CN114685755A - 一种耐养蒸聚氨酯弹性体及其制备方法 - Google Patents
一种耐养蒸聚氨酯弹性体及其制备方法 Download PDFInfo
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- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical group CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 17
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- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 15
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Abstract
本发明公开了一种耐养蒸聚氨酯弹性体及其制备方法。所述聚氨酯弹性体通过包括以下质量份的组分制备得到:聚醚多元醇30‑70份、聚烯烃多元醇10‑40份、异氰酸酯20‑50份、扩链剂10‑30份、以及可选地:包括:催化剂0.1‑1份、抗氧剂0.2‑2份、增塑降粘剂5‑15份和消泡剂0.5‑2份。所述聚氨酯弹性体的制备方法包括以下步骤:(1)将聚醚多元醇、聚烯烃多元醇和增塑降粘剂进行混合,获得混合料S1;(2)将混合料S1与扩链剂、催化剂、抗氧剂和消泡剂混合得到混合料S2;(3)将混合料S2与异氰酸酯组分混合。通过本发明的聚氨酯弹性体制得的聚氨酯模板耐碱解好、耐老化能力强,能够耐受高温、碱性环境的砼养护成型过程。
Description
技术领域
本发明属于混凝土造型技术领域,具体涉及一种耐养蒸聚氨酯弹性体及其制备方法。
背景技术
随着混凝土技术的发展,混凝土的流动性和固化后强度均有所提高。在这种情况下,混凝土的浇筑件具有更加良好的表面纹理,可以实现除具有功能外的各种创意。为了实现混凝土的浇筑,本领域技术人员开发出多种造型模板,实现混凝土的模块化浇筑。
对于模板的材料,本领域通常采用硅胶材质或聚氨酯材料,但是硅胶材料的耐撕裂性能差,在脱模过程中容易撕裂损坏,由此导致基于硅胶材质的混凝土模具通常都是一次性使用。为了降低模具成本,开发出可反复使用的混凝土浇筑模板材料,本领域技术人员尝试了多种材料。
对于常规的聚氨酯材料,其耐撕裂性能良好,可以反复使用,但由于混凝土材料的碱性,导致聚氨酯模板受到混凝土的碱性腐蚀,发生碱解,导致材料强度下降。特别是,混凝土模块在蒸汽养护期间,在蒸汽高温环境下,模板材料的强度下降快,导致常规的聚氨酯材料制备的混凝土模板无法满足蒸汽养护混凝土模块制造的需要。
发明内容
为了满足混凝土蒸汽养护的需要,本发明提供了一种耐蒸养的混凝土模板材料。具体地,本发明提供了一种耐蒸养混凝土模块聚氨酯弹性体,其耐碱解,特别是在混凝土蒸养过程中能保持良好的拉伸强度。
本发明为达到上述目的,具体通过以下技术方案得以实现的:
原料包括以下质量份的组分:聚醚多元醇30-70份、聚烯烃多元醇10-40份、异氰酸酯20-50份、扩链剂10-30份。
在本发明中,可选地原料还包括:催化剂0.1-1份、抗氧剂0.2-2份、增塑降粘剂5-15份和消泡剂0.5-3份。
