CN104448227B - 一种聚氨酯复合材料及其制备方法 - Google Patents
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- 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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Abstract
本发明涉及复合材料领域,具体而言,涉及一种聚氨酯复合材料及其制备方法。一种聚氨酯复合材料,主要由以下原料制成:按重量份计,低聚物多元醇100份,异氰酸酯85‑95份,小分子扩链剂15‑25份,亚微米粒子1‑5份。本发明提供的聚氨酯复合材料,特定选用低聚物多元醇、异氰酸酯、小分子扩链剂和亚微米粒子这四种成分作为原料,其中,低聚物多元醇构成聚氨酯复合材料的软链段,异氰酸酯和小分子扩链剂构成聚氨酯复合材料的刚性链段,亚微米粒子提供更多的交联点;通过优化各成分之间的配比,使制得的聚氨酯复合材料的耐磨性能和力学性能得到很大的提高。其制备方法简单易行,制得的聚氨酯复合材料的耐磨性能和力学性能优越。
Description
技术领域
本发明涉及复合材料领域,具体而言,涉及一种聚氨酯复合材料及其制备方法。
背景技术
聚氨酯弹性体,又称为聚氨基甲酸酯弹性体,是一种主链上含有重复氨基甲酸酯基团(—NHCOO—)的高分子合成材料,是典型的嵌段共聚物,一般由聚酯、聚醚和聚烯烃等低聚物多元醇与多异氰酸酯及二醇或二胺类扩链剂逐步加成聚合而成。
从聚集态来看,聚氨酯大分子主链是由玻璃化温度低于室温的柔性链段和玻璃化温度高于室温的刚性链段嵌段而成的。低聚物多元醇(如聚醚、聚酯等)构成软链段,二异氰酸酯和小分子扩链剂(二胺或二醇)构成刚性链段(亦称硬链段或硬段)。同时两相通过氢键的作用形成物理交联。在聚氨酯弹性体分子结构中,软链段占的比例较大,约50%~90%。由于硬链段的极性强,相互间引力大,硬链段和软链段在热力学上具有自发分离的倾向,聚氨酯就会出现微相分离的形态,微相分离是聚氨酯弹性体物理结构的特征,聚氨酯弹性体的物性不仅于化学结构有关,而且与微相分离的程度有关,微相分离程度取决于硬段之间或者硬段与软段之间的相互作用(亲和力),聚氨酯弹性体的硬度、拉伸强度、撕裂强度主要取决于硬段的组成、硬段长度和硬段相区的数量及分布。
亚微米粒子一般是指粒度在100纳米到1微米的粉末或颗粒,亚微米粒子具有特殊的表面效应和体积效应,并由此产生许多与块状样品以及纳米粒子不同的物理化学性质。亚微米粒子的增韧增强改性机理具有以下特征:(1)聚合物基体中的无机亚微米粒子作为聚合物分子链的交联点,对复合材料的抗拉强度有贡献;(2)无机亚微米粒子具有应力集中与应力辐射的平衡效应,通过吸收冲击能量与辐射能量,使基体无明显的应力集中现象,达到复合材料的力学平衡状态;(3)无机亚微米粒子具有能量传递效应,使基体树脂裂纹扩展受阻和钝化,最终终止裂纹,不致发展为破坏性开裂;(4)随着亚微米粒子粒径的减小,粒子的比表面积增大,亚微米微粒与基体接触面积增大,材料受冲击时产生更多的微裂纹,吸收更多的冲击能;(5)若亚微米微粒用量过多或填料粒径较大,复合材料的应力集中较为明显,微裂纹易发展成宏观开裂,造成复合材料性能下降。
