CN113150230B - 一种保温隔热型聚氨酯塑料及其制备方法 - Google Patents
一种保温隔热型聚氨酯塑料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种保温隔热型聚氨酯塑料及其制备方法。聚氨酯塑料包括如下重量份的原料,聚醚多元醇60~75份、扩链剂10~15份、泡沫稳定剂2~5份、催化剂1~3份、发泡剂15~20份、水1~3份、抗氧剂0.1~0.3份。其中,聚醚多元醇为棕榈油多元醇与高EO含量多元醇的复合物,棕榈油多元醇与高EO含量多元醇的质量比为2~4:1。扩链剂主要包括3,4‑二氨基苯乙酸、18‑冠‑6、极性溶剂。本发明制备得到的聚氨酯塑料具有良好的保温性能、隔热性能、抗压缩强度;可广泛应用到冰箱、太阳能、热水器、建筑、管道、集装箱等领域。
Description
技术领域
本发明涉及高分子材料技术领域,具体为一种保温隔热型聚氨酯塑料及其制备方法。
背景技术
目前,国内市场上流通的保温隔热材料主要分为有机泡沫保温隔热材料和无机泡沫保温隔热材料。有机泡沫保温隔热材料主要包括酚醛泡沫、聚氨酯塑料、聚苯乙烯等为主的有机泡沫保温隔热材料;无机泡沫保温隔热材料主要包括泡沫混凝土、岩面、玻璃棉、海泡石棉、珍珠岩、岩棉为主的无机泡沫保温隔热材料。
无机泡沫保温隔热材料大多为不可燃材料,安全性能高,但其保温效果较差、密度大、吸水率高、施工不便等缺点。而有机泡沫保温隔热材料具有质量轻、密度小、吸水率低、导热系数低、保温隔热效果良好的优点,因此得到广泛应用;聚氨酯塑料更是由于其优异的保温性能,备受市场的关注。
聚氨酯塑料也称为聚氨酯泡沫塑料,是由羟基化合物和异氰酸酯聚合形成聚氨酯预聚体,聚氨酯预聚体再经发泡剂发泡得到。聚氨酯塑料具有良好的保温隔热性,同时还具备优越的加工性、化学稳定性好、耐许多溶剂和油类、耐磨性等,因此广泛应用于冰箱、太阳能、热水器等家用电器、建筑、管道、集装箱等领域。
现有公开专利中,多使用聚酯多元醇来制备聚氨酯塑料;普通聚酯多元醇中苯环含量低,对发泡后的泡沫抗压缩强度提升效果不大,耐热性能达不到预期;普通聚酯多元醇的粘度相对较低,因此导致泡沫的脱模性能差、发泡初期容易造成泡沫破裂,降低泡沫强度和泡沫制品的表观质量。因此,需要寻找更优的聚酯多元醇组合或聚醚多元醇组合,用于提升聚氨酯泡沫塑料的整体性能。
发明内容
本发明的目的在于提供一种保温隔热型聚氨酯塑料及其制备方法,以解决上述背景技术中提出的问题。
为了解决上述技术问题,本发明提供如下技术方案:一种保温隔热型聚氨酯塑料,所述聚氨酯塑料包括如下重量份的原料,聚醚多元醇60~75份、扩链剂10~15份、泡沫稳定剂2~5份、催化剂1~3份、发泡剂15~20份、水1~3份、抗氧剂0.1~0.3份。
进一步的,所述聚醚多元醇为棕榈油多元醇与高EO含量多元醇的复合物;所述棕榈油多元醇与高EO含量多元醇的质量比为2~4:1。
进一步的,所述扩链剂主要包括3,4-二氨基苯乙酸、18-冠-6、极性溶剂。其中极性溶剂可以为乙醇、甲醇、石油醚、己烷、环己烷、甲苯、二甲苯、丙酮、二氯甲烷中的任意一种。
进一步的,所述高EO含量多元醇中E0的含量为73~75%;所述高EO含量多元醇羟值为40~44mg KOH/g。
