CN109306072A - 冻土用聚氨酯加固材料及其制备方法 - Google Patents
冻土用聚氨酯加固材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了冻土用聚氨酯加固材料及其制备方法,冻土用聚氨酯加固材料由质量比为1:1的A组分和B组分混合而成,其中A组分包括聚醚多元醇a 20‑60份;聚醚多元醇b 5‑35份;聚酯多元醇5‑10份;泡沫稳定剂0.5‑1.0份;水0.2‑0.8份;催化剂0.2‑5.0份;发泡剂1.0‑10.0份;阻燃剂4‑20份;增强剂5‑10份;防沉剂0.1‑0.5份;B组分为多苯基甲烷多异氰酸酯。制备方法为将各原料混合发泡即得。本发明提供的加固材料能够阻隔地上活动热量对地基下冻土的影响,保证地基之上建筑等的稳定,其韧性大,强度高,方数可控,能有效减少耗材。
Description
技术领域
本发明涉及聚氨酯材料制备领域,尤其涉及冻土用聚氨酯加固材料及其制备方法。
背景技术
冻土是指零摄氏度以下,一般都在-10℃至-17℃,冬季气温可低至-40℃,甚至-55℃,并含有冰的各种岩石和土壤。冻土有机质含量不高,腐殖质含量为10-20克每千克,腐殖质结构简单,70%以上是富里酸,呈酸性或碱性反应,阳离子代换量低,一般为10厘摩尔(+)每千克土左右,土壤粘粒含量少,而且淋失非常微弱,营养元素贫乏。冻土具有流变性,其长期强度远低于瞬时强度特征,此特征导致了在冻土区修筑工程构筑物必须面临两大危险:冷胀和融沉。中国的青藏铁路就有一段路需要通过冻土层,工程师需要通过多种方法使冻土层的温度稳定,以避免由于冻土层的转变而使铁路路基不平,防止意外发生;而前苏联和加拿大近一半的领土都是冻土层。目前,多用建筑垃圾做地基,解决冻土地面凹陷不平情况;也有用水泥做地基,但是这两种方法不但耗材大,而且保温性能差,很容易造成材料和冻土融为一体,起不到地基的作用;同时建筑垃圾和水泥脆性大,更为重要的是地基其强度也难以保证,用于冻土地基存在一定的风险。
发明内容
本发明的目的在于克服现有技术中所述的缺陷,从而提供冻土用聚氨酯加固材料及其制备方法,该加固材料能够阻隔地上活动热量对地基下冻土的影响,保证地基之上建筑等的稳定,同时保证与冻土接触的地基的稳定性,其韧性大,强度高,具有阻燃性在施工过程中方数可控,能有效减少耗材,解决动土地基不稳定的问题。
为了实现上述目的,本发明提供如下技术方案:
冻土用聚氨酯加固材料,由质量比为1:1的A组分和B组分混合而成,其中所述A组分包括以下重量份的原料:
所述B组分为多苯基甲烷多异氰酸酯。
优选地:所述聚醚多元醇a的官能度为4-5,分子量为550-750;所述聚醚多元醇b的官能度为4-6,分子量为250-700;所述聚酯多元醇c为芳烃聚酯多元醇,其官能度为2-3,分子量为300-800。
优选地:所述催化剂为五甲基二亚乙基三胺、三亚乙基二胺、三(二甲基丙基)六氢三嗪或N,N-二甲基卞胺中的一种或多种。
优选地:所述发泡剂为一氟二氯乙烷和/或五氟丙烷。
优选地:所述阻燃剂为磷酸三(2-氯丙基)酯和/或磷酸三乙酯。
优选地:所述增强剂为三聚氰胺、重钙或轻钙中的一种或多种。
优选地:所述防沉剂为为AEROSIL R202。
制备所述冻土用聚氨酯加固材料的方法,包括以下步骤:
(1)将上述重量份的聚醚多元醇a、聚醚多元醇b、聚酯多元醇c和水混合搅拌均匀,然后加入所述泡沫稳定剂、催化剂、阻燃剂和增强剂混匀,得A组分;