聚氨酯弹性体由于具有优异的耐磨性能、高强度、耐腐蚀、耐冲击性能和与其他材料粘接性能好等特点,是一种性能优异的工程材料。在油田、矿山、机械、纺织、建筑等领域大量应用,已成为一种不可缺少的工程材料。但其耐磨性能、力学性能还有待提高。
有鉴于此,特提出本发明。
发明内容
本发明的第一目的在于提供一种聚氨酯复合材料,所述的聚氨酯复合材料通过选用特定的原料及其配比,使其耐磨性能得到很大的提高。
本发明的第二目的在于提供一种所述的聚氨酯复合材料的制备方法,该方法简单易行,制得的聚氨酯复合材料耐磨性能和力学性能好。
为了实现本发明的上述目的,特采用以下技术方案:
一种聚氨酯复合材料,主要由以下原料制成:按重量份计,低聚物多元醇100份,异氰酸酯85-95份,小分子扩链剂15-25份,亚微米粒子1-5份。
本发明提供的聚氨酯复合材料,特定选用低聚物多元醇、异氰酸酯、小分子扩链剂和亚微米粒子这四种成分作为原料,其中,低聚物多元醇构成聚氨酯复合材料的软链段,异氰酸酯和小分子扩链剂构成聚氨酯复合材料的刚性链段,亚微米粒子提供更多的交联点;通过优化各成分之间的配比,使制得的聚氨酯复合材料的耐磨性能和力学性能得到很大的提高。
为了进一步增强制得的聚氨酯复合材料的耐磨性能和力学性能,优选地,按重量份计,低聚物多元醇100份,异氰酸酯88-90份,小分子扩链剂20-22份,亚微米粒子2-3份。
若使用的低聚物多元醇的重均分子量太低,容易造成软段和硬段之间的连接太弱,从而使制得的聚氨酯复合材料性能降低。本发明人通过调节各成分之间的配比,添加特定的亚微米粒子,加强了软硬段之间的连接,在使用较小重均分子量的低聚物多元醇时,软硬段之间的连接得到加强,并且增加了硬段的比重,增加了聚氨酯复合材料的硬度、拉伸强度和撕裂强度。优选地,所述低聚物多元醇的重均分子量为950-2050,优选为1000-1400。
进一步地,所述低聚物多元醇选自聚四氢呋喃醚二醇、THF-均聚醚二醇中的任一种或两种。
本发明从众多硬段原料中筛选,得到选用甲苯-2,4-二异氰酸酯、甲苯-2,6-二异氰酸酯中的任一种或两种,制得的聚氨酯复合材料的耐磨性能和力学性能均得到很大的提高。优选地,所述异氰酸酯选自甲苯-2,4-二异氰酸酯、甲苯-2,6-二异氰酸酯中的任一种或两种。
优选地,所述小分子扩链剂为3,3-二氯-4,4-二苯基甲烷二胺。该小分子扩链剂增强了软硬段之间的连接强度,使各原料分散更为均匀,分子支链更多,不易缠结,稳定性更好。
本发明从众多亚微米粒子中筛选,其中,经验证,常用的碳酸钙添加后,得到的聚氨酯复合材料耐磨性能和力学性能提高较小。但选用TiO2、Si3N4中的任一种或两种,很大的提升了聚氨酯复合材料强度和韧性,其中,以Si3N4更佳。优选地,所述亚微米粒子包括TiO2、Si3N4中的任一种或两种,优选为Si3N4。
另外,本申请人通过添加醋酸盐,意外的发现,醋酸根其羧基上的两个原子氧同时和低聚物多元醇上的羟基形成氢键,增强了聚氨酯大分子链间的相互作用力,制得的聚氨酯复合材料的韧性和强度均有较大的提高。优选地,所述原料还包括醋酸盐,所述醋酸盐的用量为所述原料总重量的1%-4%,所述醋酸盐选自醋酸钾、醋酸钠、醋酸铵、醋酸钙中的一种或多种,所述醋酸盐更优选为醋酸钾。
本发明还提供了所述聚氨酯复合材料的制备方法,包括以下步骤:
将所述异氰酸酯超声波处理15-20min,备用;
