CN115093541A - 基于聚氨酯弹性体的体育场地铺装材料及其制备方法 - Google Patents
基于聚氨酯弹性体的体育场地铺装材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了基于聚氨酯弹性体的体育场地铺装材料及其制备方法,属于聚氨酯材料技术领域,包括如下重量份原料:聚四氢呋喃醚二醇75‑80份、2,4‑甲苯二异氰酸酯20‑25份、二甲硫基甲苯二胺9‑12份、聚磷酸铵2‑3份、阻燃助剂0.8‑1.1份、有机蒙脱土7‑9份。本发明通过在聚氨酯原料中加入阻燃助剂,能对聚磷酸铵、有机蒙脱土起到复合协效阻燃效果,赋予聚氨酯优良的阻燃性能;能够促进聚氨酯交联网络结构的形成,提高聚氨酯的力学性能和耐磨性能;通过加入有机蒙脱土,与聚氨酯具体具有较高的相容性,提高力学性能和耐热性;本发明获得的铺装材料用于体育场地铺设时,能够大大提高体育场地的质量和使用安全性能。
Description
技术领域
本发明属于聚氨酯材料技术领域,具体地,涉及一种基于聚氨酯弹性体的体育场地铺装材料及其制备方法。
背景技术
聚氨酯基于二异氧酸酯、多异氧酸酯与二羟基、多羟基化合物加聚形成,耐磨性与弹性好,强度与伸长率较高,硬度范围宽广,且耐油性、耐酸性、耐碱性突出。因此,在体育场地的铺设中具有广泛的应用。
现代体育场的田径跑道和球类比赛场地铺装材料的聚氨酯弹性体,已知的是先用甲苯二异氰酸酯TDI和聚醚二醇及有机稀释剂制成聚氨酯预聚体(通称A组份);再将A组份与扩链—交链剂聚醚多元醇、二元醇的丁二醇、二元胺MOCA(3,3’-二氯-4,4’二氨基二苯基甲烷)和填料(通称B组份)混合,再用催化剂作用聚合制成的聚氨酯弹性体。
该配方体系存在的几个主要问题是:1)因产品的主要机械力学性能较低,不能适应体育场地因地冻、水浸等发生基础断裂、隆起、塌陷等形变所产生的应力,造成聚氨酯铺设材料的断裂;2)产品的阻燃性能较低,没有达到阻燃一级标准,难以应对火灾或极高温情况。因此,为了解决以上问题,提高聚氨酯铺设材料的机械力学性能、阻燃性能等,有必要考虑对聚氨酯弹性体的合成从新进行分子设计及配方调整以及应用新技术来获得性能更加优异的体育场地铺设材料。
发明内容
本发明的目的在于克服现有技术的缺陷,提供了基于聚氨酯弹性体的体育场地铺装材料及其制备方法。
本发明通过在聚氨酯原料中加入阻燃助剂,其一,能对聚磷酸铵、有机蒙脱土起到复合协效阻燃效果,赋予聚氨酯优良的阻燃性能;其二,阻燃助剂独特的结构,能够促进聚氨酯交联网络结构的形成,提高聚氨酯的力学性能和耐磨性能;此外,通过加入有机蒙脱土,与聚氨酯具体具有较高的相容性,提高复合材料的力学性能和耐热性;本发明获得的铺装材料用于体育场地铺设时,能够大大提高体育场地的质量和使用安全性能,使用寿命更长。
本发明的目的可以通过以下技术方案实现:
基于聚氨酯弹性体的体育场地铺装材料,包括如下重量份原料:聚四氢呋喃醚二醇75-80份、2,4-甲苯二异氰酸酯20-25份、二甲硫基甲苯二胺9-12份、聚磷酸铵2-3份、阻燃助剂0.8-1.1份、有机蒙脱土7-9份;
上述体育场地铺装材料的制备方法,包括如下步骤:
第一步、取聚四氢呋喃醚二醇于四口烧瓶中,加热至105℃抽真空除水90min,降温至85℃,加入阻燃助剂,保持85℃反应1h,降温至50℃,缓慢滴加2,4-甲苯二异氰酸酯升温至80℃反应2h,之后抽真空除气泡,得到聚氨酯预聚体,密封备用;
第二步、将二甲硫基甲苯二胺(扩链剂)、聚磷酸铵和有机蒙脱土混合后,研磨分散均匀后,再在80-90℃,真空脱水2h,冷却至50℃,得到扩链物,密封备用;
