CN101636464B - 防水材料用湿气固化型尿烷组合物及聚氨酯防水材料 - Google Patents
防水材料用湿气固化型尿烷组合物及聚氨酯防水材料 Download PDFInfo
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- CN101636464B CN101636464B CN2008800084419A CN200880008441A CN101636464B CN 101636464 B CN101636464 B CN 101636464B CN 2008800084419 A CN2008800084419 A CN 2008800084419A CN 200880008441 A CN200880008441 A CN 200880008441A CN 101636464 B CN101636464 B CN 101636464B
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Classifications
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
本发明通过如下所述的尿烷组合物,提供一种由于消泡性与流平性优异而赋予防水性、表面美观性优异的防水层的防水材料。一种尿烷组合物,其含有如下成分:尿烷预聚物(A);含噁唑啉的尿烷化合物(B);填充剂(E);增塑剂(F);以及溶剂(G);其中,相对于100重量份前述尿烷组合物,含有0.01~5重量份乙烯-α-烯烃共低聚物(C)、以及0.1~5重量份作为由丙烯腈或其改性体形成的聚合物的、平均粒径100μm以下的表面处理有机中空填料(D),前述乙烯-α-烯烃共低聚物(C)的添加量与前述有机中空填料(D)的添加量的重量比为(C)/(D)=0.01~10。
Description
技术领域
本发明涉及一种防水材料用湿气固化型尿烷组合物,其是在固化时没有涂膜发泡、固化性优异的防水材料用单成分湿气固化型尿烷组合物,特别是由于消泡性与流平性优异,因而提供表面的美观优异的固化物。
背景技术
目前,在专利文献1中公开了一种湿气固化型尿烷组合物,但其还存在如下问题:由于固化时水分与异氰酸酯基反应时产生的碳酸气体,因而有时发生涂膜膨胀的问题。
因此,为了抑制引起膨胀的碳酸气体的产生,提出了酮亚胺、烯胺等湿气离解型的交联剂的方案,其中,使用噁唑啉化合物的组合物是不会产生碳酸气体且性能比较平衡的材料,因而作为防水材料被涂布施用。(专利文献2~4)
湿气固化型防水材料不需要在施用现场将主剂与固化剂混合、能够在罐开封后立即涂布施用,但为了防止填充剂沉降以及填充剂与液体成分分离,需要提高流变性。其结果是,产生如下问题:使用噁唑啉化合物的单成分湿气固化型尿烷组合物与现有的双成分固化型尿烷相比,消泡性与流平性变更差。
另外,作为尿烷组合物的消泡剂,已知在申请人的以往申请中提出了使用乙烯-α-烯烃共低聚物的方案(专利文献5)。然而,即使将该消泡剂用于具有噁唑啉系化合物的单成分湿气固化型尿烷组合物,也不能得到实用的消泡性。(参照比较例2)
专利文献1:日本特开昭57-94056号公报
专利文献2:日本特开平6-293821号公报
专利文献3:日本特开平7-33852号公报
专利文献4:日本特开平7-10949号公报
专利文献5:日本特开平5-247161号公报
发明内容
发明所要解决的问题
本发明的目的在于,提供一种防水材料用单成分湿气型尿烷组合物及防水材料,其通过提高具有噁唑啉系化合物的尿烷组合物的消泡性与流平性,从而提供防水性、表面的美观性优异的固化物。
用于解决问题的方法
本发明人等对于上述课题进行深入研究,结果发现,通过添加特定量的特定消泡剂与特定的中空填料,从而解决上述问题并完成本发明。