将所述亚微米粒子进行表面处理,备用;
将所述低聚物多元醇在搅拌速度为2500-2800r/min状态下,升温至95-105℃,真空脱水80-100min;保持温度和转速,在氮气保护下,加入超声波处理的异氰酸酯和表面处理的亚微米粒子,真空脱水130-150min;
加入所述小分子扩链剂,混合均匀,真空脱泡后浇入涂有脱模剂的模具中,室温硫化,固化完全后,冷却脱模,即得。
本发明提供的所述聚氨酯复合材料的制备方法,将异氰酸酯、亚微米粒子和低聚物多元醇处理后在氮气的保护下混匀,得到预聚体,然后加入小分子扩链剂反应,通过硫化固化制得聚氨酯复合材料。该制备方法简单易行,制得的聚氨酯复合材料的耐磨性能和力学性能优越。
优选地,所述亚微米粒子进行表面处理具体为:将所述亚微米粒子浸渍在丙酮溶剂稀释的偶联剂KH-550中,然后于58-65℃下超声波振荡28-35min。亚微米粒子经过该处理,偶联剂KH-550包覆在每个亚微米粒子的表面,使亚微米粒子能稳定提供更多的交联点,增强了各原料之间的连接强度。
进一步地,所述原料还包括醋酸盐,所述醋酸盐的用量为所述原料总重量的1%-4%,优选地,所述醋酸盐选自醋酸钾、醋酸钠、醋酸铵、醋酸钙中的一种或多种,更优选为醋酸钾;所述醋酸盐与异氰酸酯、亚微米粒子一起添加。通过添加醋酸盐,能同时提高聚氨酯的韧性和强度。
与现有技术相比,本发明的有益效果为:
(1)本发明提供的聚氨酯复合材料,特定选用低聚物多元醇、异氰酸酯、小分子扩链剂和亚微米粒子这四种成分作为原料,通过优化各成分之间的配比,制得的聚氨酯复合材料的耐磨性能和力学性能得到很大的提高;
(2)特定选用TiO2、Si3N4中的任一种或两种,使亚微米粒子能稳定提供更多的交联点,增强了各原料之间的连接强度,很大的提升了聚氨酯复合材料的强度和韧性;
(3)通过添加醋酸盐,能同时提升聚氨酯的韧性和强度;
(4)本发明提供的聚氨酯复合材料的制备方法,简单易行,制得的聚氨酯复合材料耐磨性能和力学性能优越。
具体实施方式
下面将结合实施例对本发明的实施方案进行详细描述,但是本领域技术人员将会理解,下列实施例仅用于说明本发明,而不应视为限制本发明的范围。实施例中未注明具体条件者,按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者,均为可以通过市售获得的常规产品。
实施例1
按重量份计,取以下原料:低聚物多元醇100份,异氰酸酯85份,小分子扩链剂25份,亚微米粒子1份;
其中,低聚物多元醇为聚四氢呋喃醚二醇,其重均分子量为1000±50;异氰酸酯为甲苯-2,4-二异氰酸酯;小分子扩链剂为3,3-二氯-4,4-二苯基甲烷二胺;亚微米粒子为TiO2;
将异氰酸酯超声波处理15min,备用;
将亚微米粒子浸渍在丙酮溶剂稀释的偶联剂KH-550中,然后于58℃下超声波振荡35min,备用;
将低聚物多元醇在搅拌速度为2500r/min状态下,升温至95℃,真空脱水80min;保持温度和转速,在氮气保护下,加入超声波处理的异氰酸酯和表面处理的亚微米粒子,真空脱水150min;
加入所述小分子扩链剂,混合均匀,真空脱泡后浇入涂有脱模剂的模具中,室温硫化,固化完全后,冷却脱模,即得所述聚氨酯复合材料。
实施例2
按重量份计,取以下原料:低聚物多元醇100份,异氰酸酯88份,小分子扩链剂22份,亚微米粒子2份;
