CN110862526B - 一种高活性阻燃聚醚多元醇的制备方法 - Google Patents
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Abstract
本发明公开了一种高活性阻燃聚醚多元醇的制备方法,其特征在于,采用三羟甲基氧化磷和三羟乙基异氰脲酸酯作为双起始剂,在催化剂作用下,依次交替加入环氧丙烷和环氧乙烷,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℃,脱水后得到高活性阻燃聚醚多元醇。本发明制备的聚醚多元醇具有官能度高、反应活性高,具有自催化活性等优势,用该聚醚多元醇作为阻燃剂和交联剂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。
Description
技术领域
本发明涉及一种高活性阻燃聚醚多元醇的制备方法,属于高分子合成技术领域。
背景技术
聚氨酯泡沫体系在建筑及工业领域有广阔的应用,但是存在阻燃性能差、易燃烧的缺点,聚氨酯泡沫体系的阻燃和防火问题一直是现在的研究热点。聚醚多元醇是构成聚氨酯材料的主要成分,也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。添加型阻燃聚醚多元醇通过向聚醚多元醇中添加无机或有机阻燃剂达到阻燃目的。但添加的这些阻燃剂通常存在易迁移、阻燃效果不持久和破坏泡沫物理性能等缺点。反应型阻燃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CN108192089A公开了一种制备高官能度阻燃聚醚多元醇的方法。采用羟甲基三聚氰胺与二元酸(或其酸酐)反应,生成多羟基酯类成分;多羟基酯类成分再与环氧烷烃反应,得高官能度阻燃聚醚多元醇,该发明的阻燃聚醚多元醇具有官能度高、含氮量高、热稳定性好的特点。
专利CN 107880261 A公开了一种采用高含氮量的羟基化合物PNR1000和含磷且化学结构稳定的THPO作为起始剂,将P、N两种阻燃元素有机结合,制备的聚醚多元醇具备良好的阻燃性;是一种适用于软泡领域的高分子量、浅黄色透明液体,阻燃体系中不含卤素,绿色环保;该制备方法,反应时间短、转化效率高。
专利CN 109400866 A公开了一种阻燃型海绵用聚醚多元醇及其制备方法,是以聚酯1000和三羟甲基氧化磷(THPO)为起始剂,使用改性双金属氰化络合物催化剂,与环氧丙烷和环氧乙烷开环聚合,制得阻燃型海绵用聚醚多元醇,该发明所述的阻燃型海绵用聚醚多元醇,原料简单易得,成本低,结构稳定,阻燃性良好。
目前阻燃聚醚的研究主要集中在环保型的磷氮阻燃聚醚的研究方面,大量研究证明,单一的含氮阻燃剂阻燃效果欠佳,单一的含磷阻燃剂一般稳定性欠佳,复合的磷、氮阻燃聚醚具有更好的阻燃效果和稳定性,因此目前的阻燃聚醚把稳定性和相容性研究放在十分重要的位置。
发明内容
本发明所要解决的技术问题是:现有含氮阻燃剂多为单一组份,其阻燃效果和稳定性欠佳。
为了解决上述技术问题,本发明提供了一种高活性阻燃聚醚多元醇的制备方法,其特征在于,采用三羟甲基氧化磷和三羟乙基异氰脲酸酯作为双起始剂,在催化剂作用下,依次交替加入环氧丙烷和环氧乙烷,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℃,脱水后得到高活性阻燃聚醚多元醇。
优选地,所述三羟甲基氧化磷与三羟乙基异氰脲酸酯的重量比为(1~5):1。
优选地,所述的催化剂为二乙胺、双金属氰化物络合催化剂和氢氧化钾中的任意一种,催化剂的加入量为双起始剂和环氧丙烷、环氧乙烷总重量的0.1~0.5%。
优选地,所述的环氧丙烷与环氧乙烷的重量比为50:(40~10),且两者的总加入量与双起始剂重量比为(2~5):1。
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、乙醛和三聚甲醛中的任意一种。
优选地,所述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,所述聚醚多元醇A的数均分子量为500~1000g/mol。
优选地,上述制备方法包括以下步骤:
步骤1):将双起始剂、催化剂加入到反应釜中,升温至90~110℃,抽真空,脱水2h;控制温度90~130℃,加入环氧丙烷和环氧乙烷进行聚合反应,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,降温即得高活性阻燃聚醚多元醇。
本发明制备的聚醚多元醇采用多官能度磷氮化合物作为双起始剂,其中含氮化合物三羟乙基异氰脲酸酯主要提高聚醚的高反应活性和刚性结构,含磷化合物主要用来提高聚醚的阻燃性,并且该化合物稳定不容易分解,所以合成出的阻燃聚醚具有官能度高、反应活性高,稳定性好,同时还有叔胺基团因此具有自催化活性等优势,用该聚醚多元醇作为阻燃剂和交联剂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。
具体实施方式
为使本发明更明显易懂,兹以优选实施例,作详细说明如下。
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
