CN112300355B - 一种双组分水性聚氨酯、其用途、由其形成的聚氨酯复合抛光垫及制备方法 - Google Patents
一种双组分水性聚氨酯、其用途、由其形成的聚氨酯复合抛光垫及制备方法 Download PDFInfo
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- CN112300355B CN112300355B CN202011187555.3A CN202011187555A CN112300355B CN 112300355 B CN112300355 B CN 112300355B CN 202011187555 A CN202011187555 A CN 202011187555A CN 112300355 B CN112300355 B CN 112300355B
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- waterborne polyurethane
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Abstract
本发明提供一种双组分水性聚氨酯、其用途、由其形成的聚氨酯复合抛光垫及制备方法。本发明的双组分水性聚氨酯，包括水性聚氨酯树脂和水性聚氨酯固化剂，所述水性聚氨酯树脂和所述水性聚氨酯固化剂的重量比为(65～97):(3～30)。所述水性聚氨酯固化剂以多异氰酸酯、聚合物多元醇、扩链剂和封闭剂为原料反应制得。本发明通过水性聚氨酯固化剂与水性聚氨树脂混合后以特定的工艺对基底材料进行处理，热解封出的异氰酸根基团可以与羟基反应，通过交联反应生成网状结构，不仅减少了异氰酸酯基与水的副反应，此外还能将纤维之间的氢键结合转变为化学键结合，形成稳定的三维结构，最终显著提高黏附纤维丝后复合抛光垫的硬度、强度、耐磨性能。
Description
技术领域
本发明属于抛光垫材料的技术领域，涉及一种一种双组分水性聚氨酯、其用途、由其形成的聚氨酯复合抛光垫及制备方法。
背景技术
随着近些年人们对智能电子产品的需求越来越大，高效集成电路的性能精密度要求也随之提高，在集成电路面积不变的情况下，单晶体管减小和多层布线技术已成为主要趋势，而这对半导体晶片的表面平坦度有很高的要求，化学机械抛光(CMP)技术能够有效地对晶片表面进行平坦化处理，该技术是通过在一定的压力条件下，抛光液对工件表面产生化学腐蚀，形成软化层，然后磨粒对其进行磨削，最终是产品表面光洁。抛光垫在抛光过程中是作为储存和运输抛光液的载体，同时提供一定的物理承载能力。
目前主流的抛光垫分为三种：聚氨酯发泡抛光垫、阻尼布抛光垫和无纺布复合抛光垫。聚氨酯发泡抛光垫是将聚氨酯预聚体，发泡剂以及增链剂混合后再一起注入到模具中固化成型，然后切片得到最终产品，此类抛光垫具有很高的硬度，使用时不易发生变形，能够加工出高平坦度的产品，缺点是容易产生划痕，因此主要用化学机械抛光(CMP)过程中的粗抛阶段；阻尼布抛光垫分为基材和抛光层，抛光层是聚氨酯和发泡剂在水中凝固，高温烘干成膜状制得，该抛光垫质地柔软，能够很好的贴合工件表面，获得高平滑性和低欠陷的产品，常应用于精抛加工过程，不过由于柔韧性太好而无法达到较高的平坦度；无纺布复合抛光垫则是介于前面两种抛光垫的中间产品，由无纺布浸渍在聚氨酯溶液中，湿固化后烘干后成型，其中无纺布是用撞针反复撞击聚酯纤维使其粘合一起成毛毡，无纺布质地柔软，在受压时提供缓冲空间，增强贴合能力，而且孔隙率高，能够吸收磨粒和碎屑，使其不在表面团聚，从而减少了对工件表面的划伤，聚氨酯浸渍固化后表面的高硬度聚氨酯则提供了一定的磨削能力，因此这种复合抛光垫在保证去除速率的同时还能兼顾平滑性，但是很难达到高水准的平坦度。