进一步的,所述棕榈油多元醇羟值为380~440mg KOH/g,粘度为5000~8000mPa·s(25℃)。
进一步的,所述泡沫稳定剂为泡沫稳定剂AK8801、泡沫稳定剂AK8805、泡沫稳定剂B8870、泡沫稳定剂L6950中的任意一种或多种;
所述催化剂为二月桂酸二丁基锡、辛酸亚锡、三亚乙基二胺中的任意一种;
所述发泡剂为环戊烷、正戊烷、异戊烷、己烷中的任意一种;
所述抗氧剂为受阻酚类抗氧剂、亚磷酸酯类抗氧剂中的一种或两种组合。
一种保温隔热型聚氨酯塑料的制备方法,包括以下步骤:
(1)将18-冠-6溶于极性溶剂中,加入3,4-二氨基苯乙酸,搅拌均匀,得到扩链剂;
(2)混配得到聚醚多元醇,加入异氰酸酯、催化剂,升温反应,反应完成后,滴加扩链剂,滴加完毕后,反应得到聚氨酯预聚体;
(3)将聚氨酯预聚体与泡沫稳定剂、抗氧剂、水、催化剂混合,搅拌均匀,加入发泡剂,搅拌,倒入发泡模具中,发泡,熟化,制得聚氨酯塑料。
进一步的,一种保温隔热型聚氨酯塑料的制备方法,包括以下步骤;
(1)将18-冠-6溶于极性溶剂中,加入3,4-二氨基苯乙酸,搅拌均匀,得到扩链剂;
(2)取棕榈油多元醇与高EO含量多元醇,以质量比为2~4:1混合,搅拌均匀,得到聚醚多元醇,降温至20~25℃,加入异氰酸酯、催化剂,氮封保护条件下,升温至80~90℃,反应1~2h,降温至60~70℃;滴加步骤(1)制得的扩链剂,滴加完毕后,氮封保护条件下,反应2~3h,旋蒸去除极性溶剂,得到聚氨酯预聚体;
(3)将步骤(2)制得的聚氨酯预聚体与泡沫稳定剂、抗氧剂、水、催化剂混合,搅拌均匀,加入发泡剂,搅拌7~10s,搅拌速度为1000~1200r/min,倒入发泡模具中,发泡,熟化,制得聚氨酯塑料。
进一步的,所述棕榈油多元醇的制备方法如下:
将棕榈油、甘油、白砂糖混合,升温至95~105℃,氮封条件下,加入二甲胺、固体氢氧化钾,搅拌10~15min;滴加环氧丙烷,反应10~12h,升温至115~125℃,保温老化0.5~1h,真空脱水,酸洗,静制,得到棕榈油多元醇。
进一步的,所述高EO含量多元醇的制备方法如下:
将甘油、固体氢氧化钾混合,氮封条件下,升温至115~125℃,滴加环氧丙烷和环氧乙烷EO混合物,反应10~12h,保温老化0.5~1h,降温至110~115℃;滴加环氧乙烷EO,反应4~6h,真空脱水,保温老化0.5~1h,真空脱水,酸洗,静制,得到高EO含量多元醇。
与现有技术相比,本发明的有益效果:
本发明提供了一种聚氨酯塑料的制备方法,选择棕榈油多元醇与高EO含量多元醇以2~4:1的质量比混合得到的聚醚多元醇,其中棕榈油多元醇,是以棕榈油、少量的白砂糖和甘油为起始剂,与环氧丙烷聚合形成;白砂糖分子含有羟基,可在多元醇分子链上引入大量的羟基,制备得到的多元醇官能度高、羟值高,羟值含量高可促进多元醇与异氰酸酯的充分反应,且大量的羟基可提高其他助剂在反应体系中的相容性;生产分布均匀细密的泡孔,同时因白砂糖和棕榈油为可再生资源,从而减少了石油资源的消耗。