进一步地,所述聚醚多元醇为官能度为2或3的环氧丙烷聚醚,分子量1000-6000。优选地,本发明所述聚醚多元醇为环氧丙烷聚醚,Mn=500-2000,f=2。所述聚烯烃多元醇为官能度为2的支链多元醇。
其中所述支链多元醇的分子量为2000-4000,分子量分散系数(Mw/Mn)为1.1-1.3。优选地,所述支链多元醇其具有8-12个碳原子的支链。
在本发明优选的实施方式中,所述支链多元醇选自:Krasol LBH-P 3000,KrasolF 3000的一种或其组合。
进一步地,所述异氰酸酯为官能度为2-3,为二苯基甲烷二异氰酸酯、液化二苯基甲烷二异氰酸酯、聚合二苯基甲烷二异氰酸酯、甲苯二异氰酸酯和氢化二苯基甲烷二异氰酸酯中的一种或多种。
进一步地,所述扩链剂为对苯二酚-双(β羟乙基)醚、间苯二酚-双(β羟乙基)醚、间苯二酚-双羟丙基醚、间苯二酚双羟丙基乙基醚、三羟基甲基丙烷单烯丙基醚、2-乙基-1,3-己二醇、2,4-二乙基-1,5-戊二醇、2-丁基-2-乙基-1,3-丙二醇的一种或多种。
进一步地,所述催化剂为二月桂酸二丁基锡;和/或,所述抗氧剂为抗氧剂245、抗氧剂1010和抗氧剂1035中的一种或多种;和/或,所述增塑降粘剂为2,2,4-三甲基-1,3-戊二醇双异丁酸酯;和/或,所述消泡剂为BYK-088、BYK-141和BYK-A535中的一种或多种。
本发明进一步公开了一种聚醚多元醇的制备方法,包括以下步骤:
(1)将聚醚多元醇、聚烯烃多元醇和增塑降粘剂进行混合,获得混合料S1;
(2)将混合料S1与扩链剂、催化剂、抗氧剂和消泡剂混合得到混合料S2;
(3)将混合料S2与异氰酸酯组分混合,即得到聚氨酯弹性体。
进一步地,步骤(1)的混合温度为40-50℃,200-500rpm搅拌15-30min,真空度为-0.095MPa。
进一步地,步骤(2)的混合温度为60-80℃,200-500rpm搅拌15-30min,真空度为-0.095MPa。
进一步地,步骤(3)的混合温度为20-30℃,混合均匀后浇注于模具中,20-30℃固化7d得到耐养蒸聚氨酯弹性体。
本发明还公开了一种由上述任一所述的耐养蒸聚氨酯弹性体的制备方法制得的聚氨酯弹性体用作模板胶。
与现有技术相比,本发明的制备方法为一步法,操作简便;通过环氧丙烷聚醚和聚烯烃多元醇的复配使用,可以平衡物料工艺性能和最终弹性体的力学性能;通过强化体系物理交联点和增加化学交联点,制备特殊的聚氨酯弹性体可以耐受高温、碱性环境的砼养护成型过程。
实验效果表明,由本发明制备得到的耐养蒸聚氨酯弹性体模板的拉伸强度为≥5.5MPa,断裂伸长率为≥450%,聚氨酯模板抗撕拉能力强;70℃、10%NaOH溶液浸泡30d后拉伸强度保持率≥90%,聚氨酯模板耐碱解、耐老化能力强;压缩永久变形率依据国家标准GB/T 1683-2018,其压缩永久变形≤5%;硬度65~80ShoreA,满足造型混凝土用聚氨酯弹性体模板的硬度要求。
具体实施方式
本发明提供了一种耐养蒸聚氨酯弹性体及其制备方法,在本发明中,若无特殊说明,所有的原料均为本领域技术人员熟知的市售商品即可。
以质量份计,本发明提供的耐养蒸聚氨酯弹性体的制备原料包括环氧丙烷聚醚多元醇30-70份,优选为35-60份,更优选为45-55份;
以质量份计,本发明提供的耐养蒸聚氨酯弹性体的制备原料包括聚烯烃多元醇10-40份,优选为15-35份,更优选为20-30份;