专利CN87102270公开了一种不同熔点聚氨酯混合浸渍制备抛光垫的方法，对抛光垫加热后进行处理，使低熔点的聚氨酯融化聚集，复合在无纺布和高熔点聚氨酯上，从而改善硬度和透水性，但效果不是很明显。专利CN 104385120通过调整聚氨酯的固化方式，在水浴中预凝聚，再放在烘箱中烘干固化成型，该方法中聚氨酯在无纺布中能够均匀的分布，最终的产品同时具有良好的硬度和液体涵养量。专利CN 102119069公开了一种利用高密度超细纤维络合无纺布制作抛光垫的方法，并通过调整高分子弹性体的填充量，确保内部的体积空隙率在50％以上，由此得到的抛光垫在提供较好的抛光液涵养量的同时还具备一定的刚性，但此种方法制备过程繁琐，成本较高。
发明内容
鉴于以上所述现有技术的缺点，本发明的目的之一在于提供一种双组分水性聚氨酯。
本发明的目的之二在于提供双组分水性聚氨酯用于聚氨酯复合光垫中作为改性涂层的用途。
本发明的目的之三在于提供一种聚氨酯复合抛光垫，附着有所述双组分水性聚氨酯。
本发明的目的之四在于提供一种聚氨酯复合抛光垫的制备方法。
为实现上述目的及其他相关目的，本发明的第一方面提供一种双组分水性聚氨酯，包括水性聚氨酯树脂和水性聚氨酯固化剂，所述水性聚氨酯树脂和水性聚氨酯固化剂的重量比为(65～97):(3～30)。
优选地，所述水性聚氨酯树脂的分子量为2000～10000，pH为7～9，不挥发份含量为30～50wt％。本申请中，所述不挥发份含量的测定方法为一定量的样品在容器中，放入烘箱干燥24h，取出冷却至室温称量。
本发明采用双组分水性体系，即在单组分水性聚氨酯体系中加入水性封闭异聚氨酯固化剂后，经热解封后裸露的异氰酸根基团可以与水性聚氨酯树脂的羟基反应，减少没反应完全的物质，同时形成稳定的三维结构。其中水性聚氨酯固化剂以及水性聚氨酯树脂和水性聚氨酯固化剂的比例比较关键。若水性聚氨酯树脂与水性聚氨酯固化剂高于本发明范围，残留有多余的OH基，抛光垫硬度反而降低，打磨损失比较大，耐磨性降低。若水性聚氨酯树脂与水性聚氨酯固化剂低于本发明范围，抛光垫太硬，去除速率升高平滑性变差。
优选地，所述水性聚氨酯固化剂为以下重量份的原料的反应产物：
多异氰酸酯10～40份
聚合物多元醇50～80份
扩链剂1～2份
封闭剂1～3份。
优选地，所述多异氰酸酯可以是10～20份，也可以是15～30份，也可以是25～40份；所述聚合物多元醇可以是50～60份，也可以是55～65份，也可以是60～70份，也可以是65～75份，也可以是70～80份；所述扩链剂可以是1～1.5份，也可以是1.3～1.8份，也可以是1.6～2份；所述封闭剂可以是1～2份，也可以是1.5～2.5份，也可以是2～3份。
优选地，所述多异氰酸酯选自二苯基甲烷二异氰酸酯、甲苯二异氰酸酯和六亚甲基二异氰酸酯中的一种或多种。
优选地，所述聚合物多元醇为由氨基、羟基封端的聚酯多元醇、聚醚多元醇、聚碳酸脂多元醇。
更优选地，所述聚合物多元醇选自己二酸乙二醇酯、聚乙二醇、聚四氢呋喃、聚碳酸亚己酯二醇中的一种或多种。