第三步、使用时,往聚氨酯预聚体中加入扩链物,搅拌反应3min,快速摊铺在需要铺装的体育场地中,在20-30℃条件下,30-60min内凝胶,24h内固化,14d完全熟化后可投入使用。
进一步地,有机蒙脱土为采用十八烷基三甲基溴化铵与蒙脱土层内的阳离子进行离子交换,得到的有机蒙脱土;聚氨酯与有机蒙脱土能够达到纳米级复合,两者之间具有很强的作用力,且插层进入蒙脱土片层之间的聚氨酯分子链受到蒙脱土片层极大的阻隔作用和限制作用,从而提高复合材料的力学性能、耐热性等。
进一步地,阻燃助剂通过如下步骤制备:
S1、将三聚氯氰溶于THF(四氢呋喃)后加入至带有机械搅拌装置的四口烧瓶中,控制底物的温度为25℃,200r/min匀速搅拌下将N-甲基-2-羟基乙胺的THF溶解液逐滴滴入四口烧瓶中,滴完后将反应液升温至50℃,并在此恒温条件下反应48h,反应过程中,用浓度为0.1mol/L的NaOH溶液维持pH在10以上,反应结束后,旋蒸除去大部分THF,再利用甲苯多次萃取,有机相用饱和NaCl水溶液洗涤多次后用无水Na2SO4干燥48h,抽滤、减压浓缩,得到中间体;N-甲基-2-羟基乙胺的THF溶解液中N-甲基-2-羟基乙胺的浓度为4.95g/mL;三聚氯氰、THF、N-甲基-2-羟基乙胺的THF溶解液的用量之比为18.44g:150mL:50mL;
三聚氯氰分子上的-Cl与N-甲基-2-羟基乙胺分子上的-NH-发生化学反应,获得中间体,反应过程如下所示;
S2、将二甲苯烷二异氰酸酯和DMF(N,N-二甲基甲酰胺)加入三口烧瓶中,磁力搅拌并加热至55℃,将中间体与DMF形成的溶解液缓慢滴加进三口烧瓶中,之后再滴入二月桂酸二丁基锡,保持55℃恒温搅拌反应4h,反应结束后,向其中加入甲苯,再加入去离子水,静置分层后,取有机相,并用饱和NaCl水溶液洗涤多次后用无水Na2SO4干燥48h,抽滤、减压浓缩,获得阻燃助剂;溶解液中中间体与DMF的用量之比为1g:5mL;二甲苯烷二异氰酸酯、DMF、溶解液的用量之比为8.25g:25mL:15mL:0.2mL;
中间体分子上的-OH与二甲苯烷二异氰酸酯分子上的-NCO反应,获得阻燃助剂,反应过程如下所示:
获得的阻燃助剂分子为三聚氰胺类衍生物,属于氮系阻燃剂,氮系阻燃剂通过产生NO2、CO2、H2O、N2、NH3等不燃气体,稀释可燃气体的浓度,来阻止聚合物与空气中的氧气接触,同时N2可以吸附、捕捉高能自由基,抑制燃烧链反应,起到防火阻燃作用,因此,其能与原料中的聚磷酸铵起到协效阻燃作用,形成磷-氮复合阻燃体系;更进一步地,磷-氮复合阻燃体系更多的是在生成不燃气体以及形成膨胀炭层方面起阻燃效果,而片层状的有机纳米蒙脱土对层间大分子形成物理阻隔作用,并且蒙脱土在高温情况下能够与聚磷酸铵发生成炭化学反应,生成Si-O-P键,增加了聚磷酸铵的高温分解稳定性;以上,阻燃助剂、聚磷酸铵以及纳米蒙脱土三者协效阻燃,赋予聚氨酯弹性体良好的阻燃防火效果;
此外,阻燃助剂为一种多异氰酸酯,其单个分子上含有三个-NCO基团,加入至聚氨酯原料中,其能够与聚氨酯基体反应,促进聚氨酯交联网络结构的形成,增大聚氨酯弹性体的力学性能,从而提高聚氨酯的耐磨特性。
本发明的有益效果:
本发明通过在聚氨酯原料中加入阻燃助剂,其一,能对聚磷酸铵、有机蒙脱土起到复合协效阻燃效果,赋予聚氨酯优良的阻燃性能;其二,阻燃助剂独特的结构,能够促进聚氨酯交联网络结构的形成,提高聚氨酯的力学性能和耐磨性能;此外,通过加入有机蒙脱土,与聚氨酯具体具有较高的相容性,提高复合材料的力学性能和耐热性;本发明获得的铺装材料用于体育场地铺设时,能够大大提高体育场地的质量和使用安全性能,使用寿命更长。