以质量份计,本发明提供的耐养蒸聚氨酯弹性体的制备原料包括异氰酸酯20-50份,优选为25-45份,更优选为27-42份;在本发明中,所述异氰酸酯优选为二苯基甲烷二异氰酸酯、液化二苯基甲烷二异氰酸酯、聚合二苯基甲烷二异氰酸酯、甲苯二异氰酸酯和氢化二苯基甲烷二异氰酸酯中的一种或多种,进一步优选为二苯基甲烷二异氰酸酯、聚合二苯基甲烷二异氰酸酯、甲苯二异氰酸酯中的一种或多种;
在本发明优选的实施方式中,所述支链多元醇选自:Krasol LBH-P 3000,KrasolF 3000的一种或其组合。
其中Krasol LBH-P 3000,Krasol F 3000由Total Cray Valley提供,具体地,Krasol LBH-P 3000其Mn=3000,Mw/Mn=1.1~1.3,OH值0.6-0.7meq/g;Krasol F 3000其Mn=3000,Mw/Mn=1.1~1.3,OH值0.6-0.7meq/g。
以质量份计,本发明提供的耐养蒸聚氨酯弹性体的制备原料包括扩链剂10-30份,进一步优选为15-25份;本发明中,所述扩链剂为对苯二酚-双(β羟乙基)醚、间苯二酚-双(β羟乙基)醚、间苯二酚-双羟丙基醚、间苯二酚双羟丙基乙基醚、三羟基甲基丙烷单烯丙基醚、2-乙基-1,3-己二醇、2,4-二乙基-1,5-戊二醇、2-丁基-2-乙基-1,3-丙二醇的一种或多种,进一步优选为间苯二酚-双(β羟乙基)醚、间苯二酚双羟丙基乙基醚、间苯二酚双羟丙基乙基醚、2-乙基-1,3-己二醇、和2,4-二乙基-1,5-戊二醇中的一种和多种;
以质量份计,本发明提供的耐养蒸聚氨酯弹性体的制备原料包括催化剂0.1-1份,优选为0.2-0.8份,在本发明中,催化剂优选为二月桂酸二丁基锡;
抗氧剂0.2-2份,优选为0.5-1.5份,在本发明中,抗氧剂为抗氧剂245、抗氧剂1010和抗氧剂1035中的一种或多种;
增塑降粘剂5-15份,优选为8-12份,本发明中,增塑降粘剂为2,2,4-三甲基-1,3-戊二醇双异丁酸酯;
消泡剂0.5-3份,优选为0.7-2份,在本发明中,消泡剂为BYK-088、BYK-141和BYK-A535中的一种或多种。
本发明的耐养蒸聚氨酯弹性体的制备方法包括以下步骤:
(1)将聚醚多元醇、聚烯烃多元醇和增塑降粘剂进行混合,获得混合料S1;
(2)将混合料S1与扩链剂、催化剂、抗氧剂和消泡剂混合得到混合料S2;
(3)将混合料S2与异氰酸酯组分混合,即得到聚氨酯弹性体。
反应条件要求:
步骤(1)的混合温度为40-50℃,200-500rpm搅拌15-30min,真空度为-0.095MPa。
步骤(2)的混合温度为60-80℃,200-500rpm搅拌15-30min,真空度为-0.095MPa。
步骤(3)的混合温度为20-30℃,混合均匀后浇注于模具中,20-30℃固化7d得到耐养蒸聚氨酯弹性体。
实施例1
一种耐养蒸聚氨酯弹性体,按质量份数计,其制备原料的组分包括:
环氧丙烷聚醚(Mn=1000,f=2)50份、Krasol LBH-P 3000 20份、二苯基甲烷二异氰酸酯36.5份、间苯二酚-双(β羟乙基)醚15份、二月桂酸二丁基锡0.3份、1.5份抗氧剂1010、10份2,2,4-三甲基-1,3-戊二醇双异丁酸酯和2份消泡剂BYK-088。