优选地，所述扩链剂选自二羟甲基丙酸、酒石酸、氨基酸、乙二氨基乙磺酸钠、2-磺酸钠-1,4丁二醇、N-甲基二乙醇胺、二亚乙基三胺和三(2-羟乙基)甲基氢氧化铵中的一种或多种。
优选地，所述封闭剂选自酚类化合物、肟类化合物、受阻酰化合物和亚硫酸盐中的一种或多种。
更优选地，所述封闭剂选自酚类化合物、肟类化合物、受阻酰化合物、亚硫酸盐中的一种或多种。更优选地，所述封闭剂选自苯酚、壬基酚、丁酮肟、丙酮肟、苯乙酮肟、2,6-二甲基-4-庚酮肟、乙醛肟、丙酮肟、丁酮肟、戊酮肟、环戊酮肟、环己酮肟、丙酮酸肟、乙醛酸肟、2-氧代环戊乙酸肟、己内酰胺、三羟甲基丙烷、1,2,4-三唑、2,2,6,6-四甲基-4-氧代哌啶、咪唑、亚硫酸氢钠、亚硫酸钠中的一种或几种。
本发明中双组分水性聚氨酯的制备方法如下：i)在聚合物多元醇中加入扩链剂，混合均匀；ii)边搅拌边加入多异氰酸酯，反应完全；iii)再加入封闭剂进行封端反应，得到双组分水性聚氨酯。优选地，步骤ii)中所述反应的温度为70～80℃，步骤iii)中所述封端反应的温度为100～110℃。
本发明的目的之二在于提供上述所述双组分水性聚氨酯用于聚氨酯复合抛光垫中作为改性涂层的用途。
本发明的目的之三在于提供一种聚氨酯复合抛光垫，包括基底材料层和附着在基底材料层表面的改性涂层，所述改性涂层采用如上述所述的双组分水性聚氨酯形成。
优选地，所述基底材料的原料纤维选自丙纶、涤纶、锦纶、粘胶纤维、腈纶、乙纶和氯纶中的一种；所述基底材料为织物、无纺布或编织布中的一种。
本发明的目的之四在于提供一种聚氨酯复合抛光垫的制备方法，包括以下步骤：
1)将水性聚氨酯树脂、水性聚氨酯固化剂混合配制成浸渍液；
2)将基底材料放入步骤1)中的浸渍液中进行浸渍；
3)将浸渍过的基底材料进行热固化，得到聚氨酯复合抛光垫。
优选地，步骤1)中，所述混合时还加入添加剂，所述添加剂选自以下原料中任一种或多种：
抗氧剂：所述抗氧剂选自亚硫酸钠、亚硫酸氢钠、焦亚硫酸钠和硫代硫酸钠中的一种或多种；
填料：所述填料选自无机非金属粉体、短纤维和耐磨聚合物中的一种或多种。具体地，无机非金属粉体为碳酸钙、石墨、白炭黑、硫酸钡、滑石粉、高岭土、多孔粉石英、沉淀硫酸钡、云母粉、硅灰石、膨润土中的一种或多种；短纤维为碳纤维、棉纤维、涤纶和尼龙中的一种或多种；耐磨聚合物为氟取代聚乙烯微粉、尼龙微粉、高强度改性环氧树脂、聚甲醛中的一种或多种。
表面活性剂：所述表面活性剂选自高分子型改性助剂、阳离子表面活性剂、阴离子表面活性剂和两性离子表面活性剂中的一种或多种。具体地，所述高分子型改性助剂包括有机氟类化合物、脂肪族二羧酸衍生物、明胶、聚乙烯吡咯烷酮、甲基纤维素、聚环氧乙烷和聚乙烯醇及其衍生物中的至少一种，更具体地，有机氟类化合物选自氟改性丙烯酸酯，脂肪族二羧酸衍生物选自二甲基乙酰胺(DMA)和己二酸二辛酯(DOA)中的一种或多种；所述阳离子表面活性剂包括有机胺类衍生物，更具体地，阳离子表面活性剂选自氯化烷基三甲基铵、氯化二烷基二甲基铵中的一种或多种；所述阴离子表面活性剂为烷基硫酸钠；所述两性离子表面活性剂选自炔二醇起始烷氧基化合物、烷基二甲基氨基醋酸甜菜碱类中的至少一种，更具体地，炔二醇起始烷氧基化合物选自2,5,8,11-四甲基-6-十二碳炔-5,8-二醇，烷基二甲基氨基醋酸甜菜碱类选自十二烷基二甲基氨基醋酸甜菜碱。
