CN104448202B - 含磷阻燃热塑性聚氨酯弹性体的制备方法 - Google Patents
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Abstract
含磷阻燃热塑性聚氨酯弹性体的制备方法,含磷阻燃热塑性聚氨酯弹性体的原料及其质量分数为:含磷聚酯二元醇65%~80%,TDI11%~30%,1,4‑丁二醇1.7%~3.7%,冰乙酸1.0~2.5%,二月桂酸二丁基锡0.2~0.3%;其制备步骤为:以脱水处理的含磷聚酯二元醇和TDI为单体,向加有含磷聚酯二元醇的反应器中滴加配方量的TDI,滴加完后加入配方量的二月桂酸二丁基锡,在85℃下保温。每隔0.5h用二正丁胺法测预聚体中NCO的含量,30min内稳定不变后分步加入1,4‑丁二醇和用来封端的冰乙酸,反应0.5h后倒入预热的自制模具中,放入110~120℃的烘箱中熟化6h,得到含磷阻燃热塑性聚氨酯弹性体。
Description
技术领域
本发明属于阻燃材料领域,具体涉及一种含磷阻燃热塑性聚氨酯弹性体的制备方法。
背景技术
热塑性聚氨酯弹性体又称为热塑性聚氨酯橡胶,简称TPU,是一种嵌段线性聚合物,硬段为二异氰酸酯与扩链剂组成,软段为分子量为1000~3000的聚酯或聚醚多元醇。可熔可溶,具有高强度,高弹性和优良耐磨,耐候性,耐油,耐低温等优点。广泛应用于电线电缆,橡胶传送带,汽车工业用品等。
添加型阻燃剂已经在TPU阻燃方面得到了应用,但其添加量较大,对力学性能的影响较为明显,与TPU的混合性能不佳,阻燃剂容易析出。反应型阻燃剂克服了以上缺点,并且用量较小就可以达到较好的阻燃效果,因此制备反应型阻燃聚氨酯弹性体就具有重要的应用价值。
专利CN102276784A公开了一种环保完全达标的无卤阻燃聚氨酯弹性体,以重量百分比计,包括以下原料:三羟乙基异氰尿酸酯5-10%,金属氢氧化物3-10%,膨胀型石墨3-5%,聚醚多元醇30-45%,二异氰酸酯25-35%,扩链剂5-10%,抗氧剂0.1-0.5%,催化剂0.1-0.5%。该发明所述的无卤阻燃聚氨酯弹性体,在制备过程中没有添加含卤阻燃剂,添加的为无卤阻燃剂,而且,采用的其它原料也都是不会导致成品环保不达标的物质;这样得到的无卤阻燃聚氨酯弹性体具有良好的阻燃性能,其阻燃性可达V-0级(UL-94)。
TPU容易燃烧,燃烧时火焰非常剧烈且伴有浓烟,同时还有严重的熔滴现象。随着国内外对防火性能和环保性能的要求越来越严格,许多学者把目光转向对热塑性聚氨酯弹性体阻燃技术的研究。
阻燃聚氨酯材料在制备过程中添加无机阻燃剂会导致材料性能和使用寿命降低。
发明内容
本发明的目的是提供一种含磷阻燃热塑性聚氨酯弹性体的制备方法。
本发明是含磷阻燃热塑性聚氨酯弹性体的制备方法,其制备方法的具体步骤如下:
以脱水处理的含磷聚酯二元醇和TDI为单体,采用预聚体法合成聚氨酯;设预聚物中NCO/OH值R为3.5,并计算TDI的滴加量,向加有含磷聚酯二元醇的反应器中滴加TDI,滴加完后加入适量的二月桂酸二丁基锡,在85℃下保温;每隔0.5h用二正丁胺法测预聚体中NCO的含量,待达到预定值后分步加入丁二醇,用来封端的冰乙酸,反应0.5h后倒入预热的模具中,放入110~120℃的烘箱中熟化6h,得到含磷阻燃热塑性聚氨酯弹性体;
基于制备含磷阻燃热塑性聚氨酯弹性体的总质量,按质量百分比计,其所用的原料及其质量分数为:
含磷聚酯二元醇65%~80%,TDI11%~30%,丁二醇1.7%~3.7%,冰乙酸1.0%~2.5%。
本发明的有益之处是:通过分子设计,在聚氨酯弹性体材料分子链中引入阻燃元素磷,降低无机阻燃剂的添加,使得材料阻燃氧指数由19提高到32,阻燃性能良好。本发明具有原料廉价易得,操作简单,无需溶剂,环保的优点。
具体实施方式