将50kg环氧丙烷聚醚、20kg Krasol LBH-P 3000和10kg 2,2,4-三甲基-1,3-戊二醇双异丁酸酯在45℃、-0.095MPa、300rpm混合15min得到混合料S1,然后在混合料中加入15kg间苯二酚-双(β羟乙基)醚、0.3kg二月桂酸二丁基锡、1.5kg抗氧剂1010和2kg BYK-088,在60℃、-0.095MPa、300rpm混合15min得到混合料S2;将S2与二苯基甲烷二异氰酸酯按照重量比2.7:1混合均匀,25℃条件下浇注于模具中,固化7d得到耐养蒸聚氨酯弹性体。
实施例2
一种耐养蒸聚氨酯弹性体,按质量份数计,其制备原料的组分包括:
环氧丙烷聚醚(Mn=1000,f=2)50份、Krasol F 3000 20份、二苯基甲烷二异氰酸酯27份、间苯二酚-双(β羟乙基)醚10份、2-乙基-1,3-己二醇5份、二月桂酸二丁基锡0.3份、1.5份抗氧剂1010、10份2,2,4-三甲基-1,3-戊二醇双异丁酸酯和2份消泡剂BYK-141。
将50kg环氧丙烷聚醚、20kg Krasol F 3000和10kg2,2,4-三甲基-1,3-戊二醇双异丁酸酯在45℃、-0.095MPa、300rpm混合15min得到混合料S1,然后在混合料中加入10kg间苯二酚-双(β羟乙基)醚、5kg2-乙基-1,3-己二醇、0.3kg二月桂酸二丁基锡、1.5kg抗氧剂1010和2kg BYK-141,在60℃、-0.095MPa、300rpm混合15min得到混合料S2;将S2与二苯基甲烷二异氰酸酯按照重量比3.7:1混合均匀,25℃条件下浇注于模具中,固化7d得到耐养蒸聚氨酯弹性体。
实施例3
一种耐养蒸聚氨酯弹性体,按质量份数计,其制备原料的组分包括:
环氧丙烷聚醚1(Mn=1000,f=2)35份、环氧丙烷聚醚2(Mn=3000,f=3)15份、Krasol LBH-P 3000 25份、甲苯二异氰酸酯25份、间苯二酚双羟丙基乙基醚25份、二月桂酸二丁基锡0.3份、1.5份抗氧剂245、10份2,2,4-三甲基-1,3-戊二醇双异丁酸酯和2份消泡剂BYK-088。
将35kg环氧丙烷聚醚1、15kg环氧丙烷聚醚2、25kg Krasol LBH-P 3000和10kg2,2,4-三甲基-1,3-戊二醇双异丁酸酯在45℃、-0.095MPa、300rpm混合15min得到混合料S1,然后在混合料中加入25kg间苯二酚双羟丙基乙基醚、0.3kg二月桂酸二丁基锡、1.5kg抗氧剂245和2kg BYK-088,在60℃、-0.095MPa、300rpm混合15min得到混合料S2;将S2与甲苯二异氰酸酯按照重量比4:1混合均匀,25℃条件下浇注于模具中,固化7d得到耐养蒸聚氨酯弹性体。
实施例4
一种耐养蒸聚氨酯弹性体,按质量份数计,其制备原料的组分包括:
环氧丙烷聚醚(Mn=2000,f=2)50份、Krasol F 3000 20份、聚合二苯基甲烷二异氰酸酯30份、2-乙基-1,3-己二醇10份、二月桂酸二丁基锡0.5份、1.5份抗氧剂1010、10份2,2,4-三甲基-1,3-戊二醇双异丁酸酯和2份消泡剂BYK-088。
将50kg环氧丙烷聚醚、20kg Krasol F 3000和10kg 2,2,4-三甲基-1,3-戊二醇双异丁酸酯在45℃、-0.095MPa、300rpm混合15min得到混合料S1,然后在混合料S1中加入10kg2-乙基-1,3-己二醇、0.5kg二月桂酸二丁基锡、1.5kg抗氧剂1010和2kg BYK-088,在60℃、-0.095MPa、300rpm混合15min得到混合料S2;将S2与聚合二苯基甲烷二异氰酸酯按照重量比3:1混合均匀,25℃条件下浇注于模具中,固化7d得到耐养蒸聚氨酯弹性体。
