CN110845720B - 一种含溴阻燃聚醚多元醇及其制备方法 - Google Patents
一种含溴阻燃聚醚多元醇及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种含溴阻燃聚醚多元醇的制备方法,其特征在于,采用含溴化合物作为起始剂,在催化剂作用下,加入环氧丙烷,控制温度进行聚合反应,制得聚醚多元醇A;在聚醚多元醇A中加入小分子醛和二乙醇胺进行曼尼西反应,反应温度为60~80℃,脱水后得到含溴阻燃聚醚多元醇。本发明制备的含溴聚醚多元醇具有官能度高、反应活性高,阻燃性及稳定性好等优点,采用该含溴阻燃聚醚多元醇制备的硬质聚氨酯泡沫塑料具有优异的阻燃性能和力学性能。
Description
技术领域
本发明涉及一种含溴阻燃聚醚多元醇及其制备方法,属于高分子合成技术领域。
背景技术
硬质聚氨酯泡沫材料具有隔热效果好、强度高、耐候性好、粘结牢固等优点,在建筑及工业领域具有广泛的应用。但是硬质聚氨酯泡沫存在阻燃性能差、易燃烧等缺点,因此,聚氨酯泡沫体系的防火和阻燃问题一直是现在研究的热点。其中,构成硬质聚氨酯泡沫材料的主要成分聚醚多元醇是阻燃技术研究的重点,聚醚多元醇按其阻燃方式可分为两类:添加型阻燃聚醚多元醇和反应型阻燃聚醚多元醇。反应型阻燃聚醚多元醇是通过化学反应的方式接入到聚氨酯材料分子链中,该种方式对基材性能损害小,阻燃性能持久,是当前阻燃领域的主流趋势。
专利CN201510078499.2公开了一种高官能度高阻燃多元醇的制备方法,具体是将含溴环氧树脂与二元醇按一定的摩尔比混合,加入聚氨酯催化剂,加热反应得到中间体多元醇;再加入一定质量比的含磷阻燃剂,在120℃搅拌均匀既得产品。该发明优点在于根据现有市场常用的原材料,就能生产出高官能度、高强度的、高阻燃性能的含溴含磷聚醚多元醇产品。
专利CN201410511867.3,公开了一种含氮含溴阻燃聚醚的制备方法及制得产品的应用,该阻燃聚醚含有N、Br元素,是一种反应型阻燃聚醚。制备方法是由以乙二胺和二溴新戊二醇做起始剂;加入催化剂二甲胺;通入环氧丙烷反应得到产品。采用该阻燃聚醚制备的聚氨酯泡沫塑料具有良好的阻燃效果,相对于外加阻燃剂制备的聚氨酯泡沫塑料阻燃性能稳定,泡沫质量更好。
目前,常规的含溴阻燃聚醚多元醇基本都是以含溴化合物为起始剂、通过与环氧乙烷和环氧丙烷的聚合反应得到,虽然阻燃性能良好,但存在官能度低,产品稳定性和组合料稳定性差等弊端。因此需要制造一种高活性、高稳定性的含溴阻燃聚醚多元醇。
发明内容
本发明的目的是提供一种含溴阻燃聚醚多元醇及其制备方法。
为了达到上述目的,本发明提供了一种含溴阻燃聚醚多元醇的制备方法,其特征在于,采用含溴化合物作为起始剂,在催化剂作用下,加入环氧丙烷,控制温度进行聚合反应,制得聚醚多元醇A;在聚醚多元醇A中加入小分子醛和二乙醇胺进行曼尼西反应,反应温度为60~80℃,脱水后得到含溴阻燃聚醚多元醇。
优选地,所述的起始剂含溴化合物为二溴新戊二醇、四溴双酚A和四溴双酚F中的任一种。
优选地,所述的环氧丙烷的加入量与含溴化合物的重量比为(2~5):1。
优选地,所述的催化剂为三乙胺、双金属氰化物络合催化剂和氢氧化钾中的任一种,催化剂加入量为含溴化合物和环氧丙烷总重量的0.1~0.5%。
优选地,所述聚合反应的温度为90~130℃。
优选地,所述的小分子醛为甲醛、乙醛和三聚甲醛中之任一种。
优选地,所述的曼尼西反应中聚醚多元醇A、小分子醛、二乙醇胺的摩尔比为1:(1~2):(1~2)。
优选地,上述制备方法具体包括以下步骤:
步骤1):将起始剂含溴化合物加入到反应釜中,升温至90~110℃,抽真空,脱水2h;加入后催化剂,控制温度90~130℃,加入环氧丙烷进行聚合反应,加完后继续反应3h,降温得到聚醚多元醇A;