一种高活性阻燃聚醚多元醇的制备方法:(1)称取三羟甲基氧化磷10g和三羟乙基异氰脲酸酯10g,加入到高压反应釜中,升温至90℃,抽真空至-0.1MPa,脱水2h;加入催化剂二乙胺0.55g,控制温度130℃,依次交替加入环氧丙烷50g和环氧乙烷40g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A100g,加入甲醛水溶液8g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,得产品。
实施例2
一种高活性阻燃聚醚多元醇的制备方法:(1)称取三羟甲基氧化磷50g和三羟乙基异氰脲酸酯10g,催化剂氢氧化钾0.45g加入到高压反应釜中,升温至100℃,抽真空至-0.1MPa,脱水2h;控制温度110℃,依次交替加入环氧丙烷100g和环氧乙烷20g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 100g,加入甲醛水溶液32g和二乙醇胺42g,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,得产品。
实施例3
一种高活性阻燃聚醚多元醇的制备方法:(1)称取三羟甲基氧化磷30g和三羟乙基异氰脲酸酯10g,双金属氰化物络合催化剂0.20g加入到高压反应釜中,升温至110℃,抽真空至-0.1MPa,脱水2h;控制温度90℃,依次交替加入环氧丙烷94g和环氧乙烷46g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A100g,加入甲醛15g和二乙醇胺20g,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,得产品。
实施例4
一种高活性阻燃聚醚多元醇的制备方法:(1)称取三羟甲基氧化磷40g和三羟乙基异氰脲酸酯10g,加入到高压反应釜中,升温至90℃,抽真空至-0.1MPa,脱水2h;加入催化剂二乙胺0.8g,控制温度120℃,依次交替加入环氧丙烷120g和环氧乙烷30g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A100g,加入甲醛16g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,得产品。
将实施例1-4所制得的高活性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,称取高活性阻燃聚醚多元醇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-301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,按照异氰酸酯指数1.10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
由表1可见,采用本发明制备的一种高活性阻燃聚醚多元醇制备的硬质聚氨酯泡沫塑料氧指数为26-30,压缩强度为0.16-0.25MPa,由此表明,由于制备的多元醇具有三嗪环刚性结构和高磷含量的阻燃元素,制备的聚醚多元醇具有官能度高、反应活性高,具有自催化活性等优势,用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。
Claims (7)
1.一种高活性阻燃聚醚多元醇的制备方法,其特征在于,采用三羟甲基氧化磷和三羟乙基异氰脲酸酯作为双起始剂,在催化剂作用下,依次交替加入环氧丙烷和环氧乙烷,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℃,脱水后得到高活性阻燃聚醚多元醇;
所述三羟甲基氧化磷与三羟乙基异氰脲酸酯的重量比为(1~5):1;
所述的催化剂为二乙胺、双金属氰化物络合催化剂和氢氧化钾中的任意一种,催化剂的加入量为双起始剂和环氧丙烷、环氧乙烷总重量的0.1~0.5%。
2.如权利要求1所述的高活性阻燃聚醚多元醇的制备方法,其特征在于,所述的环氧丙烷与环氧乙烷的重量比为50:(40~10),且两者的总加入量与双起始剂重量比为(2~5):1。
3.如权利要求1所述的高活性阻燃聚醚多元醇的制备方法,其特征在于,所述聚合反应的温度为90~130℃。
4.如权利要求1所述的高活性阻燃聚醚多元醇的制备方法,其特征在于,所述的小分子醛为甲醛、乙醛和三聚甲醛中的任意一种。
5.如权利要求1所述的高活性阻燃聚醚多元醇的制备方法,其特征在于,所述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)。
6.如权利要求1所述的高活性阻燃聚醚多元醇的制备方法,其特征在于,所述聚醚多元醇A的数均分子量为500~1000g/mol。
7.如权利要求1所述的高活性阻燃聚醚多元醇的制备方法,其特征在于,包括以下步骤:
步骤1):将双起始剂、催化剂加入到反应釜中,升温至90~110℃,抽真空,脱水2h;控制温度90~130℃,加入环氧丙烷和环氧乙烷进行聚合反应,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,降温即得高活性阻燃聚醚多元醇。
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CN112679722B (zh) * | 2020-12-28 | 2023-03-07 | 山东一诺威新材料有限公司 | 全水阻燃体系用聚醚多元醇的制备方法 |
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