(2)将所述B组份加入所述A组分中进行发泡,即得所述冻土用聚氨酯加固材料。
优选地:步骤(1)中所述混匀为在混合釜中搅拌1-2h。
五甲基二亚乙基三胺,别称N,N,N′,N″,N″-五甲基二亚乙基三胺,简称PMDETA,是聚氨酯反应的高活性催化剂,它以催化发泡反应为主,也用于平衡整体发泡及凝胶反应。由于它的强烈发泡效果,能够改善泡沫流动性,因此改善产品生产工艺和提高制量。其催化剂活性大,发泡速度快,制品具有高韧性以及高承载性。五甲基二亚乙基三胺季铵盐是软泡延迟催化剂,用于延长发泡乳白时间,适合复杂形状泡沫制品及箱式发泡工艺,改善泡孔结构,提高模塑质量。其自身用量范围相当宽,并且用量变化对乳白时间影响不明显;但增加用量能缩短泡沫上升时间,能缩短固化时间。
三亚乙基二胺,又称1,4-二氮杂二环[2.2.2]辛烷、1,4-二叠氮双环辛烷、三乙烯二胺、TEDA、1,4-二偶氮双环[2.2.2]辛烷、1,4-乙烯哌嗪、二环[2.2.2]-1,4-二氮杂辛烷、三乙撑二胺、1,4-二叠氮双环[2.2.2]辛烷等,分子式是C14H28N2,分子量为224.3855,该物质主要用作聚氨酯的催化剂,因室温时是结晶固体,直接使用有困难,必须先将其溶解于相应的溶剂配成溶液,如乙二醇、丙二醇等。
三(二甲基丙基)六氢三嗪,又名1,3,5-三(二甲基胺丙基)-1,3,5-六氢化三嗪、N,N,N’,N’,N”,N”-六甲基-1,3,5-三嗪-1,3,5(2H,4H,6H)-三丙胺、1,3,5-三(二甲基胺丙基)-1,3,5-六氢化三嗪、1,3,5-三(3-二甲氨基丙基)六氢-S-三嗪、三嗪催化剂、1,3,5-三(二甲基胺丙基)-1,3,5-六氢化三嗪,分子式为C18H42N6,简称JD-10催化剂,JD-10催化剂是一种温和的三聚催化剂,可使用于各种聚氨酯及聚异氰脲酸酯等的硬质泡沫系统中。JD-10催化剂应与其它聚氨酯及聚异氰脲酸酯催化剂共同使用。JD-10催化剂的反应性比其它三聚催化剂(例如辛酸钾)较为温和,因此更容易平衡控制反应曲线。其具有优质的发泡催化能力和优质的全水发泡催化能力。
N,N-二甲基卞胺,分子式为C9H13N,N,N-二甲基苄胺在聚氨酯行业是聚酯型聚氨酯块状软泡、聚氨酯硬泡及胶黏剂涂料的催化剂,主要用于硬泡,可使聚氨酯泡沫具有良好的前期流动性和均匀的泡孔,泡沫体与基材间有较好的粘结力。
一氟二氯乙烷简称HCFC-141b,是一种高纯度的液体,广泛应用于清洗和溶剂领域。由于其对臭氧层的破坏是CFC-113的1/10,因而被指定为全卤代氟氯碳化合物的一种理想的替代物。化学式为CCl2F-CH3,HCFC-141b没有闪点,属非可燃液体。具有优良的热稳定性、化学稳定性,但不能同强碱性化合物、碱性金属接触。
五氟丙烷,又名1,1,1,3,3-五氟丙烷,简称HFC-245fa,化学式为CF3-CH2-CHF2,与水不溶,可混溶于乙醇、乙醚、氯仿、油类、烃类等多数有机溶剂,用于冰箱、板材聚氨酯绝热材料发泡等。
磷酸三(2-氯丙基)酯,又称磷酸三(1-氯-2-丙基)酯、阻燃增塑剂TCPP、异丙基苯酚磷酸酯、异丙基磷酸酯、磷酸三异丙基苯酯、IPPP、异丙基三芳基磷酸酯等,英文名为tris(1-chloro-2-propyl)phosphate,分子式是C9H18Cl3O4P,分子量为327.5696。用于条状、块状泡沫生产中的火焰阻燃剂。是一种成本低廉的火焰阻燃剂,且具有良好的稳定性。磷酸三异丙基苯酯35(阻燃剂ippp35)Reofos35广泛用于橡胶制品和PVC塑料阻燃输送带、皮革、农用地膜、地板材料、电缆、氯丁橡胶、丁腈橡胶等合成橡胶的阻燃增塑剂,环氧树酯的阻燃剂。