增粘剂：所述增粘剂选自聚醚类化合物、聚乙烯醇(PVA)、淀粉、纤维素类化合物甲基纤维素、羟丙基甲基纤维素、羧基甲纤维素、丙烯酸类聚合物、胶琼脂、胶体二氧化硅、胶体粘土、铝的氧化物、铝的氢氧化物、铁的氧化物和铁的氢氧化物中的一种或多种。更具体地，所述聚醚类化合物选自聚乙二醇和聚乙烯甲基醚中的一种或多种。
更优选地，按浸渍液的原料总重量为基准计，所述添加剂的量不超过5wt％。
优选地，步骤2)中，所述浸渍采用浸渍-辊压交替处理的方式，具体地，所述辊压采用胶辊装置进行，所述胶辊转速为1～5r/min，所述辊压的压力为9～11MPa。
本发明中所述浸渍-辊压交替处理，包括以下步骤：A)将双组分水性聚氨酯配制成的浸渍液放入浸渍槽中，在浸渍槽中间隔设置锟压装置；B)将基底材料放入浸渍槽中，基底材料浸渍于浸渍液中且在浸渍槽中移动，并在锟压装置下进行锟压；C)锟压后的基底材料，继续浸渍于水性聚氨酯树脂中且继续在浸渍槽中移动，并在下一个锟压装置下进行锟压；D)重复步骤C)后，取出基底材料。
优选地，步骤3)中，所述热固化温度为90～150℃，时间为3～90min。
更优选地，所述热固化采用热空气、红外灯、烘箱、烘道等方式进行。
本发明通过水性聚氨酯固化剂与水性聚氨树脂混合后以特定的工艺对基底材料进行处理，热解封出的异氰酸根基团可以与羟基反应，通过交联反应生成网状结构，不仅减少了异氰酸酯基与水的副反应，此外还能将纤维之间的氢键结合转变为化学键结合，形成稳定的三维结构，最终显著提高黏附纤维丝后复合抛光垫的硬度、强度、耐磨性能。
与现有技术相比，本发明具有以下有益效果：
1)传统单组分水性聚氨酯体系因浸渍料性能差不能满足半导体抛光去除率的要求，且在单组分体系中无论设计配方时各组分的量有多么的精准，活性基团都不能完全反应掉的，而聚氨酯树脂中的羟基过剩，会降低交联体型结构聚氨酯的最终性能。本发明采用双组分水性体系，即在单组分水性聚氨酯体系中加入水性封闭异聚氨酯固化剂后，经热解封后裸露的异氰酸根基团可以与水性聚氨酯树脂的羟基反应，减少没反应完全的物质，同时形成稳定的三维结构，最终显著提高黏附纤维丝后复合抛光垫的硬度、强度、耐磨性能。由于能够有效提高无纺布抛光垫摩擦性能，可延长抛光垫使用寿命。
2)传统单组分水性聚氨酯浸渍液的固化交联反应过于缓慢，导致体系粘度上升较慢，所制得的聚氨酯复合抛光垫微观形貌过于平坦，孔隙率降低。本发明采用双组分体系，可以通过添加剂调节固化速度来达到理想的凝胶反应同时减弱发泡反应，提高表面粗糙度，保留无纺布原有孔隙，提高承载抛光液能力。
3)传统单组分水性聚氨酯浸渍液往往固化较慢，所以制备得到的复合无纺布抛光垫固化时间久，影响生产加工效率。而本发明采用水性封闭聚氨酯固化剂在高温下解封进行反应，反应不仅可以调节，且比单组份湿固化效率高，大大缩短加工时间，提高生产加工效率。
具体实施方式
以下由特定的具体实施例说明本发明的实施方式，熟悉此技术的人士可由本说明书所揭露的内容轻易地了解本发明的其他优点及功效。
在进一步描述本发明具体实施方式之前，应理解，本发明的保护范围不局限于下述特定的具体实施方案；还应当理解，本发明实施例中使用的术语是为了描述特定的具体实施方案，而不是为了限制本发明的保护范围。下列实施例中未注明具体条件的试验方法，通常按照常规条件，或者按照各制造商所建议的条件。