实施例5
一种耐养蒸聚氨酯弹性体,按质量份数计,其制备原料的组分包括:
环氧丙烷聚醚(Mn=2000,f=2)45份、Krasol LBH-P 3000 25份、氢化二苯基甲烷二异氰酸酯39份、2-乙基-1,3-己二醇15份、二月桂酸二丁基锡0.8份、1.5份抗氧剂1010、10份2,2,4-三甲基-1,3-戊二醇双异丁酸酯和1.5份消泡剂BYK-141。
将45kg环氧丙烷聚醚、25kg Krasol LBH-P 3000和10kg 2,2,4-三甲基-1,3-戊二醇双异丁酸酯在45℃、-0.095MPa、300rpm混合15min得到混合料S1,然后在混合料S1中加入15kg2-乙基-1,3-己二醇、0.8kg二月桂酸二丁基锡、1.5kg抗氧剂1010和2kg BYK-088,在60℃、-0.095MPa、300rpm混合15min得到混合料S2;将S2与氢化二苯基甲烷二异氰酸酯按照重量比2.5:1混合均匀,25℃条件下浇注于模具中,固化7d得到耐养蒸聚氨酯弹性体。
实施例6
基于实施例1的实施方案,将聚烯烃多元醇选自端羟基氢化聚异戊二烯多元醇(f=2,37mgKOH/g),其余条件不变,得到耐养蒸聚氨酯弹性体。
对比例1
一种聚氨酯弹性体,按质量份数计,其制备原料的组分包括:
环氧丙烷聚醚(Mn=2000,f=2)20份、Krasol LBH-P 3000多元醇50份、聚合二苯基甲烷二异氰酸酯29份、2-乙基-1,3-己二醇10份、二月桂酸二丁基锡0.5份、1.5份抗氧剂1010、5份2,2,4-三甲基-1,3-戊二醇双异丁酸酯和2份消泡剂BYK-088。
将20kg环氧丙烷聚醚、50kgKrasol LBH-P 3000和5kg2,2,4-三甲基-1,3-戊二醇双异丁酸酯在45℃、-0.095MPa、300rpm混合15min得到混合料S1,然后在混合料S1中加入10kg2-乙基-1,3-己二醇、0.5kg二月桂酸二丁基锡、1.5kg抗氧剂1010和2kg BYK-088,在60℃、-0.095MPa、300rpm混合15min得到混合料S2;将S2与聚合二苯基甲烷二异氰酸酯按照重量比3:1混合均匀,25℃条件下浇注于模具中,固化7d得到耐养蒸聚氨酯弹性体。
对比例2
一种聚氨酯弹性体,按质量份数计,其制备原料的组分包括:
环氧丙烷聚醚(Mn=2000,f=2)45份、Krasol LBH-P 3000多元醇25份、氢化二苯基甲烷二异氰酸酯40份、1,4-丁二醇10份、二月桂酸二丁基锡0.8份、1.5份抗氧剂1010和1.5份消泡剂BYK-141。
将45kg环氧丙烷聚醚和25kg Krasol LBH-P 3000在45℃、-0.095MPa、300rpm混合15min得到混合料S1,然后在混合料S1中加入10kg1,4-丁二醇、0.8kg二月桂酸二丁基锡、1.5kg抗氧剂1010和2kg BYK-088,在60℃、-0.095MPa、300rpm混合15min得到混合料S2;将S2与氢化二苯基甲烷二异氰酸酯按照重量比2:1混合均匀,25℃条件下浇注于模具中,固化7d得到耐养蒸聚氨酯弹性体。
实施例1-6与对比例1-2所得聚氨酯弹性体测试结果表1:
表1实施例1-6与对比例1-2所得聚氨酯弹性体测试结果