磷酸三乙酯,英文名Triethyl phosphate,又称阻燃剂TEP、三乙基磷酸酯、三乙磷酸酯、三乙氧基磷、TEP、阻燃剂-TEP等,分子式是C6H15O4P,分子量182.1547,磷酸三乙酯(阻燃剂TEP)为高沸点溶剂,橡胶和塑料的增塑剂,也用作制取农药杀虫剂的原料,用作乙基化试剂和乙烯酮生产。在日本,该品的70%用于催化剂,约20%用作溶剂。主要用途如下:(1)催化剂:二甲苯异构体催化剂、烯烃的聚合催化剂、制造四乙基铅的催化剂、制造碳化二亚胺的催化剂、三烷基硼和烯烃的置换反应催化剂、用乙酸高温脱水制造乙烯酮的催化剂、苯乙烯同共轭二烯类化合物聚合用的催化剂;如果在对苯二甲酸、乙二醇聚合时使用则有防止纤维变色的作用。(2)溶剂:硝酸纤维素及乙酸纤维素的溶剂、用于保持有机过氧化物催化剂寿命的溶剂、氟化乙烯分散用的溶剂、作聚酯树脂、环氧树脂的固化催化剂的过氧化物剂及稀释剂。(3)稳定剂:氯系杀虫剂和稳定剂、酚醛树脂的稳定剂、糖醇树脂的固体剂。(4)合成树脂方面:二甲酚甲醛树脂的固化剂、壳型塑模所使用的酚醛树脂的软化剂、氯乙烯的柔软剂、乙酸乙烯聚合物的增塑剂、聚酯树脂的阻燃剂。
三聚氰胺,化学式为C3N3(NH2)3),俗称密胺、蛋白精、三聚氰酰胺等,IUPAC命名为1,3,5-三嗪-2,4,6-三胺,三聚氰胺是氨基氰的三聚体,由它制成的树脂加热分解时会释放出大量氮气,因此可用作阻燃剂。三聚氰胺不可燃,在常温下性质稳定。水溶液呈弱碱性(pH值=8),与盐酸、硫酸、硝酸、乙酸、草酸等都能形成三聚氰胺盐。在中性或微碱性情况下,与甲醛缩合而成各种羟甲基三聚氰胺,但在微酸性中(pH值5.5~6.5)与羟甲基的衍生物进行缩聚反应而生成树脂产物。遇强酸或强碱水溶液水解,胺基逐步被羟基取代,先生成三聚氰酸二酰胺,进一步水解生成三聚氰酸一酰胺,最后生成三聚氰酸。
重钙就是方解石粉,是重质碳酸钙的简称,重质碳酸钙(Heavy CalciumCarbonate)又称研磨碳酸钙(Ground Calcium Carbonate,简称GCC,美国称Kotamite),是由天然碳酸盐矿物如方解石、大理石、石灰石磨碎而成。是常用的粉状无机填料,具有化学纯度高、惰性大、不易化学反应、热稳定性好、在400℃以下不会分解、白度高、吸油率低、折光率低、质软、干燥、不含结晶水、硬度低磨耗值小、无毒、无味、无臭、分散性好等优点。按粒度(D97,mm)可分为重质碳酸钙粗粉和细粉(D97>10mm)和超细重质碳酸钙(D97≤10mm);按是否表面改性分为重质碳酸钙(简称重钙)和活性重质碳酸钙(简称活性重钙);活性重质碳酸钙还可细分为活性重钙粉和超细活性重钙粉。重钙价格便宜,在乳胶漆中使用和轻质碳酸钙相比,容易沉降。重钙可以增加产品体积、降低成本,改善加工性能(如调节粘度、流变性能、硫化性能),提高尺寸稳定性,补强或半补强,提高印刷性能,提高物理性能(如耐热性、消光性、耐磨性、阻燃性、白度、光泽度)等。