其中,低聚物多元醇为四氢呋喃醚二醇,其重均分子量为2000±50;异氰酸酯为甲苯-2,6-二异氰酸酯;小分子扩链剂为3,3-二氯-4,4-二苯基甲烷二胺;亚微米粒子为Si3N4;
将异氰酸酯超声波处理20min,备用;
将亚微米粒子浸渍在丙酮溶剂稀释的偶联剂KH-550中,然后于65℃下超声波振荡28min,备用;
将低聚物多元醇在搅拌速度为2800r/min状态下,升温至105℃,真空脱水100min;保持温度和转速,在氮气保护下,加入超声波处理的异氰酸酯和表面处理的亚微米粒子,真空脱水130min;
加入所述小分子扩链剂,混合均匀,真空脱泡后浇入涂有脱模剂的模具中,室温硫化,固化完全后,冷却脱模,即得所述聚氨酯复合材料。
实施例3
按重量份计,取以下原料:低聚物多元醇100份,异氰酸酯88份,小分子扩链剂22份,亚微米粒子2份,醋酸铵1.13份;
其中,低聚物多元醇为四氢呋喃醚二醇,其重均分子量为2000±50;异氰酸酯为甲苯-2,6-二异氰酸酯;小分子扩链剂为3,3-二氯-4,4-二苯基甲烷二胺;亚微米粒子为Si3N4;
将异氰酸酯超声波处理20min,备用;
将亚微米粒子浸渍在丙酮溶剂稀释的偶联剂KH-550中,然后于65℃下超声波振荡28min,备用;
将低聚物多元醇在搅拌速度为2800r/min状态下,升温至105℃,真空脱水100min;保持温度和转速,在氮气保护下,加入超声波处理的异氰酸酯和表面处理的亚微米粒子以及醋酸钾,真空脱水130min;
加入所述小分子扩链剂,混合均匀,真空脱泡后浇入涂有脱模剂的模具中,室温硫化,固化完全后,冷却脱模,即得所述聚氨酯复合材料。
实施例4
按重量份计,取以下原料:低聚物多元醇100份,异氰酸酯90份,小分子扩链剂20份,亚微米粒子3份;
其中,低聚物多元醇为THF-均聚醚二醇,其重均分子量为1000;异氰酸酯为甲苯-2,4-二异氰酸酯和甲苯-2,6-二异氰酸酯按重量比为1:1进行混合的混合物;小分子扩链剂为3,3-二氯-4,4-二苯基甲烷二胺;亚微米粒子为TiO2和Si3N4按重量比为1:1混合的混合物;
将异氰酸酯超声波处理20min,备用;
将亚微米粒子浸渍在丙酮溶剂稀释的偶联剂KH-550中,然后于60℃下超声波振荡30min,备用;
将低聚物多元醇在搅拌速度为2600r/min状态下,升温至100℃,真空脱水90min;保持温度和转速,在氮气保护下,加入超声波处理的异氰酸酯和表面处理的亚微米粒子,真空脱水140min;
加入所述小分子扩链剂,混合均匀,真空脱泡后浇入涂有脱模剂的模具中,室温硫化,固化完全后,冷却脱模,即得所述聚氨酯复合材料。
实施例5
按重量份计,取以下原料:低聚物多元醇100份,异氰酸酯90份,小分子扩链剂20份,亚微米粒子3份,醋酸钾6.587份;
其中,低聚物多元醇为THF-均聚醚二醇,其重均分子量为1000;异氰酸酯为甲苯-2,4-二异氰酸酯和甲苯-2,6-二异氰酸酯按重量比为1:1进行混合的混合物;小分子扩链剂为3,3-二氯-4,4-二苯基甲烷二胺;亚微米粒子为TiO2和Si3N4按重量比为1:1混合的混合物;
将异氰酸酯超声波处理20min,备用;
将亚微米粒子浸渍在丙酮溶剂稀释的偶联剂KH-550中,然后于60℃下超声波振荡30min,备用;