步骤2):将聚醚多元醇A、小分子醛和二乙醇胺按比例加入到反应釜中,升温至60℃,反应2h,然后提高温度至80℃,再反应2h;在80~100℃条件下抽真空脱水和未反应单体,降温即得到含溴阻燃聚醚多元醇。
本发明还提供了上述方法制备的含溴阻燃聚醚多元醇。
本发明和已有技术相比,其技术进步是显著的。本发明制备的含溴聚醚多元醇具有官能度高、反应活性高,阻燃性及稳定性好等优点,采用该聚醚多元醇制备的硬质聚氨酯泡沫塑料具有优异的阻燃性能和力学性能。
具体实施方式
下面结合具体实施例,进一步阐述本发明。应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解,在阅读了本发明讲授的内容之后,本领域技术人员可以对本发明作各种改动或修改,这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例1-4所采用的各种原料均为市售的常用原料。采用实施例1-4制备的硬质聚氨酯泡沫塑料的氧指数测定参照GB/T2406-2009标准进行,采用HC900-2型氧指数仪,南京上元分析仪器有限公司;硬质聚氨酯泡沫塑料的压缩强度按照GB/T8813-2008标准测试,测定所用仪器为SUN500型万能电子试验机,意大利GALDABINI公司。
实施例1
本实施例提供了一种含溴阻燃聚醚多元醇的制备方法,具体步骤如下:
(1)称取二溴新戊二醇26.2g加入到高压反应釜中,升温至90℃,抽真空至-0.1MPa,脱水2h;加入催化剂三乙胺0.8g,控制温度130℃,加入环氧丙烷131g进行反应,加完后继续反应3h,降温,得到聚醚多元醇A;
(2)称取聚醚多元醇A 157g,加入甲醛水溶液(37%)8.1g和二乙醇胺10.5g,升温至60℃,反应2h,后提高温度至80℃,再反应2h,在80℃抽真空脱水及未反应单体,降温放料,得到含溴阻燃聚醚多元醇。
实施例2
本实施例提供了一种含溴阻燃聚醚多元醇的制备方法,具体步骤如下:
(1)称取四溴双酚A54.4g加入到高压反应釜中,升温至110℃,抽真空至-0.1MPa,脱水2h;加入催化剂双金属氰化物络合催化剂0.16g,控制温度90℃,加入环氧丙烷108.8g进行反应,加完后继续反应3h,降温,得到聚醚多元醇A;
(2)称取聚醚多元醇A163g,加入乙醛水溶液(40%)22g和二乙醇胺21g,升温至60℃,反应2h,后提高温度至80℃,再反应2h,在100℃抽真空脱水及未反应单体,降温放料,得到含溴阻燃聚醚多元醇。
实施例3
本实施例提供了一种含溴阻燃聚醚多元醇的制备方法,具体步骤如下:
(1)称取四溴双酚F 51.6g加入到高压反应釜中,升温至100℃,抽真空至-0.1MPa,脱水2h;加入催化剂氢氧化钾0.69g,控制温度130℃,加入环氧丙烷180.6g进行反应,加完后继续反应3h,降温,得到聚醚多元醇A;
(2)称取聚醚多元醇A232g,加入三聚甲醛13.5g和二乙醇胺15.75g,升温至60℃,反应2h,后提高温度至80℃,再反应2h,在90℃抽真空脱水及未反应单体,降温放料,得到含溴阻燃聚醚多元醇。
实施例4
本实施例提供了一种含溴阻燃聚醚多元醇的制备方法,具体步骤如下:
(1)称取四溴双酚A 54.4g加入到高压反应釜中,升温至100℃,抽真空至-0.1MPa,脱水2h;加入催化剂三乙胺1.2g,控制温度110℃,加入环氧丙烷190.4g进行反应,加完后继续反应3h,降温,得到聚醚多元醇A;
(2)称取聚醚多元醇A 245g,加入甲醛水溶液(37%)12.2g和二乙醇胺15.75g,升温至60℃,反应2h,后提高温度至80℃,再反应2h,在100℃抽真空脱水及未反应单体,降温放料,得到含溴阻燃聚醚多元醇。