即,本发明提供一种防水材料用湿气固化型尿烷组合物及使用其的防水材料,其特征在于,该尿烷组合物含有如下成分:使多异氰酸酯与聚氧化烯多元醇反应而获得的末端具有2个以上异氰酸酯基的尿烷预聚物(A);使多异氰酸酯或通过多异氰酸酯与聚氧化烯多元醇反应而获得且末端含有2个以上异氰酸酯基的尿烷预聚物(b1)与N-2-羟烷基噁唑啉(b2)反应获得的末端具有至少一个以上噁唑啉基的含噁唑啉的尿烷化合物(B);填充剂(E);增塑剂(F);以及溶剂(G);其中,相对于100重量份前述尿烷组合物,含有0.01~5重量份乙烯-α-烯烃共低聚物(C)、以及0.1~5重量份作为由丙烯腈或其改性体形成的聚合物的、平均粒径100μm以下的表面处理有机中空填料(D),前述乙烯-α-烯烃共低聚物(C)的添加量与前述有机中空填料(D)的添加量的重量比为(C)/(D)=0.01~10。
发明效果
本发明是由含有噁唑啉化合物的防水材料用尿烷组合物、乙烯-α-烯烃共低聚物(C)以及由丙烯腈或其改性体形成的聚合物,通过含有特定量的平均粒径100μm以下的表面处理有机中空填料(D),平衡性良好地改良了消泡性和流平性,从而能够提供防水性与表面美观优异的防水性固化物。
具体实施方式
用于本发明的使多异氰酸酯与聚氧化烯多元醇反应而获得的末端具有2个以上异氰酸酯基的尿烷预聚物(A)是指,将多异氰酸酯与多元醇、例如聚氧乙二醇、聚氧丙二醇、聚氧丁二醇等聚氧化烯多元醇在过量多异氰酸酯的基础上通过常规方法调制得到的尿烷预聚物。
另外,末端具有2个以上异氰酸酯基的尿烷预聚物(b1)是指,将多异氰酸酯与同上述一样的聚氧化烯多元醇在过量多异氰酸酯的基础上通过常规方法调制得到的尿烷预聚物。
前述聚氧化烯多元醇是指,将乙二醇、丙二醇、水、甘油、TMP(三羟甲基丙烷)、季戊四醇等与环氧乙烷、环氧丙烷、环氧丁烷单个或其中2种以上通过公知的方法进行加成而获得的多元醇。
作为用于本发明的多异氰酸酯,可列举出例如、2,4-甲苯二异氰酸酯、2,6-甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、一部份被碳二亚胺化的二苯基甲烷二异氰酸酯、聚甲撑基聚苯基多异氰酸酯、甲苯二异氰酸酯、萘二异氰酸酯、苯撑二异氰酸酯、六甲撑二异氰酸酯、异佛乐酮二异氰酸酯、二甲苯二异氰酸酯、氢化二甲苯二异氰酸酯、氢化二苯基甲烷二异氰酸酯、环己烷二异氰酸酯等芳香族二异氰酸酯、脂肪族二异氰酸酯、脂环式二异氰酸酯的1种或2种以上的混合物。
作为尿烷预聚物(A)的组成成分的聚氧化烯多元醇优选数均分子量500~16000的二元醇或三元醇。
特别地,尿烷预聚物(A)的聚氧化烯多元醇成分优选亚乙基醚键0~10重量%及亚丙基醚键10~95重量%的范围。
尿烷预聚物(A)的末端异氰酸酯基数优选2以上、更优选2~3。进而,异氰酸酯与多元醇的NCO/OH比优选1.4以上、进一步优选1.4~5.0、特别优选1.5~3.0。尿烷预聚物(A)的残留NCO%优选1~20重量%,更优选1~5重量%。
本发明中使用的含噁唑啉的尿烷化合物(B)是使多异氰酸酯或通过多异氰酸酯与聚氧化烯多元醇反应而获得且末端含有2个以上异氰酸酯基的尿烷预聚物(b1)与N-2-羟烷基噁唑啉(b2)反应获得的末端具有至少一个以上噁唑啉基的含噁唑啉的尿烷化合物(B)。
所述尿烷预聚物的聚氧化烯多元醇优选具有氧化乙烯链。其中,即使是将不具有氧化乙烯链的多元醇与具有氧化乙烯链的多元醇混合而得到的多元醇也能够用作(b1)成分。另外,优选氧化烯链中的氧化乙烯链的平均含量为1~30重量%。氧化乙烯链的含量为上述范围时固化速度高、而且固化性、耐水性优异。其中,计算(A)成分、(B)成分的氧化乙烯链量,算出其总和,其氧化乙烯链的含量相对于(A)成分与(B)成分的总量优选不足10重量%。若在该范围则获得优选的耐水性。
前述尿烷预聚物(b1)优选数均分子量为500~8000。数均分子量为500~8000的情况下,能满足基底追随性、固化速度。另外,尿烷预聚物(b1)的末端的平均NCO基数优选为2.0~2.6。若是所述NCO基数,则结果是固化性及基底追随性更好。进而,异氰酸酯与多元醇的NCO/OH比优选1.6以上、进一步优选1.8~4.0。残留NCO%优选1~15重量%。