当实施例给出数值范围时，应理解，除非本发明另有说明，每个数值范围的两个端点以及两个端点之间任何一个数值均可选用。除非另外定义，本发明中使用的所有技术和科学术语与本技术领域技术人员通常理解的意义相同。除实施例中使用的具体方法、设备、材料外，根据本技术领域的技术人员对现有技术的掌握及本发明的记载，还可以使用与本发明实施例中所述的方法、设备、材料相似或等同的现有技术的任何方法、设备和材料来实现本发明。
实施例1：
本实施例中，水性聚氨酯固化剂的原料配方如下：
| 原料类别 | 原料名称 | 原料重量份数 |
| 多异氰酸酯 | 甲苯二异氰酸酯(TDI) | 20份 |
| 聚合物多元醇 | 聚四氢呋喃 | 77份 |
| 扩链剂 | 三(2-羟乙基)甲基氢氧化铵 | 1份 |
| 封闭剂 | 苯酚 | 2份 |
本实施例中，水性聚氨酯固化剂的制备方法如下：在聚四氢呋喃中加入三(2-羟乙基)甲基氢氧化铵，混合均匀；边搅拌边加入甲苯二异氰酸酯(TDI)，进行聚合反应，聚合反应温度为75℃，反应完全后用甲乙酮降低粘度；然后加入苯酚进行封端反应，封端反应温度为100℃，最后减压除去甲乙酮溶剂，即得水性聚氨酯固化剂样品1#。
本实施例中，双组分水性聚氨酯的制备方法如下：将水性聚氨酯树脂预分散在水中，再将水性聚氨酯固化剂样品1#倒入其中混合均匀，其中水性聚氨酯树脂和水性聚氨酯固化剂样品1#的重量比95：5。其中水性聚氨酯树脂的分子量为6210，pH为7.6，不挥发份含量为41％。
本实施例中，聚氨酯复合抛光垫的制备方法如下：将双组分水性聚氨酯混合均匀，配制成浸渍液；选择聚酯制备的无纺布作为基底材料，将其浸渍于前述浸渍液，采用浸渍-辊压交替处理2h，即将基底材料放入浸渍槽中，基底材料浸渍于前述浸渍液，胶辊以4r/min的转速转动，并给予10MPa的压力进行锟压；再将基底材料放入烘箱中，在100℃烘20min，并使烘干后的基底材料的重量保持恒重并进行抛光打磨，即得聚氨酯复合抛光垫样品1*。
实施例2：
本实施例中，水性聚氨酯固化剂的原料配方如下：
| 原料类别 | 原料名称 | 原料重量份数 |
| 多异氰酸酯 | 二苯基甲烷二异氰酸酯(MDI) | 30份 |
| 聚合物多元醇 | 聚乙二醇(PEG) | 66份 |
| 扩链剂 | 三(2-羟乙基)甲基氢氧化铵 | 1份 |
| 封闭剂 | 壬基酚 | 2份 |
本实施例中，水性聚氨酯固化剂的制备方法如下：在聚乙二醇(PEG)中加入三(2-羟乙基)甲基氢氧化铵，混合均匀；边搅拌边加入二苯基甲烷二异氰酸酯(MDI)，进行聚合反应，聚合反应温度为70℃，反应完全后用甲乙酮降低粘度；然后加入苯酚进行封端反应，封端反应温度为105℃，最后减压除去甲乙酮溶剂，即得水性聚氨酯固化剂样品2#。
本实施例中，双组分水性聚氨酯的制备方法如下：将水性聚氨酯树脂预分散在水中，再将水性聚氨酯固化剂样品2#倒入其中混合均匀，其中水性聚氨酯树脂和水性聚氨酯固化剂样品2#的重量比90：10。其中水性聚氨酯树脂的分子量为2014，pH为8.1，不挥发份含量为32％。
本实施例中，聚氨酯复合抛光垫的制备方法如下：将双组分水性聚氨酯混合均匀，配制成浸渍液；选择聚酯制备的无纺布作为基底材料，将其浸渍于前述浸渍液，采用浸渍-辊压交替处理2h，即将基底材料放入浸渍槽中，基底材料浸渍于前述浸渍液中，胶辊以3r/min的转速转动，并给予10MPa的压力进行锟压；再将基底材料放入烘箱中，在140℃烘5min，并使烘干后的基底材料的重量保持恒重并进行抛光打磨，即得聚氨酯复合抛光垫样品2*。