将实施例1-4所制得的含溴阻燃聚醚多元醇为原料制备硬质聚氨酯泡沫塑料,对其抗压强度和氧指数进行了测定。聚氨酯泡沫塑料的制备方法如下:
1)A组分:按重量份数计,称取含溴阻燃聚醚多元醇60份,发泡剂一氟二氯乙烷20份,磷酸三(1-氯-乙丙基)酯(TCPP)16份,有机硅泡沫稳定剂AK-8803 2份,催化剂DMP-30 1份,催化剂辛酸亚锡1份;
2)B组分:多亚甲基多苯基异氰酸酯(PAPI)。
3)将A组分与B组分以重量比1:1的比例混合后,进行发泡,然后经80℃熟化,即得硬质聚氨酯泡沫塑料样品。
将硬质聚氨酯泡沫塑料样品进行相关性能测试,试验结果如表1所示。
表1
材料性能 | 实施例1 | 实施例2 | 实施例3 | 实施例4 |
压缩强度/MPa | 0.16 | 0.28 | 0.21 | 0.18 |
氧指数/% | 27 | 31 | 28 | 30 |
综上所述,采用本发明含溴阻燃聚醚多元醇制备的硬质聚氨酯泡沫塑料氧指数为27-31,压缩强度为0.16-0.28MPa,由此表明,由该聚醚多元醇制备的聚氨酯硬质泡沫塑料具有优异的阻燃性能和力学强度。
以上所述仅是本发明的实施方式的举例,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明技术原理的前提下,还可以做出若干改进,这些改进也应视为本发明的保护范围。
Claims (3)
1.一种含溴阻燃聚醚多元醇的制备方法,其特征在于,采用含溴化合物作为起始剂,在催化剂作用下,加入环氧丙烷,控制温度进行聚合反应,制得聚醚多元醇A;在聚醚多元醇A中加入小分子醛和二乙醇胺进行曼尼西反应,反应温度为60~80℃,脱水后得到含溴阻燃聚醚多元醇;
所述的起始剂含溴化合物为二溴新戊二醇、四溴双酚A和四溴双酚F中的任一种;
所述的环氧丙烷的加入量与含溴化合物的重量比为(2~5):1;
所述的催化剂为三乙胺、双金属氰化物络合催化剂中的任一种,催化剂加入量为含溴化合物和环氧丙烷总重量的0.1~0.5%;
所述聚合反应的温度为90~130℃;
所述的小分子醛为甲醛、乙醛和三聚甲醛中的任一种;
所述的曼尼西反应中聚醚多元醇A、小分子醛、二乙醇胺的摩尔比为1:(1~2):(1~2)。
2.如权利要求1所述的含溴阻燃聚醚多元醇的制备方法,其特征在于,所述方法具体包括以下步骤:
步骤1):将起始剂含溴化合物加入到反应釜中,升温至90~110℃,抽真空,脱水2h;加入催化剂,控制温度90~130℃,加入环氧丙烷进行聚合反应,加完后继续反应3h,降温得到聚醚多元醇A;
步骤2):将聚醚多元醇A、小分子醛和二乙醇胺按比例加入到反应釜中,升温至60℃,反应2h,然后提高温度至80℃,再反应2h;在80~100℃条件下抽真空脱水和未反应单体,降温即得到含溴阻燃聚醚多元醇。
3.权利要求1-2任一项所述方法制备的含溴阻燃聚醚多元醇。
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JPS5832625A (ja) * | 1982-07-23 | 1983-02-25 | Asahi Glass Co Ltd | 硬質ポリウレタンフオ−ムの製造方法 |
CN102803342A (zh) * | 2009-06-16 | 2012-11-28 | 旭硝子株式会社 | 聚醚多元醇的制造方法及采用其的硬质发泡合成树脂的制造方法 |
CN103539932A (zh) * | 2013-09-11 | 2014-01-29 | 江苏雅克科技股份有限公司 | 一种具有永久阻燃效果的反应型曼尼希聚醚多元醇的制备方法和用途 |
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