由表1可见,本发明实施例1-6得到的耐蒸养聚氨酯弹性体模板的拉伸强度为≥5.5MPa,断裂伸长率为≥450%,聚氨酯模板抗撕拉能力强;70℃、10%NaOH溶液浸泡30d后拉伸强度保持率≥90%,聚氨酯模板耐碱解、耐老化能力强;压缩永久变形率依据国家标准GB/T 1683-2018,其压缩永久变形≤5%;硬度65~80ShoreA,满足造型混凝土用聚氨酯弹性体模板的硬度要求。
本发明中的具体实施例仅仅是对本发明的解释,其并不是对本发明的限制,本领域技术人员在阅读完本说明书后可以根据需要对本实施例做出没有创造性贡献的修改,但只要在本发明的权利要求范围内都受到专利法的保护。
Claims (10)
1.一种耐养蒸聚氨酯弹性体,其特征在于,其由包括以下质量份的组分制备得到:聚醚多元醇30-70份、聚烯烃多元醇10-40份、异氰酸酯20-50份、扩链剂10-30份。
2.如权利要求1所述的耐养蒸聚氨酯弹性体,其中原料还包括以下组分:催化剂0.1-1份、抗氧剂0.2-2份、增塑降粘剂5-15份和消泡剂0.5-2份。
3.如权利要求1所述的耐养蒸聚氨酯弹性体,其中所述聚醚多元醇为官能度为2或3的环氧丙烷聚醚,分子量1000-6000。
4.如权利要求1所述的耐养蒸聚氨酯弹性体,其中所述聚烯烃多元醇为官能度为2的支链多元醇,所述支链多元醇的分子量为2000-4000,分子量分散系数(Mw/Mn)为1.1-1.3;优选地,所述支链其具有8-12个碳原子。
5.如权利要求1所述的耐养蒸聚氨酯弹性体,其特征在于,所述异氰酸酯官能度为2-3,为二苯基甲烷二异氰酸酯、液化二苯基甲烷二异氰酸酯、聚合二苯基甲烷二异氰酸酯、甲苯二异氰酸酯和氢化二苯基甲烷二异氰酸酯中的一种或多种。
6.如权利要求1所述的耐养蒸聚氨酯弹性体,其特征在于,所述扩链剂为对苯二酚-双(β羟乙基)醚、间苯二酚-双(β羟乙基)醚、间苯二酚-双羟丙基醚、间苯二酚双羟丙基乙基醚、三羟基甲基丙烷单烯丙基醚、2-乙基-1,3-己二醇、2,4-二乙基-1,5-戊二醇、2-丁基-2-乙基-1,3-丙二醇的一种或多种。
7.如权利要求2所述的耐养蒸聚氨酯弹性体,其特征在于,所述催化剂为二月桂酸二丁基锡;和/或,所述抗氧剂为抗氧剂245、抗氧剂1010和抗氧剂1035中的一种或多种;和/或,所述增塑降粘剂为2,2,4-三甲基-1,3-戊二醇双异丁酸酯;和/或,所述消泡剂为BYK-088、BYK-141和BYK-A535中的一种或多种。
8.一种制备如权利要求1或2所述耐养蒸聚氨酯弹性体的方法,包括以下步骤:
(1)将聚醚多元醇、聚烯烃多元醇和增塑降粘剂进行混合,获得混合料S1;
(2)将混合料S1与扩链剂、催化剂、抗氧剂和消泡剂混合得到混合料S2;
(3)将混合料S2与异氰酸酯组分混合,即得到聚氨酯弹性体。
9.根据权利要求8所述的耐养蒸聚氨酯弹性体的制备方法,其特征在于,步骤(1)的混合温度为40-50℃,200-500rpm搅拌15-30min,体系真空度为-0.095MPa,步骤(2)的混合温度为60-80℃,200-500rpm搅拌15-30min,体系真空度为-0.095MPa。
10.根据权利要求8所述的耐养蒸聚氨酯弹性体的制备方法,其特征在于,步骤(3)的混合温度为20-30℃,混合均匀后浇注于模具中,20-30℃固化7d得到耐养蒸聚氨酯弹性体。
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