实施例3：
本实施例中，水性聚氨酯固化剂的原料配方如下：
| 原料类别 | 原料名称 | 原料重量份数 |
| 多异氰酸酯 | 六亚甲基二异氰酸酯(HDI) | 16.5份 |
| 聚合物多元醇 | 己二酸乙二醇酯 | 80份 |
| 扩链剂 | 二羟甲基丙酸 | 1份 |
| 封闭剂 | 丙酮肟 | 2.5份 |
本实施例中，水性聚氨酯固化剂的制备方法如下：在己二酸乙二醇酯中加入二羟甲基丙酸，混合均匀；边搅拌边加入六亚甲基二异氰酸酯(HDI)，进行聚合反应，聚合反应温度为75℃，反应完全后用甲乙酮降低粘度；然后加入苯酚进行封端反应，封端反应温度为110℃，最后减压除去甲乙酮溶剂，即得水性聚氨酯固化剂样品3#。
本实施例中，双组分水性聚氨酯的制备方法如下：将水性聚氨酯树脂预分散在水中，再将水性聚氨酯固化剂样品3#倒入其中混合均匀，其中水性聚氨酯树脂和水性聚氨酯固化剂样品3#的重量比70：30。其中水性聚氨酯树脂的分子量为9807，pH为7.2，不挥发份含量为41％。
本实施例中，聚氨酯复合抛光垫的制备方法如下：将双组分水性聚氨酯混合均匀，配制成浸渍液；选择聚酯制备的无纺布作为基底材料，将其浸渍于前述浸渍液，采用浸渍-辊压交替处理2h，即将基底材料放入浸渍槽中，基底材料浸渍于前述浸渍液中，胶辊以2r/min的转速转动，并给与9MPa的压力进行锟压；再将基底材料放入烘箱中，在120℃烘10min，并使烘干后的基底材料的重量保持恒重并进行抛光打磨，即得聚氨酯复合抛光垫样品3*。
实施例4：
本实施例中，水性聚氨酯固化剂的原料配方如下：
| 原料类别 | 原料名称 | 原料重量份数 |
| 多异氰酸酯 | 二苯基甲烷二异氰酸酯(MDI) | 20.5份 |
| 聚合物多元醇 | 聚碳酸亚己酯二醇 | 75份 |
| 扩链剂 | 二羟甲基丙酸 | 2份 |
| 封闭剂 | 壬基酚 | 2.5份 |
本实施例中，水性聚氨酯固化剂的制备方法如下：在聚碳酸亚己酯二醇中加入二羟甲基丙酸，混合均匀；边搅拌边加入二苯基甲烷二异氰酸酯(MDI)，进行聚合反应，聚合反应温度为80℃，反应完全后用甲乙酮降低粘度；然后加入壬基酚进行封端反应，封端反应温度为110℃，最后减压除去甲乙酮溶剂，即得水性聚氨酯固化剂样品4#。
本实施例中，双组分水性聚氨酯的制备方法如下：将水性聚氨酯树脂预分散在水中，再将水性聚氨酯固化剂样品4#倒入其中混合均匀，其中水性聚氨酯树脂和水性聚氨酯固化剂样品1#的重量比97：3。其中水性聚氨酯树脂的分子量为8007，pH为8.1，不挥发份含量为48％。
本实施例中，聚氨酯复合抛光垫的制备方法如下：将双组分水性聚氨酯和添加剂按重量比98：2混合，配制成浸渍液；选择聚酯制备的无纺布作为基底材料，将其浸渍于前述浸渍液，采用浸渍-辊压交替处理2h，即将基底材料放入浸渍槽中，基底材料浸渍于前述浸渍液中，胶辊以4r/min的转速转动，并给与10MPa的压力进行锟压；再将基底材料放入烘箱中，在120℃烘20min，并使烘干后的基底材料的重量保持恒重并进行抛光打磨，即得聚氨酯复合抛光垫样品4*。
实施例5：
本实施例中，水性聚氨酯固化剂的原料配方如下：
| 原料类别 | 原料名称 | 原料重量份数 |
| 多异氰酸酯 | 甲苯二异氰酸酯(TDI) | 38份 |