具体实施方式
下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅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作出创造性劳动前提下所获得的所有其它实施例,都属于本发明保护的范围。
实施例1
制备阻燃助剂:
S1、将18.44g三聚氯氰溶于150mL的THF(四氢呋喃)后加入至带有机械搅拌装置的四口烧瓶中,控制底物的温度为25℃,200r/min匀速搅拌下将50mL的N-甲基-2-羟基乙胺的THF溶解液(浓度为4.95g/mL)逐滴滴入四口烧瓶中,滴完后将反应液升温至50℃,并在此恒温条件下反应48h,反应过程中,用浓度为0.1mol/L的NaOH溶液维持pH在10以上,反应结束后,旋蒸除去大部分THF,再利用甲苯多次萃取,有机相用饱和NaCl水溶液洗涤多次后用无水Na2SO4干燥48h,抽滤、减压浓缩,得到中间体;
S2、将82.5g二甲苯烷二异氰酸酯和250mL的DMF(N,N-二甲基甲酰胺)加入三口烧瓶中,磁力搅拌并加热至55℃,将30g中间体与150mL的DMF形成的溶解液缓慢滴加进三口烧瓶中,之后再滴入2mL二月桂酸二丁基锡,保持55℃恒温搅拌反应4h,反应结束后,向其中加入300mL甲苯,再加入500mL去离子水,静置分层后,取有机相,并用饱和NaCl水溶液洗涤4次后用无水Na2SO4干燥48h,抽滤、减压浓缩,获得阻燃助剂。
实施例2
制备阻燃助剂:
S1、将9.22g三聚氯氰溶于75mL的THF(四氢呋喃)后加入至带有机械搅拌装置的四口烧瓶中,控制底物的温度为25℃,200r/min匀速搅拌下将25mL的N-甲基-2-羟基乙胺的THF溶解液(浓度为4.95g/mL)逐滴滴入四口烧瓶中,滴完后将反应液升温至50℃,并在此恒温条件下反应48h,反应过程中,用浓度为0.1mol/L的NaOH溶液维持pH在10以上,反应结束后,旋蒸除去大部分THF,再利用甲苯多次萃取,有机相用饱和NaCl水溶液洗涤多次后用无水Na2SO4干燥48h,抽滤、减压浓缩,得到中间体;
S2、将41.25g二甲苯烷二异氰酸酯和125mL的DMF(N,N-二甲基甲酰胺)加入三口烧瓶中,磁力搅拌并加热至55℃,将15g中间体与75mL的DMF形成的溶解液缓慢滴加进三口烧瓶中,之后再滴入1mL二月桂酸二丁基锡,保持55℃恒温搅拌反应4h,反应结束后,向其中加入150mL甲苯,再加入250mL去离子水,静置分层后,取有机相,并用饱和NaCl水溶液洗涤3次后用无水Na2SO4干燥48h,抽滤、减压浓缩,获得阻燃助剂。
实施例3
将10g纳米蒙脱土分散于100mL去离子水中形成质量分散液,在80℃下逐滴加入100mL十八烷基三甲基溴化铵的水溶液(浓度1mol/L),搅拌反应1h,抽滤,水洗5次,80℃真空烘箱中干燥至恒重,粉碎,过200目筛,获得有机蒙脱土。
实施例4
基于聚氨酯弹性体的体育场地铺装材料,包括如下重量的原料:聚四氢呋喃醚二醇75g、2,4-甲苯二异氰酸酯20g、二甲硫基甲苯二胺9g、聚磷酸铵2g、实施例1制得的阻燃助剂0.8g、实施例3制得的有机蒙脱土7g;
上述体育场地铺装材料的制备方法,包括如下步骤:
第一步、取聚四氢呋喃醚二醇于四口烧瓶中,加热至105℃抽真空除水90min,降温至85℃,加入阻燃助剂,保持85℃反应1h,降温至50℃,缓慢滴加2,4-甲苯二异氰酸酯升温至80℃反应2h,之后抽真空除气泡,得到聚氨酯预聚体,密封备用;