另外,尿烷预聚物(b1)与N-2-羟烷基噁唑啉(b2)的反应摩尔比优选NCO/OH=0.95~3.0。NCO/OH摩尔比若在所述范围的话,得到未反应的N-2-羟烷基噁唑啉残留倾向低、贮藏稳定性好的结果,而且能够容易地抑制固化速度降低和粘度上升。
另外,用于含噁唑啉的尿烷化合物(B)合成的N-2-羟烷基噁唑啉(b2)是通过例如甲醛、乙醛、丙醛、丁醛、苯醛等醛类与例如二乙醇胺、二丙醇胺等二羟烷基胺类进行公知缩合反应而获得的化合物。
含噁唑啉的尿烷化合物(B)的末端噁唑啉基的数优选1~3。若在该范围的话,固化后的拉伸性高,故优选。另外,尿烷噁唑啉预聚物(B)的末端具有1个以上噁唑啉基的话,则其他末端当然可以为异氰酸酯基。
对于预聚物(A)与含噁唑啉的尿烷化合物(B)的比例,预聚物(A)的NCO基与用水开环含噁唑啉的尿烷化合物(B)而产生的活性氢基之比优选为0.4~4.0的范围。若为该范围的话,则碳酸气体的产生少且能够抑制涂膜膨胀,贮藏稳定性优异。考虑到这些的话,则(A)与(B)的混合比优选在以重量比60∶1~1∶30的范围。
本发明的组合物除了含有前述(A)、(B)、(E)、(F)、(G)成分以外,为了消泡性和流平性,还需要含有特定量的(C)乙烯-α-烯烃共低聚物、(D)特定量的由丙烯腈或其改性体形成的聚合物、以及平均粒径100μm以下的有机中空填料。
本发明中所用的乙烯-α-烯烃共低聚物(C)由乙烯与α-烯烃共聚而得,并优选数均分子量为50~3000、更优选为500~2500。作为α-烯烃共低聚物,可列举出例如丙烯、1-丁烯、4-甲基-1-戊烯、2-甲基-1戊烯。作为乙烯-α-烯烃共低聚物的代表的性状,优选比重0.80~0.90、动力粘度50~50000cSt、碘值1.0以下,动力粘度低则混合性良好但容易分离,动力粘度高则混合性变差但不易分离,因而需要考虑相对于添加对象适宜的混合性、分离性来进行选择。作为满足上述要件的乙烯-α-烯烃共低聚物(C)的市售品,可列举出例如三井化学(株)制的ル一カントHC-20、HC-40、HC-100、HC-600等。乙烯-α-烯烃共低聚物(C)的添加量相对于由前述(A)、(B)、(E)、(F)、(G)的总计100重量份组成的组合物,为0.01~5重量份、优选为0.05~3重量份。若配合不足0.01重量份,则消泡效果少;若配合超过5重量份,则组合物的表面大量浮起、与最上涂层之间的粘接性变差。另外,组合物的表面也会变模糊。
作为前述表面处理有机中空填料(D),是将由丙烯腈或其改性体形成的聚合物作为外皮的中空球状颗粒,平均粒径100μm以下的粒状物。然而,在不损害本发明效果的范围内,还可以组合使用玻璃球、二氧化硅球、白砂球等无机球。优选使偏二氯乙烯、丙烯腈等共聚而得的有机球。通常在制造混合无机球时球大多被破坏,因而本发明优选不使用。另外,若平均粒径超过100μm,则存在中空填料(D)在组合物中分离的倾向,因而不优选使用。若平均粒径为100μm以下,则不分离,更优选为80μm以下、10μm以上。作为市售品,可列举出MFL-80GCA、MFL-80CA(松本油脂制品)等。
前述平均粒径100μm以下的表面处理有机中空填料(D)通过与前述乙烯-α-烯烃共低聚物(C)组合使用,能够突破性地提高组合物的流平性、消泡性。
进而,前述中空填料(D)的表面是经过处理的,作为其处理剂,有由碳酸钙、滑石或氧化钛的至少1种覆盖的前述中空填料(D),该中空填料(D)与聚氨酯树脂的比重差少,在组合物中难以分离,故优选使用。特别优选由碳酸钙表面处理覆盖。
前述中空填料(D)的添加量相对于前述(A)、(B)、(E)、(F)、(G)的总计100重量份,使用0.1~5.0重量份,优选0.2~3重量份。若添加量不足0.1重量份,则消泡性、流平性的效果少;若超过5.0重量份,则组合物的粘度变高、操作性降低,故不优选。