将低聚物多元醇在搅拌速度为2600r/min状态下,升温至100℃,真空脱水90min;保持温度和转速,在氮气保护下,加入超声波处理的异氰酸酯和表面处理的亚微米粒子以及醋酸钾,真空脱水140min;
加入所述小分子扩链剂,混合均匀,真空脱泡后浇入涂有脱模剂的模具中,室温硫化,固化完全后,冷却脱模,即得所述聚氨酯复合材料。
实施例6
按重量份计,取以下原料:低聚物多元醇100份,异氰酸酯95份,小分子扩链剂15份,亚微米粒子5份;
其中,低聚物多元醇为聚四氢呋喃醚二醇和THF-均聚醚二醇按重量比为1:1的混合物,聚四氢呋喃醚二醇的重均分子量为1400±50,THF-均聚醚二醇的重均分子量为1000;异氰酸酯为甲苯-2,4-二异氰酸酯和甲苯-2,6-二异氰酸酯按1:3混合的混合物;小分子扩链剂为3,3-二氯-4,4-二苯基甲烷二胺;亚微米粒子为Si3N4;
将异氰酸酯超声波处理20min,备用;
将亚微米粒子浸渍在丙酮溶剂稀释的偶联剂KH-550中,然后于65℃下超声波振荡30min,备用;
将低聚物多元醇在搅拌速度为2800r/min状态下,升温至100℃,真空脱水100min;保持温度和转速,在氮气保护下,加入超声波处理的异氰酸酯和表面处理的亚微米粒子,真空脱水150min;
加入所述小分子扩链剂,混合均匀,真空脱泡后浇入涂有脱模剂的模具中,室温硫化,固化完全后,冷却脱模,即得所述聚氨酯复合材料。
实施例7
按重量份计,取以下原料:低聚物多元醇100份,异氰酸酯90份,小分子扩链剂20份,亚微米粒子3份,醋酸钾8.875份;
其中,低聚物多元醇为THF-均聚醚二醇,其重均分子量为1000;异氰酸酯为甲苯-2,4-二异氰酸酯和甲苯-2,6-二异氰酸酯按重量比为1:1进行混合的混合物;小分子扩链剂为3,3-二氯-4,4-二苯基甲烷二胺;亚微米粒子为TiO2和Si3N4按重量比为1:1混合的混合物;
将异氰酸酯超声波处理20min,备用;
将亚微米粒子浸渍在丙酮溶剂稀释的偶联剂KH-550中,然后于60℃下超声波振荡30min,备用;
将低聚物多元醇在搅拌速度为2600r/min状态下,升温至100℃,真空脱水90min;保持温度和转速,在氮气保护下,加入超声波处理的异氰酸酯和表面处理的亚微米粒子以及醋酸钾,真空脱水140min;
加入所述小分子扩链剂,混合均匀,真空脱泡后浇入涂有脱模剂的模具中,室温硫化,固化完全后,冷却脱模,即得所述聚氨酯复合材料。
试验例1
将实施例1-6制得的聚氨酯复合材料进行拉伸强度、断裂伸长率、硬度、以及磨损性能的测定,测定标准为:用CMT6104微机控制万能(拉力)试验机,按照GB-T1040-92方法测定复合材料的扯断伸长率和拉伸强度;硬度测试按橡胶邵氏D型实验方法;磨损性能测定方法为:采用MSH型冲蚀磨损试验进行冲蚀磨损试验,悬臂上装有4个试样,当试样插入浆体中一定深度转动时与浆体中的磨料发生撞击,造成冲蚀磨损,用45#钢进行误差校核,测得该方法平均误差为5%;磨蚀面为浇注底面,冲蚀磨损线速度为317m/s,攻角为30°,浆体浓度为40%(415L清水加入3L的石英砂);pH=7,石英砂粒度为0105~0118mm;每组试样更换1次浆体,每次冲蚀试验时间为48h;用失重法评价复合材料相对抗冲蚀磨损性;相对抗冲蚀磨损性β=(对比试样磨损量Δw’/对比试样密度)/(试样磨损量Δw/试样密度,对比试样为纯聚氨酯弹性体(-NCO%=6%)。测得的数据如表1所示。