轻钙别名轻质碳酸钙,又称为沉淀碳酸钙、沉降碳酸钙轻质超细碳酸钙,俗称轻钙。轻钙是将石灰石等原料段烧生成石灰和二氧化碳,再加水消化石灰生成石灰乳(主要成分氢氧化钙),通入二氧化碳碳化石灰乳生成碳酸钙沉淀,经脱水、干燥和粉碎制得。或者由碳酸纳和氯化钙进行复分解反应生成碳酸钙沉淀,经脱水、干燥和粉碎制得。分子式为CaCO3,轻钙粒度比重质碳酸钙小,吸油量比重质碳酸钙大,价格比重质碳酸钙高。他们都是乳胶漆中常用的填料,最好搭配使用。轻钙在沉降方面好些,但吸油量大于重钙,价格一般也较重钙贵些,尽管稳定性方面不如重钙,但还是具备稳定性的,即使是外墙漆,其应用量也是很大的。
AEROSIL R202是通过亲水性气相二氧化硅,经二甲基聚硅氧烷改良后的疏水性气相法二氧化硅。在复杂极性液体中使用,如环氧树脂、聚氨酯、乙烯基树脂、具有良好的增稠性和触变效果。用于光缆的电缆胶中作增稠和触变剂,高密度填料的防沉剂。AEROSIL R202可以使环氧树脂获得稳定的增稠和触变性。当加入胺固化剂后,在固化过程中流体的粘度值和触变性能基本保持恒定。AEROSIL R202是一种用聚二甲基硅氧烷不完全处理的疏水气相二氧化硅,其微粒的表面固定着较长链的聚二甲基硅氧烷,具有非常强的疏水性,当这种疏水产品分散于极性体系中时,这种疏水基团可以保护白炭黑表面剩余的硅羟基,以防止其被过分润湿,剩余的硅羟基基团和长链疏水基团使这种疏水气相二氧化硅产生较强的增稠和触变效果,从而克服了亲水性气相二氧化硅在极性体系中增稠触变性变差,触变网络稳定性易降低的缺点。
多苯基甲烷多异氰酸酯是以多异氰酸酯的单体或均聚物为主体材料的胶粘剂,正名为多异氰酸酯胶粘剂。
多苯基多亚甲基多异氰酸酯简称PAPI,或称粗MDI,PAPI实际上是由50%MDI与50%官能度大于2以上的多异氰酸酯组成的混合物。升温时能发生自聚作用。溶于氯苯、邻二氯苯、甲苯等。PAPI的活性低,蒸气压低,只是TDI的百分之一,故毒性很低,空气中最高容许浓度0.2mg/m³。用于制造聚氨脂胶粘剂。也可直接加入橡胶胶粘剂中,改善橡胶与尼龙或聚酯线的粘接性能。聚合MDI可广泛应用于聚氨酯硬泡保温材料的制造;还可用于异氰脲酸酯泡沫、涂料、粘合剂、防渗堵漏、结构泡沫、微孔自结皮泡沫、汽车保险杠、内饰件、高回弹泡沫、合成木材等领域。由于其特有的组成结构,具有较好的泡沫流动性能,还适合应用于对发泡原液流动性能要求严格的制品的制造。
聚酯多元醇PS-3152具有优异的抗水解性,非常好的热稳定性和伯羟基优势,可促进与各种金属和塑料基材的粘合,并具有易于混合的低粘度特性及高芳烃含量。用于生产硬质聚异氰脲酸酯板材和低密度、浇铸、喷塑、高密度及包装聚氨酯泡沫;可用于生产聚氨酯涂料、胶黏剂、密封剂及弹性体。
与现有技术相比,本发明具有以下有益效果:
本发明采用两种聚醚多元醇和一种聚酯多元醇作为主料,并配以泡沫稳定剂、水、催化剂、发泡剂阻燃剂、增强剂和防沉剂,其中各原料均按上述重量份进行配比,所得到的产品不仅可以保证材料的强度和韧性,而且阻燃性佳、低温尺寸稳定性好、强度高、韧性好、原料液运输方便、储存稳定性好,本发明所用到的原料绿色、无污染,发泡过程不会产生任何有毒气体,且制备方法简单,可以高效地解决冻土地基不稳定问题。