| 聚合物多元醇 | 聚四氢呋喃(PTMEG) | 58份 |
| 扩链剂 | 2-磺酸钠-1，4丁二醇 | 1份 |
| 封闭剂 | 苯酚 | 2份 |
本实施例中，水性聚氨酯固化剂的制备方法如下：在聚四氢呋喃(PTMEG)中加入2-磺酸钠-1,4丁二醇，混合均匀；边搅拌边加入甲苯二异氰酸酯(TDI)，进行聚合反应，聚合反应温度为76℃，反应完全后用甲乙酮降低粘度；然后加入苯酚进行封端反应，封端反应温度为108℃，最后减压除去甲乙酮溶剂，即得水性聚氨酯固化剂样品5#。
本实施例中，双组分水性聚氨酯的制备方法如下：将水性聚氨酯树脂预分散在水中，再将水性聚氨酯固化剂样品5#倒入其中混合均匀，其中水性聚氨酯树脂和水性聚氨酯固化剂样品1#的重量比65：35。其中水性聚氨酯树脂的分子量为8207，pH为8.3，不挥发份含量为37％。
本实施例中，聚氨酯复合抛光垫的制备方法如下：将双组分水性聚氨酯和添加剂按重量比96：4混合，配制成浸渍液；选择聚酰制备的无纺布作为基底材料，将其浸渍于前述浸渍液，采用浸渍-辊压交替处理2h，即将基底材料放入浸渍槽中，基底材料浸渍于前述浸渍液中，胶辊以2r/min的转速转动，并给与9MPa的压力进行锟压；再将基底材料放入烘箱中，在140℃烘10min，并使烘干后的基底材料的重量保持恒重并进行抛光打磨，即得聚氨酯复合抛光垫样品5*。其中所述添加剂由芳香族仲胺、环氧树脂、羟丙基甲基纤维素、氯化烷基三甲基铵按照重量比2：50：20：28组成。
对比例1：
浸渍液配制：100％水性聚氨酯树脂溶液，无水性聚氨酯固化剂和添加剂，其余步骤同实施例1)。其中水性聚氨酯树脂的参数同实施例1。
对比例2：
浸渍液配制：由水性聚氨酯树脂与添加剂按照重量比98：2配制而成，添加剂的成分及配比与实施例4相同，其余步骤同实施例1)。其中水性聚氨酯树脂的参数同实施例1。
对比例3
浸渍液配制：由水性聚氨酯树脂与水性聚氨酯固化剂按照重量比95：5配制而成，水性聚氨酯固化剂的成分及配比与实施例2相同，其余步骤同实施例1。其中水性聚氨酯树脂的参数同实施例1。
对比例4
浸渍液配制：由水性聚氨酯树脂与水性聚氨酯固化剂按照重量比60：40配制而成，水性聚氨酯固化剂的成分及配比与实施例2相同，其余步骤同实施例1。其中水性聚氨酯树脂的参数同实施例1。
将聚氨酯复合抛光垫1～5和对比例1～4分别进行耐磨性测试、硬度测试等性能测试，其实验结果如表所示。其中，
硬度测试：依照标准《GB/T 2411-2008塑料和硬橡胶使用硬度计测定压痕硬度(邵氏硬度)》进行；
抛光垫压缩比和压缩弹性率测试：依照《GB/T 24442.1-2009纺织品压缩性能的测定第1部分：恒定法》进行；
耐磨性测试：具体方法为100目砂纸粘贴在抛光机的上盘，转速80r/min，抛光垫下盘转速40r/min，打磨5min，记录前后损失质量，其中抛光机为沈阳科晶自动化设备有限公司，型号UNIPOL-1200S；
去粗速率：采用沈阳科晶自动化设备有限公司的UNIPOL-1200S型抛光机对2in蓝宝石片进行抛光1h，抛光液流速100ml/min压力100KPa；
表面划痕数量：依照标准GB/T 6624-2009《硅抛光片表面质量目测检验方法》进行。
由表可知，与对比例1～2相比，实施例1～5所制备的聚氨酯复合抛光垫的硬度、去除速率和划痕数量更高，压缩弹性率、打磨损失和压缩比更低。对比例3中水性聚氨酯树脂与水性聚氨酯固化剂高于本发明范围，抛光垫硬度反而降低，打磨损失比较大，耐磨性降低。对比例4中水性聚氨酯树脂与水性聚氨酯固化剂低于本发明范围，抛光垫太硬，去除速率升高平滑性变差。