本发明是含磷阻燃热塑性聚氨酯弹性体的制备方法,其技术方案为:
第一步 含磷聚酯二元醇制备的具体步骤如下:
采用一步法合成聚酯二元醇,在装有搅拌器、温度计、冷凝管、分水器的容器中加入己二酸﹑6-氧-6H-二苯并(c,e)(1,2)氧磷杂己环-6-酮-丁二酸(DOPOMA)﹑邻苯二甲酸酐﹑乙二醇、1,2-丙二醇、二甲苯、对甲苯磺酸,缓慢升温。待固体全部溶解后,开始搅拌,继续缓慢升温至140℃。采用阶梯升温法,140℃~150℃恒温1h,150~160℃恒温1h,继续缓慢升温,最高温度不得超过230℃。当出水量接近理论值时,降温至180~220℃抽真空,真空度逐渐增大,最后达到0.08~0.09MPa,直至酸值降到10mgKOH/g以下停止反应。根据GB/T 5530-2005标准测酸值,用吡啶-高氯酸法测羟值,控制羟值40~60mgKOH/g。
上述含磷聚酯二元醇制备所用的原料及其质量分数为:
邻苯二甲酸酐20%~24%,己二酸33%~40%,DOPOMA4%~17%,乙二醇20%~22%,丙二醇8%~9%,催化剂0.03%~0.05%,带水剂5%~10%。
含磷聚酯二元醇的制备方法中丁二醇为1,4-丁二醇,丙二醇为1,2-丙二醇,乙二醇﹑丙二醇的物质的量之比为3:1,己二酸﹑邻苯二甲酸酐的物质的量之比为1:0.6,改变DOPOMA与上述两种酸的物质的量之比可以合成不同磷含量的聚酯二元醇,催化剂为对甲苯磺酸,带水剂为二甲苯。
第二步 含磷阻燃热塑性聚氨酯弹性体制备的具体步骤如下:
以脱水处理的聚酯二元醇和TDI为单体,采用预聚体法合成聚氨酯。设预聚物中NCO/OH值R为3.5,并计算TDI的滴加量,滴加完后加入配方量的二月桂酸二丁基锡,在85℃下保温。每隔0.5h用二正丁胺法测预聚体中NCO的含量,30min内稳定不变后分步加入1,4-丁二醇,冰乙酸(用来封端),反应0.5h后倒入预热的模具(自制)中,放入110~120℃的烘箱中熟化6h。
含磷阻燃热塑性聚氨酯弹性体的原料及其质量分数为:聚酯二元醇65%~80%,TDI11%~30%,1,4-丁二醇1.7%~3.7%,冰乙酸1.0~2.5%,二月桂酸二丁基锡0.2~0.3%;所述的的聚酯二元醇的平均分子量为1500~2500,TDI为甲苯-2,4-二异氰酸酯或甲苯-2,6-二异氰酸酯。
下面以具体实施例来对本发明做进一步说明,但本发明的保护范围不限于此中。
实施例1
采用一步法合成聚酯二元醇,在装有搅拌器、温度计、冷凝器、分水器的容器中加入36.8kg己二酸﹑5kg DOPOMA﹑22.4kg邻苯二甲酸酐﹑20.8kg乙二醇、8.5kg 1,2-丙二醇、6kg二甲苯、40g对甲苯磺酸,缓慢升温。待固体全部溶解后,开始搅拌,继续缓慢升温至140℃。采用阶梯升温法,140℃~150℃恒温1h,150~160℃恒温1h,继续缓慢升温,最高温度不得超过230℃。当出水量接近理论值时,降温至180~220℃抽真空,真空度逐渐增大,最后达到0.08~0.09MPa,直至酸值降到10mgKOH/g以下停止反应。根据GB/T 5530-2005标准测酸值,用吡啶-高氯酸法测羟值,控制羟值40~60mgKOH/g。
实施例2
采用一步法合成聚酯二元醇,在装有搅拌器、温度计、冷凝器、分水器的容器中加入34.9kg己二酸﹑6kg DOPOMA﹑22kg邻苯二甲酸酐﹑22kg乙二醇、8.9kg 1,2-丙二醇、6kg二甲苯、50g对甲苯磺酸,缓慢升温。待固体全部溶解后,开始搅拌,继续缓慢升温至140℃。采用阶梯升温法,140℃~150℃恒温1h,150~160℃恒温1h,继续缓慢升温,最高温度不得超过230℃。当出水量接近理论值时,降温至180~220℃抽真空,真空度逐渐增大,最后达到0.08~0.09MPa,直至酸值降到10mgKOH/g以下停止反应。根据GB/T 5530-2005标准测酸值,用吡啶-高氯酸法测羟值,控制羟值40~60mgKOH/g。