其中本发明对多元醇作进一步优选,聚醚多元醇a为官能度为4-5,分子量为550-750;聚醚多元醇b的官能度为4-6,分子量为250-700;聚酯多元醇c为芳烃聚酯多元醇,其官能度为2-3,分子量为300-800,通过对多元醇、增强剂、阻燃剂及异氰酸酯的选择,在反应体系中通过主体聚醚的选择搭配,保证了材料的强度和韧性,本发明的用于冻土的地基,自身具有一定的保温性能,能够阻隔地上活动热量对地基下冻土的影响,保证地基之上建筑等的稳定,所制得的材料起发时间短,约为38-60s,凝胶时间约为128-145s,可有效提升施工效率;且强度高,抗压强度为0.512-0.788kPa/10%;抗拉强度为0.68-0.88kPa/10%,延伸率为6-11%,使得本发明的材料具备相当的韧性和支撑作用,成为冻土地基的优选;其低温尺寸稳定性好,闭孔率为92.51-93.34%%,吸水率为0.11-0.13kg/m3,从而保证了与冻土接触的地基的稳定性;同时由于其密度可控,因此在施工过程中出方数可控,可有效地减少耗材;除此之外还具备一定的阻燃性能,阻燃性能为23.5-24.3O%,可以满足基本阻燃要求。
具体实施方式
下面将对本发明的技术方案进行清楚、完整地描述,显然,所描述的实施例是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。此外,下面所描述的本发明不同实施方式中所涉及的技术特征只要彼此之间未构成冲突就可以相互结合。
需要说明的是,下述实施例中1份代指1Kg,所用到的聚醚多元醇A、聚醚多元醇B以及聚酯多元醇C均由山东一诺威新材料有限公司提供,各型号如实施例中所示;其中聚酯多元醇C也可由南京金陵斯泰潘化学有限公司提供,型号为PS-3152;泡沫稳定剂由迈图高新材料集团提供,型号为L6950;或由沧州市骏驰伟业化工有限公司提供,型号为JC7750;防沉剂由赢创德固赛特种化学(上海)有限公司提供,型号为AEROSIL R202;多亚甲基多苯基多异氰酸酯由拜耳(中国)有限公司提供,型号为44V20;或由烟台万华聚氨酯股份有限公司提供,型号为PM200。
实施例1
本发明提供了一种冻土用聚氨酯加固材料,包括以下重量份的原料:
制备所述冻土用聚氨酯加固材料的方法,包括以下步骤:
(1)将上述重量份的聚醚多元醇a、聚醚多元醇b、聚酯多元醇c和水混合搅拌均匀,然后加入所述泡沫稳定剂、催化剂、阻燃剂和增强剂并在混合釜中搅拌1h,得A组分;
(2)将所述B组份加入所述A组分中进行发泡,即得所述冻土用聚氨酯加固材料。
实施例2
本发明提供了一种冻土用聚氨酯加固材料,包括以下重量份的原料:
制备所述冻土用聚氨酯加固材料的方法,包括以下步骤:
(1)将上述重量份的聚醚多元醇a、聚醚多元醇b、聚酯多元醇c和水混合搅拌均匀,然后加入所述泡沫稳定剂、催化剂、阻燃剂和增强剂并在混合釜中搅拌1.5h,得A组分;
(2)将所述B组份加入所述A组分中进行发泡,即得所述冻土用聚氨酯加固材料。
实施例3
本发明提供了一种冻土用聚氨酯加固材料,包括以下重量份的原料:
制备所述冻土用聚氨酯加固材料的方法,包括以下步骤:
(1)将上述重量份的聚醚多元醇a、聚醚多元醇b、聚酯多元醇c和水混合搅拌均匀,然后加入所述泡沫稳定剂、催化剂、阻燃剂和增强剂并在混合釜中搅拌1.8h,得A组分;
(2)将所述B组份加入所述A组分中进行发泡,即得所述冻土用聚氨酯加固材料。
实施例4
本发明提供了一种冻土用聚氨酯加固材料,包括以下重量份的原料:
制备所述冻土用聚氨酯加固材料的方法,包括以下步骤:
(1)将上述重量份的聚醚多元醇a、聚醚多元醇b、聚酯多元醇c和水混合搅拌均匀,然后加入所述泡沫稳定剂、催化剂、阻燃剂和增强剂并在混合釜中搅拌2h,得A组分;
