所述的方法,其中在发泡剂的超临界或接近临界的条件下混合头中的混合物具有≥ 0秒至≤ 20秒的停留时间。
6.如权利要求1所述的方法,其中所述对异氰酸酯呈反应活性的组分A)包含具有羟基值为 ≥ 200 mg KOH/g至≤ 600 mg KOH/g的聚醚酯多元醇和具有羟基值为≥ 800 mg KOH/g的短链多元醇。
7.如权利要求1所述的方法,其中所述表面活性剂组分B)包含聚硅氧烷-聚氧化烯共聚物。
8.如权利要求1所述的方法,其中所述发泡剂组分C)的比例基于混合物的总重量计为≥ 4重量%至≤ 12重量%。
9.如权利要求1所述的方法,其中所述多异氰酸酯组分D)包含单体的和/或聚合的二苯甲烷4,4'-二异氰酸酯。
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DE102011050014.6 | 2011-04-29 | ||
DE102011050014A DE102011050014A1 (de) | 2011-04-29 | 2011-04-29 | Polyurethanschaum und Verfahren zu seiner Herstellung |
PCT/EP2012/057433 WO2012146571A1 (de) | 2011-04-29 | 2012-04-24 | Polyurethanschaum und verfahren zu seiner herstellung |
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CN103562282A CN103562282A (zh) | 2014-02-05 |
CN103562282B true CN103562282B (zh) | 2015-08-19 |
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US (1) | US9834655B2 (zh) |
EP (1) | EP2702095B1 (zh) |
JP (1) | JP2014513181A (zh) |
KR (1) | KR101949547B1 (zh) |
CN (1) | CN103562282B (zh) |
CA (1) | CA2834325C (zh) |
DE (1) | DE102011050014A1 (zh) |
MX (1) | MX2013012602A (zh) |
RU (1) | RU2013152643A (zh) |
TR (1) | TR201819513T4 (zh) |
WO (1) | WO2012146571A1 (zh) |
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US10131759B2 (en) | 2013-11-08 | 2018-11-20 | Covestro Deutschland Ag | Polyurethane foam and process for producing same |
FR3020365B1 (fr) * | 2014-04-29 | 2017-10-27 | Michelin & Cie | Procede de fabrication par microcoulee d'une mousse de polyurethane |
EP3372625A1 (de) * | 2017-03-07 | 2018-09-12 | Covestro Deutschland AG | Polyurethanschaum und verfahren zu seiner herstellung |
CN106947009B (zh) * | 2017-03-22 | 2019-06-28 | 北京化工大学 | 一种开孔型有机泡沫材料的制备方法 |
KR102691261B1 (ko) * | 2023-06-14 | 2024-08-05 | 주식회사 람스타일컴퍼니 | 허리 지지력이 우수한 폼의 제조방법 |
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DE3312215A1 (de) * | 1983-04-05 | 1984-10-11 | Bayer Ag, 5090 Leverkusen | Verfahren zur herstellung eines zelligen polyurethans |
AU2927295A (en) | 1994-07-18 | 1996-02-16 | Bayer Aktiengesellschaft | Process and device for preparing foam using carbon dioxide dissolved under pressure |
PL179287B1 (pl) | 1994-11-28 | 2000-08-31 | Bayer Ag | Sposób wytwarzania materialów piankowych,zwlaszcza poliuretanowych materialów piankowychoraz urzadzenie do wytwarzania materialów piankowych, zwlaszcza poliuretanowych materialów piankowych PL |
DE4442254A1 (de) | 1994-11-28 | 1996-05-30 | Hennecke Gmbh Maschf | Verfahren und Vorrichtung zur Schaumherstellung mittels unter Durck gelöstem Kohlendioxid |
IT1313609B1 (it) | 1999-08-09 | 2002-09-09 | Worldwide Polyurethanes B V | Procedimento e dispositivo per la produzione di una schiumapoliuretanica espansa |
US6818675B2 (en) | 2002-08-06 | 2004-11-16 | General Electric Company | Process for preparing polyurethane foam |
JP4154654B2 (ja) | 2002-09-13 | 2008-09-24 | アキレス株式会社 | 硬質ポリウレタンフォームの製造方法 |
CN102203158B (zh) * | 2008-11-06 | 2013-11-27 | 旭有机材工业株式会社 | 聚氨酯泡沫体用发泡性组合物及聚氨酯泡沫体 |
JP5226129B2 (ja) * | 2009-04-22 | 2013-07-03 | パナソニック株式会社 | 混合吐出装置 |
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2011
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2012
- 2012-04-24 US US14/113,594 patent/US9834655B2/en active Active
- 2012-04-24 EP EP12716419.2A patent/EP2702095B1/de active Active
- 2012-04-24 CN CN201280020955.2A patent/CN103562282B/zh not_active Expired - Fee Related
- 2012-04-24 JP JP2014506830A patent/JP2014513181A/ja active Pending
- 2012-04-24 KR KR1020137031275A patent/KR101949547B1/ko active IP Right Grant
- 2012-04-24 TR TR2018/19513T patent/TR201819513T4/tr unknown
- 2012-04-24 CA CA2834325A patent/CA2834325C/en not_active Expired - Fee Related
- 2012-04-24 RU RU2013152643/05A patent/RU2013152643A/ru not_active Application Discontinuation
- 2012-04-24 WO PCT/EP2012/057433 patent/WO2012146571A1/de active Application Filing
- 2012-04-24 MX MX2013012602A patent/MX2013012602A/es unknown
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EP0353061A2 (en) * | 1988-07-29 | 1990-01-31 | Pmc, Inc. | Blowing agents for polyurethane foam |
CN1437622A (zh) * | 2000-06-21 | 2003-08-20 | 亨内克股份有限公司 | 块状泡沫的生产方法 |
CN102686628A (zh) * | 2009-11-06 | 2012-09-19 | 拜尔材料科学股份公司 | 制造聚氨酯泡沫的方法和能由其获得的聚氨酯泡沫 |
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MX2013012602A (es) | 2013-12-06 |
CA2834325C (en) | 2019-03-12 |
WO2012146571A1 (de) | 2012-11-01 |
RU2013152643A (ru) | 2015-06-10 |
DE102011050014A1 (de) | 2012-10-31 |
TR201819513T4 (tr) | 2019-01-21 |
JP2014513181A (ja) | 2014-05-29 |
KR101949547B1 (ko) | 2019-02-18 |
US20140066534A1 (en) | 2014-03-06 |
US9834655B2 (en) | 2017-12-05 |
CN103562282A (zh) | 2014-02-05 |
KR20140043352A (ko) | 2014-04-09 |
EP2702095A1 (de) | 2014-03-05 |
CA2834325A1 (en) | 2012-11-01 |
EP2702095B1 (de) | 2018-10-03 |
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