实施例3
以经过脱水处理的聚酯二元醇和TDI为单体,采用预聚体法合成聚氨酯。设预聚物中R值为3.5,向加有65kg含磷聚酯二元醇的反应器中滴加28kgTDI,滴加完后加入2kg二月桂酸二丁基锡,在85℃下保温;每隔0.5h用二正丁胺法测预聚体中NCO的含量,30min内稳定不变后分步加入2.5kg丁二醇和2.5kg用来封端的冰乙酸,反应0.5h后倒入预热的自制模具中,放入110~120℃的烘箱中熟化6h,得到含磷阻燃热塑性聚氨酯弹性体。
实施例4
以经过脱水处理的聚酯二元醇和TDI为单体,采用预聚体法合成聚氨酯。设预聚物中R值为3.5,向加有70kg含磷聚酯二元醇的反应器中滴加22kgTDI,滴加完后加入3kg二月桂酸二丁基锡,在85℃下保温;每隔0.5h用二正丁胺法测预聚体中NCO的含量,30min内稳定不变后分步加入2.7kg丁二醇和2.3kg用来封端的冰乙酸,反应0.5h后倒入预热的自制模具中,放入110~120℃的烘箱中熟化6h,得到含磷阻燃热塑性聚氨酯弹性体。
Claims (3)
1.含磷阻燃热塑性聚氨酯弹性体的制备方法,其特征在于:制备方法的具体步骤如下:
第一步:含磷聚酯二元醇制备的具体步骤如下:采用一步法合成聚酯二元醇,在装有搅拌器、温度计、冷凝管、分水器的三口烧瓶中加入己二酸、6-氧-6H-二苯并(c,e)(1,2)氧磷杂己环-6-酮-丁二酸、邻苯二甲酸酐、乙二醇、丙二醇、带水剂、催化剂,缓慢升温;待固体全部溶解后,开始搅拌,继续缓慢升温至140℃;采用阶梯升温法,140℃~150℃恒温1h,150~160℃恒温1h,继续缓慢升温,最高温度不得超过230℃;当出水量接近理论值时,降温至180~220℃抽真空,真空度逐渐增大,最后达到0.08~0.09MPa,直至酸值降到10mgKOH/g以下停止反应;根据GB/T 5530-2005标准测酸值,用吡啶-高氯酸法测羟值,控制羟值40~60mgKOH/g;
第二步,以脱水处理的含磷聚酯二元醇和TDI为单体,采用预聚体法合成聚氨酯;设预聚物中NCO/OH值R为3.5,并计算TDI的滴加量,向加有含磷聚酯二元醇的反应器中滴加TDI,滴加完后加入适量的二月桂酸二丁基锡,在85℃下保温;每隔0.5h用二正丁胺法测预聚体中NCO的含量,待达到预定值后分步加入丁二醇,用来封端的冰乙酸,反应0.5h后倒入预热的模具中,放入110~120℃的烘箱中熟化6h,得到含磷阻燃热塑性聚氨酯弹性体;
基于制备含磷聚酯二元醇的总质量,所用的原料及其质量分数为:
邻苯二甲酸酐20%~24%,己二酸33%~40%,DOPOMA 4%~17%,乙二醇20%~22%,丙二醇8%~9%,催化剂0.03%~0.05%,带水剂5%~10%;
基于制备含磷阻燃热塑性聚氨酯弹性体的总质量,所用原料的质量百分含量之和满足100%,按质量百分比计,其所用的原料及其质量分数为:
含磷聚酯二元醇65%~80%,TDI11%~30%,丁二醇1.7%~3.7%,冰乙酸1.0%~2.5%。
2.根据权利要求1所述的含磷阻燃热塑性聚氨酯弹性体的制备方法,其特征在于:含磷聚酯二元醇的平均分子量为1500~2500,TDI为甲苯-2,4-二异氰酸酯或甲苯-2,6-二异氰酸酯。
3.根据权利要求1所述的含磷阻燃热塑性聚氨酯弹性体的制备方法,其特征在于:丁二醇为1,4-丁二醇,丙二醇为1,2-丙二醇,乙二醇、丙二醇的物质的量之比为3:1,己二酸、邻苯二甲酸酐的物质的量之比为1:0.6,改变DOPOMA与己二酸、邻苯二甲酸酐的物质的量之比可以合成不同磷含量的聚酯二元醇,催化剂为对甲苯磺酸,带水剂为二甲苯。
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