(2)将所述B组份加入所述A组分中进行发泡,即得所述冻土用聚氨酯加固材料。
实施例5
本发明提供了一种冻土用聚氨酯加固材料,包括以下重量份的原料:
制备所述冻土用聚氨酯加固材料的方法,包括以下步骤:
(1)将上述重量份的聚醚多元醇a、聚醚多元醇b、聚酯多元醇c和水混合搅拌均匀,然后加入所述泡沫稳定剂、催化剂、阻燃剂和增强剂并在混合釜中搅拌1.5h,得A组分;
(2)将所述B组份加入所述A组分中进行发泡,即得所述冻土用聚氨酯加固材料。
下面对本发明实施例1-3所得的产品进行检测,结果如下:
本发明所述的冻土用聚氨酯加固材料,所制得的材料作用速度快,可有效提升施工效率;其抗压强度、抗拉强度、延伸率、闭孔率、吸水率、阻燃性能均能达到要求,本发明的材料具备相当支撑作用和韧性,成为冻土地基的优选;低温尺寸稳定性好,从而保证了与冻土接触的地基的稳定性;同时在施工过程中出方数可控,可有效地减少耗材;除此之外还具备一定的阻燃性能,保证了材料的安全使用。综合各项性能指标,实施例2为优选结果,其中,较为显著的是:聚醚R403和重钙的使用,对材料强度的提高起到重要作用;聚醚5118和聚酯PE-B175的使用对材料的抗拉效果具有重要作用;聚酯PE-B175、重钙和阻燃剂磷酸三(2-氯丙基)酯的使用,对材料阻燃性能的提高较大作用。
以上所述仅为本发明的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,可轻易想到的变化或替换,都应涵盖在本发明的保护范围之内。因此,本发明的保护范围应以所述权利要求的保护范围为准。
Claims (9)
1.冻土用聚氨酯加固材料,其特征在于,由质量比为1:1的A组分和B组分混合而成,其中所述A组分包括以下重量份的原料:
所述B组分为多苯基甲烷多异氰酸酯。
2.根据权利要求1所述的冻土用聚氨酯加固材料,其特征在于,所述聚醚多元醇a的官能度为4-5,分子量为550-750;所述聚醚多元醇b的官能度为4-6,分子量为250-700;所述聚酯多元醇c为芳烃聚酯多元醇,其官能度为2-3,分子量为300-800。
3.根据权利要求1所述的冻土用聚氨酯加固材料,其特征在于,所述催化剂为五甲基二亚乙基三胺、三亚乙基二胺、三(二甲基丙基)六氢三嗪或N,N-二甲基卞胺中的一种或多种。
4.根据权利要求1所述的冻土用聚氨酯加固材料,其特征在于,所述发泡剂为一氟二氯乙烷和/或五氟丙烷。
5.根据权利要求1所述的冻土用聚氨酯加固材料,其特征在于,所述阻燃剂为磷酸三(2-氯丙基)酯和/或磷酸三乙酯。
6.根据权利要求1所述的冻土用聚氨酯加固材料,其特征在于,所述增强剂为三聚氰胺、重钙或轻钙中的一种或多种。
7.根据权利要求1所述的冻土用聚氨酯加固材料,其特征在于,所述防沉剂为为AEROSIL R202。
8.制备如权利要求1-7中任一项所述冻土用聚氨酯加固材料的方法,其特征在于,包括以下步骤:
(1)将上述重量份的聚醚多元醇a、聚醚多元醇b、聚酯多元醇c和水混合搅拌均匀,然后加入所述泡沫稳定剂、催化剂、阻燃剂和增强剂混匀,得A组分;
(2)将所述B组份加入所述A组分中进行发泡,即得所述冻土用聚氨酯加固材料。
9.根据权利要求8所述的方法,其特征在于,步骤(1)中所述混匀为在混合釜中搅拌1-2h。
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