表1 聚氨酯复合材料的性能测定
从表1可以看出,本发明提供的聚氨酯复合材料的耐磨性能、韧性和硬度都非常优越,特别是在添加了醋酸盐以后,聚氨酯的韧性和硬度同时得到了较大的提高,很好的满足了市场的需求。
尽管已用具体实施例来说明和描述了本发明,然而应意识到,在不背离本发明的精神和范围的情况下可以作出许多其它的更改和修改。因此,这意味着在所附权利要求中包括属于本发明范围内的所有这些变化和修改。
Claims (14)
1.一种聚氨酯复合材料,其特征在于,主要由以下原料制成:按重量份计,低聚物多元醇100份,异氰酸酯85-95份,小分子扩链剂15-25份,亚微米粒子1-5份;
所述亚微米粒子为TiO2、Si3N4中的任一种或两种;
所述原料还包括醋酸盐,所述醋酸盐的用量为所述原料总重量的1%-4%。
2.根据权利要求1所述的聚氨酯复合材料,其特征在于,所述低聚物多元醇的重均分子量为950-2050。
3.根据权利要求1所述的聚氨酯复合材料,其特征在于,所述低聚物多元醇的重均分子量为1000-1400。
4.根据权利要求1所述的聚氨酯复合材料,其特征在于,所述低聚物多元醇选自聚四氢呋喃醚二醇、THF-均聚醚二醇中的任一种或两种。
5.根据权利要求1所述的聚氨酯复合材料,其特征在于,所述异氰酸酯选自甲苯-2,4-二异氰酸酯、甲苯-2,6-二异氰酸酯中的任一种或两种。
6.根据权利要求1所述的聚氨酯复合材料,其特征在于,所述小分子扩链剂为3,3-二氯-4,4-二苯基甲烷二胺。
7.根据权利要求1所述的聚氨酯复合材料,其特征在于,所述亚微米粒子为Si3N4。
8.根据权利要求1所述的聚氨酯复合材料,其特征在于,所述醋酸盐选自醋酸钾、醋酸钠、醋酸铵、醋酸钙中的一种或多种。
9.根据权利要求8所述的聚氨酯复合材料,其特征在于,所述醋酸盐为醋酸钾。
10.权利要求1-7任一项所述的聚氨酯复合材料的制备方法,其特征在于,包括以下步骤:
将所述异氰酸酯超声波处理15-20min,备用;
将所述亚微米粒子进行表面处理,备用;
将所述低聚物多元醇在搅拌速度为2500-2800r/min状态下,升温至95-105℃,真空脱水80-100min;保持温度和转速,在氮气保护下,加入超声波处理的异氰酸酯和表面处理的亚微米粒子,真空脱水130-150min;
加入所述小分子扩链剂,混合均匀,真空脱泡后浇入涂有脱模剂的模具中,室温硫化,固化完全后,冷却脱模,即得。
11.根据权利要求10所述的聚氨酯复合材料的制备方法,其特征在于,所述亚微米粒子进行表面处理具体为:将所述亚微米粒子浸渍在丙酮溶剂稀释的偶联剂KH-550中,然后于58-65℃下超声波振荡28-35min。
12.根据权利要求10所述的聚氨酯复合材料的制备方法,其特征在于,所述原料还包括醋酸盐,所述醋酸盐的用量为所述原料总重量的1%-4%;所述醋酸盐与异氰酸酯、亚微米粒子一起添加。
13.根据权利要求12所述的聚氨酯复合材料的制备方法,其特征在于,所述醋酸盐选自醋酸钾、醋酸钠、醋酸铵、醋酸钙中的一种或多种。
14.根据权利要求12所述的聚氨酯复合材料的制备方法,其特征在于,所述醋酸盐为醋酸钾。
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