第二步、将二甲硫基甲苯二胺(扩链剂)、聚磷酸铵和有机蒙脱土混合后,研磨分散均匀后,再在80℃,真空脱水2h,冷却至50℃,得到扩链物,密封备用。
实施例5
基于聚氨酯弹性体的体育场地铺装材料,包括如下重量的原料:聚四氢呋喃醚二醇77.5g、2,4-甲苯二异氰酸酯22.5g、二甲硫基甲苯二胺10.5g、聚磷酸铵2.5g、实施例1制得的阻燃助剂0.9g、实施例3制得的有机蒙脱土8g;
上述体育场地铺装材料的制备方法,包括如下步骤:
第一步、取聚四氢呋喃醚二醇于四口烧瓶中,加热至105℃抽真空除水90min,降温至85℃,加入阻燃助剂,保持85℃反应1h,降温至50℃,缓慢滴加2,4-甲苯二异氰酸酯升温至80℃反应2h,之后抽真空除气泡,得到聚氨酯预聚体,密封备用;
第二步、将二甲硫基甲苯二胺(扩链剂)、聚磷酸铵和有机蒙脱土混合后,研磨分散均匀后,再在85℃,真空脱水2h,冷却至50℃,得到扩链物,密封备用。
实施例6
基于聚氨酯弹性体的体育场地铺装材料,包括如下重量的原料:聚四氢呋喃醚二醇80g、2,4-甲苯二异氰酸酯25g、二甲硫基甲苯二胺12g、聚磷酸铵3g、实施例1制得的阻燃助剂1.1g、实施例3制得的有机蒙脱土9g;
上述体育场地铺装材料的制备方法,包括如下步骤:
第一步、取聚四氢呋喃醚二醇于四口烧瓶中,加热至105℃抽真空除水90min,降温至85℃,加入阻燃助剂,保持85℃反应1h,降温至50℃,缓慢滴加2,4-甲苯二异氰酸酯升温至80℃反应2h,之后抽真空除气泡,得到聚氨酯预聚体,密封备用;
第二步、将二甲硫基甲苯二胺(扩链剂)、聚磷酸铵和有机蒙脱土混合后,研磨分散均匀后,再在90℃,真空脱水2h,冷却至50℃,得到扩链物,密封备用。
对比例1
将实施例4中的阻燃助剂原料去掉,其余原料及制备过程不变。
对比例2
将实施例4中的有机蒙脱土原料去掉,其余原料及制备过程不变。
对比例3
将实施例4中的聚磷酸铵、阻燃助剂和纳米蒙脱土原料都去掉,其余原料及制备过程不变。
将实施例4-6和对比例1-3获得的扩链物分别加入至聚氨酯预聚体中,搅拌反应3min,最后将其快速倒入模具中,并使用扁平硫化机在100℃硫化1h,成型后将其放入100℃烘箱硫化24h,进行如下性能测试:
力学性能:按照GB/T 16584-1996,AL-7000M进行测试,拉伸速度为500mm/min;
基本性能:邵A硬度按GB/T531-1992测试;测试弹性体的回弹性和压缩复原率;
阻燃性能:垂直燃烧按GB/T2408-1996测试,氧指数按GB/T2406-1993测试;
测得的结果如下表所示:
由上表数据可知,本发明获得的聚氨酯弹性体材料具有较高的力学性能,尤其体现在拉伸强度上,具有符合使用要求的硬度、回弹性以及压缩复原率,此外,具备优良的阻燃防火性能,能够提高聚氨酯材料的使用安全性;结合对比例1的数据可知,阻燃助剂的加入不仅能够辅助提升聚氨酯的阻燃效果,且能促进聚氨酯交联网络结构的形成,提高聚氨酯的力学性能;结合对比例2的数据可知,纳米蒙脱土除能提升聚氨酯的力学性能以外,还能与其余阻燃成分协效阻燃,提升聚氨酯的阻燃效果。
实施例7
使用时,往聚氨酯预聚体中加入扩链物,搅拌反应3min,快速摊铺在需要铺装的体育场地中,在20-30℃条件下,30-60min内凝胶,24h内固化,14d完全熟化后可投入使用。