但由于棕榈油多元醇的粘度较高,在发泡初期会因泡孔壁的弹性较强,产生闭孔,连续闭孔会导致泡孔收缩;为解决这一问题,本发明添加了高EO含量多元醇,该多元醇粘度较低,可适当中和聚醚多元醇混合物的粘度,减少泡孔收缩;高EO含量多元醇,其EO含量高达73~75%,伯羟基含量高故反应活性较高,与异氰酸酯的反应速度快,短时间内热量聚集,使发泡充分,泡孔表层和芯部密度接近;从而弥补了棕榈油聚醚因粘度大而导致的闭孔现象;另外,由于高EO含量多元醇不饱和度低、分子质量分布窄,带来的副反应少,发泡得到的聚氨酯塑料绵密度高、均匀性好,隔热效果良好。
尽管棕榈油多元醇和高EO含量多元醇均从不同方面提高了,多元醇与异氰酸酯的反应活性和反应程度,但体系中依然会存在少量未参与反应的异氰酸酯,此时再加入扩链剂,扩链剂中3,4-二氨基苯乙酸分子结构中含有两个活性胺基,胺基可快速与异氰酸根反应,清除少量未参与反应的异氰酸酯;3,4-二氨基苯乙酸与异氰酸酯反应后,裸露出一个羧基,提高其与反应体系的相容性;另外,3,4-二氨基苯乙酸分子结构中含有刚性的苯环结构,与二乙醇胺、三乙醇胺的线型结构相比,不但不会降低聚氨酯塑料的强度和耐热性,反而会提高聚氨酯塑料的强度和耐热性。
由于聚醚多元醇中通常会含有钾离子,尤其是棕榈油多元醇由于粘度较大,后处理难度大,导致其产品中钾离子含量较高,在10PPm左右;钾离子的存在会导致聚醚提前凝胶,发泡过程中易产生结块、塌泡的现象;为了解决这一问题,在封端过程中,扩链剂内的组份18-冠-6可与钾离子配位形成稳定的环状配合物,一方面去除了聚醚多元醇中的钾离子,另一方面稳定的环状结构,给体系带来刚性结构,增强聚氨酯塑料的强度和耐热性。
本发明制备的聚氨酯塑料具有良好的保温性能、隔热性能、抗压缩强度;可应用到冰箱、太阳能、热水器、建筑、管道、集装箱等领域。
具体实施方式
下面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做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
一种保温隔热型聚氨酯塑料,包括如下重量份的原料,聚醚多元醇60份、扩链剂10份、泡沫稳定剂2份、催化剂1份、发泡剂15份、水1份、抗氧剂0.1份。
聚醚多元醇为棕榈油多元醇与高EO含量多元醇的复合物;棕榈油多元醇与高EO含量多元醇的质量比为2:1。
高EO含量多元醇中E0的含量为73%;所述高EO含量多元醇羟值为40mg KOH/g。
棕榈油多元醇羟值为380mg KOH/g,粘度为5050mPa·s(25℃)。
泡沫稳定剂为泡沫稳定剂AK8801、催化剂为二月桂酸二丁基锡、发泡剂为环戊烷、抗氧剂为受阻酚类抗氧剂。
一种保温隔热型聚氨酯塑料的制备方法,包括以下步骤;
(1)将18-冠-6溶于极性溶剂中,加入3,4-二氨基苯乙酸,搅拌均匀,得到扩链剂;
(2)取棕榈油多元醇与高EO含量多元醇,以质量比为2:1混合,搅拌均匀,得到聚醚多元醇,降温至20℃,加入异氰酸酯、催化剂,氮封保护条件下,升温至80℃,反应1h,降温至60℃;滴加步骤(1)制得的扩链剂,滴加完毕后,氮封保护条件下,反应2h,旋蒸去除极性溶剂,得到聚氨酯预聚体;
(3)将步骤(2)制得的聚氨酯预聚体与泡沫稳定剂、抗氧剂、水、催化剂混合,搅拌均匀,加入发泡剂,搅拌7s,搅拌速度为1000r/min,倒入发泡模具中,发泡,熟化,制得聚氨酯塑料。
棕榈油多元醇的制备方法如下:
将棕榈油、甘油、白砂糖混合,升温至95℃,氮封条件下,加入二甲胺、固体氢氧化钾,搅拌10min;滴加环氧丙烷,反应10h,升温至115℃,保温老化0.5h,真空脱水,酸洗,静制,得到棕榈油多元醇。
高EO含量多元醇的制备方法如下:
将甘油、固体氢氧化钾混合,氮封条件下,升温至115℃,滴加环氧丙烷和环氧乙烷EO混合物,反应10h,保温老化0.5h,降温至110℃;滴加环氧乙烷EO,反应4h,真空脱水,保温老化0.5h,真空脱水,酸洗,静制,得到高EO含量多元醇。
实施例2
一种保温隔热型聚氨酯塑料,包括如下重量份的原料,聚醚多元醇68份、扩链剂12份、泡沫稳定剂3份、催化剂2份、发泡剂16份、水1.5份、抗氧剂0.2份。
聚醚多元醇为棕榈油多元醇与高EO含量多元醇的复合物;棕榈油多元醇与高EO含量多元醇的质量比为3:1。
高EO含量多元醇中E0的含量为74%;所述高EO含量多元醇羟值为42mg KOH/g。
棕榈油多元醇羟值为400mg KOH/g,粘度为6700mPa·s(25℃)。
泡沫稳定剂为泡沫稳定剂AK8805、辛酸亚锡、发泡剂为正戊烷、抗氧剂为亚磷酸酯类抗氧剂。
一种保温隔热型聚氨酯塑料的制备方法,包括以下步骤;
(1)将18-冠-6溶于极性溶剂中,加入3,4-二氨基苯乙酸,搅拌均匀,得到扩链剂;
(2)取棕榈油多元醇与高EO含量多元醇,以质量比为3:1混合,搅拌均匀,得到聚醚多元醇,降温至22℃,加入异氰酸酯、催化剂,氮封保护条件下,升温至85℃,反应1.5h,降温至64℃;滴加步骤(1)制得的扩链剂,滴加完毕后,氮封保护条件下,反应2.5h,旋蒸去除极性溶剂,得到聚氨酯预聚体;
(3)将步骤(2)制得的聚氨酯预聚体与泡沫稳定剂、抗氧剂、水、催化剂混合,搅拌均匀,加入发泡剂,搅拌8s,搅拌速度为1100r/min,倒入发泡模具中,发泡,熟化,制得聚氨酯塑料。
棕榈油多元醇的制备方法如下:
将棕榈油、甘油、白砂糖混合,升温至100℃,氮封条件下,加入二甲胺、固体氢氧化钾,搅拌12min;滴加环氧丙烷,反应11h,升温至118℃,保温老化0.7h,真空脱水,酸洗,静制,得到棕榈油多元醇。
高EO含量多元醇的制备方法如下:
将甘油、固体氢氧化钾混合,氮封条件下,升温至118℃,滴加环氧丙烷和环氧乙烷EO混合物,反应11h,保温老化0.6h,降温至112℃;滴加环氧乙烷EO,反应5h,真空脱水,保温老化0.7h,真空脱水,酸洗,静制,得到高EO含量多元醇。
实施例3
一种保温隔热型聚氨酯塑料,包括如下重量份的原料,聚醚多元醇75份、扩链剂15份、泡沫稳定剂5份、催化剂3份、发泡剂20份、水3份、抗氧剂0.3份。
聚醚多元醇为棕榈油多元醇与高EO含量多元醇的复合物;棕榈油多元醇与高EO含量多元醇的质量比为4:1。
高EO含量多元醇中E0的含量为75%;所述高EO含量多元醇羟值为44mg KOH/g。
棕榈油多元醇羟值为440mg KOH/g,粘度为8000mPa·s(25℃)。
泡沫稳定剂为泡沫稳定剂B8870、催化剂为三亚乙基二胺、发泡剂为异戊烷、抗氧剂为受阻酚类抗氧剂与亚磷酸酯类抗氧剂的组合物。
一种保温隔热型聚氨酯塑料的制备方法,包括以下步骤;
(1)将18-冠-6溶于极性溶剂中,加入3,4-二氨基苯乙酸,搅拌均匀,得到扩链剂;