作为本发明中使用的无机填充剂(E),可列举出例如碳酸钙、氧化钙、粘土、滑石、氧化钛、硫酸铝、高岭土、硅藻土等无机化合物的粉粒体。其添加量在组合物中优选5~70重量%、更优选10~60重量%。
作为本发明中使用的增塑剂(F),可列举出例如邻苯二甲酸二丁酯、邻苯二甲酸二辛酯、邻苯二甲酸二(十一烷)酯、邻苯二甲酸二月桂酯、邻苯二甲酸丁基苄基酯、邻苯二甲酸二异癸酯、己二酸二丁酯、己二酸二辛酯、己二酸二异壬酯、壬二酸二辛酯、癸二酸二辛酯等酯系增塑剂、磷酸三辛酯、磷酸三苯酯等磷酸酯系增塑剂。
作为本发明中使用的溶剂(G),可列举出例如二甲苯、甲苯、石油系高沸点芳香族系馏分、石油树脂等,可以混合1种以上。
本发明的组合物在用于这些用途中时,还可以根据需要包含催化剂、触变剂、体质颜料、用于保持耐侯性的防紫外线剂、稳定剂等各种添加剂等。可以通过能够将这些混合物均匀混合且充分确保保存性的混合、混炼装置来制造。
作为前述触变剂,可列举出表面处理碳酸钙、聚氯化乙烯粉末、微粉末二氧化硅、膨润土等。
作为催化剂,可以使用公知的辛酸、丙酸、对苯二甲酸、水杨酸、铅、DBTDL等催化剂。
作为稳定剂,可列举出例如抗氧化剂、紫外线吸收剂等,可以添加到组合物中。
本发明的防水材料用作涂布于阳台、屋上等的水泥面、现有的地板面、壁面的建筑物的防水材料,通过喷涂、刷涂等涂布。
实施例
接着,通过实施例、比较例详细地说明本发明,本发明并不限于这些实施例。以下,份和%没有特别限定则都是重量基准。
<(A)成分的合成>
(尿烷预聚物的制作例1)
在氮气气流下于80℃,在烧瓶中向数均分子量2000的聚丁烯醚二元醇700g(0.35摩尔)、数均分子量3000的聚丙烯醚三元醇300g(0.1摩尔)中加入2,4-甲苯二异氰酸酯191.4g(1.1摩尔)、即NCO/OH的当量比2.2,边搅拌边使其反应15小时,得到NCO%为4.25%的尿烷预聚物(A-1)。
(尿烷预聚物的制作例2)
代替尿烷预聚物的制作例1中的数均分子量2000的聚丁烯醚二元醇700g(0.35摩尔)使用数均分子量2000的聚丙烯醚二元醇700g(0.35摩尔),除此以外以相同方法进行合成,得到NCO%为4.28%的尿烷预聚物(A-2)。
<含噁唑啉基尿烷化合物(B)成分的合成>
(尿烷噁唑啉预聚物的制作例1)
混合数均分子量4800、氧化乙烯链的含量15%的聚乙烯丙烯醚三元醇500g(0.104摩尔)与数均分子量2000的聚丙烯醚二元醇500g(0.25摩尔),得到氧化乙烯链的平均含量7.5%、平均官能团数2.29、数均分子量2820的多元醇。进一步,在氮气气流下于80℃,在烧瓶中将六甲撑二异氰酸酯143.3g(0.853摩尔)、即NCO/OH的当量比2.1边搅拌边使其反应48小时,得到NCO%为3.28%、每1分子的末端NCO基数2.29的尿烷预聚物(b1-1)。
在氮气气流下于60℃下,在烧瓶中将尿烷预聚物(b1-1)140.8g与2-异丙基3(2羟乙基)1,3噁唑啉15.9g、即NCO/OH的当量比1.1,边搅拌边使其反应48小时,得到尿烷噁唑啉预聚物(OXZ-1)。测定该组合物的GPC,结果确认残留的2-异丙基-3-(2羟乙基)-1,3噁唑啉的含有率为1%以下。
<配合物的配合>
接着,将表中记载的原料放入密闭型行星式搅拌器中,均匀混合后,以50托脱泡5分钟,得到试样。
另外,碳酸钙粉末(NS-200、日东粉化制)使用预先在120℃下干燥,确认到水分为500ppm以下的物质。
[试验方法]
(粘度的测定)
将试样调节到25℃,使用BM型旋转粘度计测定粘度。
(消泡性试验)
在围上四边的瓦楞板(30cm×30cm)上按照厚1.5mm的比例涂布试样,在室温25℃×湿度50%的条件下使用镘刀使其整个面起泡。测定直到泡全部破泡并消失的时间。
(中空填料分离性试验)
将试样200g密闭在200CC的玻璃容器中,并在50℃氛围下培养7天后,目视观察中空填料是否分离。
(流平性试验)