在说明书的描述中,参考术语“一个实施例”、“示例”、“具体示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不一定指的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。
以上内容仅仅是对本发明所作的举例和说明,所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代,只要不偏离发明或者超越本权利要求书所定义的范围,均应属于本发明的保护范围。
Claims (7)
1.基于聚氨酯弹性体的体育场地铺装材料,其特征在于,包括如下重量份原料:聚四氢呋喃醚二醇75-80份、2,4-甲苯二异氰酸酯20-25份、二甲硫基甲苯二胺9-12份、聚磷酸铵2-3份、阻燃助剂0.8-1.1份、有机蒙脱土7-9份;
其中,所述阻燃助剂通过如下步骤制备:
S1、将三聚氯氰溶于THF后加入至带有机械搅拌装置的四口烧瓶中,控制底物的温度为25℃,200r/min匀速搅拌下将N-甲基-2-羟基乙胺的THF溶解液逐滴滴入四口烧瓶中,滴完后将反应液升温至50℃,并在此恒温条件下反应48h,反应过程中,用浓度为0.1mol/L的NaOH溶液维持pH在10以上,反应结束后,后处理,得到中间体;
S2、将二甲苯烷二异氰酸酯和DMF加入三口烧瓶中,磁力搅拌并加热至55℃,将中间体与DMF形成的溶解液缓慢滴加进三口烧瓶中,之后再滴入二月桂酸二丁基锡,保持55℃恒温搅拌反应4h,反应结束后,纯化,获得阻燃助剂。
2.根据权利要求1所述的基于聚氨酯弹性体的体育场地铺装材料,其特征在于,步骤S1中N-甲基-2-羟基乙胺的THF溶解液中N-甲基-2-羟基乙胺的浓度为4.95g/mL;三聚氯氰、THF、N-甲基-2-羟基乙胺的THF溶解液的用量之比为18.44g:150mL:50mL。
3.根据权利要求1所述的基于聚氨酯弹性体的体育场地铺装材料,其特征在于,步骤S1中后处理过程:旋蒸,再利用甲苯多次萃取,有机相用饱和NaCl水溶液洗涤多次后用无水Na2SO4干燥48h,抽滤、减压浓缩。
4.根据权利要求1所述的基于聚氨酯弹性体的体育场地铺装材料,其特征在于,步骤S2中溶解液中中间体与DMF的用量之比为1g:5mL;二甲苯烷二异氰酸酯、DMF、溶解液的用量之比为8.25g:25mL:15mL:0.2mL。
5.根据权利要求1所述的基于聚氨酯弹性体的体育场地铺装材料,其特征在于,步骤S2中纯化过程:向产物中加入甲苯,再加入去离子水,静置分层后,取有机相,并用饱和NaCl水溶液洗涤多次后用无水Na2SO4干燥48h,抽滤、减压浓缩。
6.根据权利要求1所述的基于聚氨酯弹性体的体育场地铺装材料,其特征在于,所述有机蒙脱土为采用十八烷基三甲基溴化铵与蒙脱土层内的阳离子进行离子交换,得到的有机蒙脱土。
7.根据权利要求1所述的基于聚氨酯弹性体的体育场地铺装材料的制备方法,其特征在于,包括如下步骤:
第一步、取聚四氢呋喃醚二醇于四口烧瓶中,加热至105℃抽真空除水90min,降温至85℃,加入阻燃助剂,保持85℃反应1h,降温至50℃,缓慢滴加2,4-甲苯二异氰酸酯升温至80℃反应2h,之后抽真空除气泡,得到聚氨酯预聚体,密封备用;
第二步、将二甲硫基甲苯二胺、聚磷酸铵和有机蒙脱土混合后,研磨分散均匀后,再在80-90℃,真空脱水2h,冷却至50℃,得到扩链物,密封备用;
第三步、使用时,往聚氨酯预聚体中加入扩链物,搅拌反应3min,快速摊铺在需要铺装的体育场地中,完全熟化后投入使用。
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