(2)取棕榈油多元醇与高EO含量多元醇,以质量比为4:1混合,搅拌均匀,得到聚醚多元醇,降温至25℃,加入异氰酸酯、催化剂,氮封保护条件下,升温至90℃,反应2h,降温至70℃;滴加步骤(1)制得的扩链剂,滴加完毕后,氮封保护条件下,反应3h,旋蒸去除极性溶剂,得到聚氨酯预聚体;
(3)将步骤(2)制得的聚氨酯预聚体与泡沫稳定剂、抗氧剂、水、催化剂混合,搅拌均匀,加入发泡剂,搅拌10s,搅拌速度为1200r/min,倒入发泡模具中,发泡,熟化,制得聚氨酯塑料。
棕榈油多元醇的制备方法如下:
将棕榈油、甘油、白砂糖混合,升温至105℃,氮封条件下,加入二甲胺、固体氢氧化钾,搅拌15min;滴加环氧丙烷,反应12h,升温至125℃,保温老化1h,真空脱水,酸洗,静制,得到棕榈油多元醇。
高EO含量多元醇的制备方法如下:
将甘油、固体氢氧化钾混合,氮封条件下,升温至125℃,滴加环氧丙烷和环氧乙烷EO混合物,反应12h,保温老化1h,降温至115℃;滴加环氧乙烷EO,反应6h,真空脱水,保温老化1h,真空脱水,酸洗,静制,得到高EO含量多元醇。
对比例1
棕榈油多元醇与高EO含量多元醇的质量比为1:3,其余内容与实施例2相同。
对比例2
聚醚多元醇仅为棕榈油多元醇,其余内容与实施例2相同。
对比例3
聚醚多元醇仅为高EO含量多元醇,其余内容与实施例2相同。
对比例4
扩链剂为二乙醇胺,其余内容与实施例2相同。
实验例
取实施例1~3、对比例1~3制备得到的聚氨酯塑料,检测其导热系数和压缩强度,检测结果见表1:
导热系数10℃,mW/m.K | 平均压缩强度,KPa | 泡沫芯密度,g/cm3 | |
实施例1 | 18.1 | 213.5 | 34.0 |
实施例2 | 17.8 | 213.9 | 34.0 |
实施例3 | 18.2 | 213.6 | 34.1 |
对比例1 | 18.2 | 211.7 | 34.0 |
对比例2 | 18.5 | 205.6 | 34.6 |
对比例3 | 18.7 | 202.3 | 33.8 |
对比例4 | 18.4 | 201.5 | 34.1 |
表1
由表1数据知道,实施例1~3制备得到的聚氨酯塑料的导热系数低,压缩强度高的特点;对比例1中,棕榈油多元醇与高EO含量多元醇的质量比为1:3,与实施例2相比低粘度的高EO含量多元醇含量较高,发泡初期由于部分泡孔破裂,导致塑料导热系数和压缩强度降低;对比例2和对比例3中单独使用棕榈油多元醇与高EO含量多元醇,制备的聚氨酯塑料导热系数和压缩强度均比实施例2差,对比例4中使用二乙醇胺代替本方案中的扩链剂,由于二乙醇胺线型结构,而实施例2中扩链剂含有刚性苯环结构,因此导致对比例4聚氨酯塑料的压缩强度比实施例2要差。
最后应说明的是:以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (7)
1.一种保温隔热型聚氨酯塑料,其特征在于;所述聚氨酯塑料包括如下重量份的原料,聚醚多元醇60~75份、扩链剂10~15份、泡沫稳定剂2~5份、催化剂1~3份、发泡剂15~20份、水1~3份、抗氧剂0.1~0.3份;