将试样放入150mL聚乙烯杯(容量200cc)中后,在瓦楞板(30×30cm)上将聚乙烯杯口朝下倒扣并不使试样从聚乙烯杯中露出。接着,将聚乙烯杯垂直地拿起,使试样呈圆形地自然扩展。将聚乙烯杯拿起后经过10分钟,然后,测定呈圆形扩展的试样的平均直径(cm),按照以下判定基准进行判定。
判定基准:
○:30cm以上、
△:25~不足30cm、
×:不足25cm
(固化性试验)
在围上四边的铺面板(30×30cm)上按厚1.5mm的比例涂布试样,在室温25℃×湿度50%的条件下培养,将直至在涂膜表面能够步行(不粘鞋底的状态)的时间作为固化时间。
(防水性能试验)
使用试样制作1mm厚的片材(30cm×30cm)。使用针孔试验机对片材施加电压,确认是否由针孔(导通孔)导致电流流入,将没有电流流入的情况判定为防水性能良好“○”、将有电流流入的情况判定为防水性能不良“×”。
表-1配合条件及试验结果
[表1]
备注
HC-40、HC-600:三井化学制“ル一カント”、乙烯-α-烯烃低聚物
MFL-80GCA:松本油脂制、表面经过碳酸钙处理的丙烯腈系中空填料、平均粒径20μm
MFL-80CA:松本油脂制、表面经过碳酸钙处理的丙烯腈系中空填料、平均粒径100μm
炭カルNS-200:日东粉化制、碳酸钙粉末
DOP:邻苯二甲酸二辛酯
RY-200S:日本アエロジル制、疏水性二氧化硅粉末
表-2配合条件及试验结果
[表2]
比较例1中丙烯腈系中空填料和乙烯-α-烯烃共低聚物均不含有,因此相比于实施例,得到消泡时间变长、流平性变差的结果。
比较例2虽然含有乙烯-α-烯烃共低聚物,但由于不含有丙烯腈系中空填料,因而得到了比实施例的消泡时间长、流平性差的结果。
比较例3虽然含有丙烯腈系中空填料,但由于不含有乙烯-α-烯烃共低聚物,因而得到了比实施例消泡时间长、流平性变差的结果。
比较例4虽然含有丙烯腈系中空填料,但由于乙烯-α-烯烃共低聚物量少,因而得到了比实施例消泡时间长、流平性变差的结果。
比较例5虽然含有丙烯腈系中空填料和乙烯-α-烯烃共低聚物,但由乙烯-α-烯烃共低聚物/丙烯腈系中空填料之比过小,因而得到了比实施例消泡时间长、流平性变差的结果。
比较例6虽然含有丙烯腈系中空填料和乙烯-α-烯烃共低聚物,但由于乙烯-α-烯烃共低聚物/丙烯腈系中空填料之比过大,因而得到了比实施例消泡时间长、流平性变差的结果。
产业上的可利用性
本发明由于能够提高具有噁唑啉系化合物的尿烷组合物的消泡性与流平性,因而可以涂布到土木建筑物,形成表面的美观性、防水性优异的防水层。
Claims (3)
1.一种防水材料用湿气固化型尿烷组合物,其特征在于,该尿烷组合物含有如下成分:
使多异氰酸酯与聚氧化烯多元醇反应而获得的末端具有2个以上异氰酸酯基的尿烷预聚物(A);
使多异氰酸酯或通过多异氰酸酯与聚氧化烯多元醇反应而获得且末端含有2个以上异氰酸酯基的尿烷预聚物(b1)与N-2-羟烷基噁唑啉(b2)反应获得的末端具有至少一个以上噁唑啉基的含噁唑啉的尿烷化合物(B);
填充剂(E);
增塑剂(F);
以及溶剂(G);
其中,相对于100重量份前述尿烷组合物,含有0.01~5重量份乙烯-α-烯烃共低聚物(C)、以及0.1~5重量份作为由丙烯腈或其改性体形成的聚合物的、平均粒径100μm以下的表面处理有机中空填料(D),前述乙烯-α-烯烃共低聚物(C)的添加量与前述有机中空填料(D)的添加量的重量比为(C)/(D)=0.01~10。
2.根据权利要求1所述的防水材料用湿气固化型尿烷组合物,前述中空填料(D)的表面处理通过碳酸钙、滑石或氧化钛的1种以上被覆。
3.一种防水材料,其使用权利要求1或2所述的防水材料用湿气固化型尿烷组合物。
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CN105579477B (zh) * | 2014-03-26 | 2018-07-27 | 积水化学工业株式会社 | 光湿固化型树脂组合物、电子部件用粘接剂及显示元件用粘接剂 |
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