上述实施例仅例示性说明本发明的原理及其功效，而非用于限制本发明。任何熟悉此技术的人士皆可在不违背本发明的精神及范畴下，对上述实施例进行修饰或改变。因此，举凡所属技术领域中具有通常知识者在未脱离本发明所揭示的精神与技术思想下所完成的一切等效修饰或改变，仍应由本发明的权利要求所涵盖。
Claims (8)
1.一种双组分水性聚氨酯，其特征在于，包括水性聚氨酯树脂和水性聚氨酯固化剂，所述水性聚氨酯树脂和所述水性聚氨酯固化剂的重量比为(65~97):(3~30)；
所述水性聚氨酯固化剂为以下重量份的原料的反应产物：
多异氰酸酯10～40份
聚合物多元醇50～80份
扩链剂1～2份
封闭剂1～3份；
所述多异氰酸酯选自二苯基甲烷二异氰酸酯、甲苯二异氰酸酯和六亚甲基二异氰酸酯中的一种或多种；
所述聚合物多元醇选自己二酸乙二醇酯、聚乙二醇、聚四氢呋喃、聚碳酸亚己酯二醇中的一种或多种；
所述扩链剂选自二羟甲基丙酸、酒石酸、氨基酸、乙二氨基乙磺酸钠、2-磺酸钠-1,4丁二醇、N-甲基二乙醇胺、二亚乙基三胺和三(2-羟乙基)甲基氢氧化铵中的一种或多种；
所述封闭剂选自酚类化合物、肟类化合物、受阻酰化合物和亚硫酸盐中的一种或多种。
2.根据权利要求1所述双组分水性聚氨酯用于聚氨酯复合抛光垫中作为改性涂层的用途。
3.一种聚氨酯复合抛光垫，其特征在于，包括基底材料层和附着在基底材料层表面的改性涂层，所述改性涂层采用如权利要求1所述的双组分水性聚氨酯形成。
4.根据权利要求3所述的聚氨酯复合抛光垫的制备方法，其特征在于，包括如下步骤：
1）将水性聚氨酯树脂、水性聚氨酯固化剂混合配制成浸渍液；
2）将基底材料放入步骤1）中的浸渍液中进行浸渍；
3）将浸渍过的基底材料进行热固化，得到聚氨酯复合抛光垫。
5.根据权利要求4所述的聚氨酯复合抛光垫的制备方法，其特征在于，步骤1）中，所述混合时还加入添加剂，所述添加剂选自以下原料中任一种或多种：
抗氧剂：所述抗氧剂选自亚硫酸钠、亚硫酸氢钠、焦亚硫酸钠和硫代硫酸钠中的一种或多种；
填料：所述填料选自无机非金属粉体、短纤维和耐磨聚合物中的一种或多种；
表面活性剂：所述表面活性剂选自高分子型改性助剂、阳离子表面活性剂、阴离子表面活性剂和两性离子表面活性剂中的一种或多种；
增粘剂：所述增粘剂选自聚醚类化合物、PVA、淀粉、纤维素类化合物甲基纤维素、羟丙基甲基纤维素、羧基甲纤维素、丙烯酸类聚合物、胶琼脂、胶体二氧化硅、胶体粘土、铝的氧化物、铝的氢氧化物、铁的氧化物和铁的氢氧化物中的一种或多种。
6.根据权利要求5所述的聚氨酯复合抛光垫的制备方法，其特征在于，步骤1）中，按浸渍液的原料的总重量为基准计，所述添加剂的量不超过5wt%。
7.根据权利要求4所述的聚氨酯复合抛光垫的制备方法，其特征在于，步骤2）中，所述浸渍采用浸渍-辊压交替处理的方式，所述辊压采用胶辊装置进行，所述胶辊转速为1~5r/min，辊压压力为9~11Mpa。
8.根据权利要求4所述的聚氨酯复合抛光垫的制备方法，其特征在于，步骤3）中，所述热固化温度为90~150℃，热固化时间为3~90min。
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