所述的一种保温隔热型聚氨酯塑料,其特征在于:所述聚醚多元醇为棕榈油多元醇与高EO含量多元醇的复合物;所述高EO含量多元醇中EO的含量为73~75%;所述棕榈油多元醇与高EO含量多元醇的质量比为2~4:1;
所述扩链剂主要包括3,4-二氨基苯乙酸、18-冠-6、极性溶剂;
所述泡沫稳定剂为泡沫稳定剂AK8801、泡沫稳定剂AK8805、泡沫稳定剂B8870、泡沫稳定剂L6950中的任意一种或多种;
所述催化剂为二月桂酸二丁基锡、辛酸亚锡、三亚乙基二胺中的任意一种;
所述发泡剂为环戊烷、正戊烷、异戊烷、己烷中的任意一种;
所述抗氧剂为受阻酚类抗氧剂、亚磷酸酯类抗氧剂中的一种或两种组合。
2.根据权利要求1所述的一种保温隔热型聚氨酯塑料,其特征在于:所述高EO含量多元醇羟值为40~44mg KOH/g。
3.根据权利要求1所述的一种保温隔热型聚氨酯塑料,其特征在于:所述棕榈油多元醇羟值为380~440mg KOH/g,粘度为5000~8000mPa·s。
4.一种保温隔热型聚氨酯塑料的制备方法,其特征在于:包括以下步骤:
(1)将18-冠-6溶于极性溶剂中,加入3,4-二氨基苯乙酸,搅拌均匀,得到扩链剂;
(2)混配得到聚醚多元醇,加入异氰酸酯、催化剂,升温反应,反应完成后,滴加扩链剂,滴加完毕后,反应得到聚氨酯预聚体;
(3)将聚氨酯预聚体与泡沫稳定剂、抗氧剂、水、催化剂混合,搅拌均匀,加入发泡剂,搅拌,倒入发泡模具中,发泡,熟化,制得聚氨酯塑料。
5.根据权利要求4所述的一种保温隔热型聚氨酯塑料的制备方法,其特征在于:包括以下步骤;
(1)将18-冠-6溶于极性溶剂中,加入3,4-二氨基苯乙酸,搅拌均匀,得到扩链剂;
(2)取棕榈油多元醇与EO的含量为73~75%的高EO含量多元醇,以质量比为2~4:1混合,搅拌均匀,得到聚醚多元醇,降温至20~25℃,加入异氰酸酯、催化剂,氮封保护条件下,升温至80~90℃,反应1~2h,降温至60~70℃;滴加步骤(1)制得的扩链剂,滴加完毕后,氮封保护条件下,反应2~3h,旋蒸去除极性溶剂,得到聚氨酯预聚体;
(3)将步骤(2)制得的聚氨酯预聚体与泡沫稳定剂、抗氧剂、水、催化剂混合,搅拌均匀,加入发泡剂,搅拌7~10s,搅拌速度为1000~1200r/min,倒入发泡模具中,发泡,熟化,制得聚氨酯塑料。
6.根据权利要求5所述的一种保温隔热型聚氨酯塑料的制备方法,其特征在于:所述棕榈油多元醇的制备方法如下:
将棕榈油、甘油、白砂糖混合,升温至95~105℃,氮封条件下,加入二甲胺、固体氢氧化钾,搅拌10~15min;滴加环氧丙烷,反应10~12h,升温至115~125℃,保温老化0.5~1h,真空脱水,酸洗,静制,得到棕榈油多元醇。
7.根据权利要求5所述的一种保温隔热型聚氨酯塑料的制备方法,其特征在于:所述高EO含量多元醇的制备方法如下:
将甘油、固体氢氧化钾混合,氮封条件下,升温至115~125℃,滴加环氧丙烷和环氧乙烷EO混合物,反应10~12h,保温老化0.5~1h,降温至110~115℃;滴加环氧乙烷EO,反应4~6h,真空脱水,保温老化0.5~1h,真空脱水,酸洗,静制,得到高EO含量多元醇。
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