CN107226905A - 一种异山梨醇缩水甘油醚改性多元醇的方法及其应用 - Google Patents
一种异山梨醇缩水甘油醚改性多元醇的方法及其应用 Download PDFInfo
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Abstract
本发明公开了一种异山梨醇缩水甘油醚改性商用多元醇的方法及其在合成聚氨酯泡沫中的应用。将异山梨醇缩水甘油醚与商品聚合多元醇进行接枝反应,将改性后的混合多元醇用于制备聚氨酯泡沫。异山梨醇缩水甘油醚改性后的多元醇制备的聚氨酯泡沫比未改性的多元醇制备的聚氨酯泡沫抗压强度提高8‑31%,密度降低5‑9%,尺寸稳定性提高32‑60%。
Description
技术领域
本发明属于聚氨酯发泡材料合成领域,涉及改性多元醇的合成及其在合成聚氨酯泡沫材料中的应用,具体涉及利用异山梨醇缩水甘油醚改性多元醇的方法及其在聚氨酯泡沫中的应用。
背景技术
聚氨酯泡沫是一种以异氰酸酯和多元醇为主要原料,在发泡剂、催化剂等多种助剂的作用下发泡而成的由硬链段和软链段构成的嵌段共聚物。聚氨酯泡沫具有低导热性,低密度,高强度重量比和低透湿性等优点。其应用范围广泛,包括建筑外墙保温材料、家电保温材料、航空保温材料等。
聚氨酯泡沫的两大主要原料为异氰酸酯和多元醇。异氰酸酯使聚氨酯材料具有硬链段特征,多元醇是一种碳碳键或碳氧键为主链的大分子多元醇,具有较强的挠曲作用,成为聚合物的软链段。
目前的市售多元醇以聚醚多元醇为主,聚醚多元醇具有生产工艺简单、安全、成本低廉等优点,因此在聚氨酯泡沫领域应用非常广泛。随着社会生产的不断发展,对高强度、低密度聚氨酯泡沫的需求也不断增加,如何进一步降低聚氨酯泡沫的密度并提高强度,成为人们研究的重点。现有的改性技术大都通过添加无机材料来增强聚氨酯泡沫的强度,这种改性只能在一定程度上增强聚氨酯泡沫的强度,对密度的降低作用很小。例如,中国专利CN106188494A公开的“硬质聚氨酯外墙泡沫材料”,通过添加粉煤灰、硅藻土等无机材料来增强泡沫材料的强度。通过添加无机材料的方法来增强聚氨酯泡沫材料强度的应用范围受到了限制。
通过单体分子结构设计与可控合成的方法,改进聚氨酯合成材料的性质,增强聚氨酯泡沫材料的强度仍具有发展的空间。
发明内容
本发明需要解决的技术问题在于现有技术中,合成聚氨酯材料力学性能不佳,结构稳定性不强的问题。为了克服该问题,本发明改进了聚氨酯泡沫材料的合成原料,即采用异山梨醇缩水甘油醚对商用多元醇原料进行改性,利用改性后的多元醇混合物制备聚氨酯泡沫材料。
具体的,本发明的技术方案为:
一种改性多元醇的方法,其中,将异山梨醇缩水甘油醚与多元醇混合,在催化剂作用下进行反应改性,获得异山梨醇缩水甘油醚改性的多元醇混合物。
其中,异山梨醇缩水甘油醚聚合物结构式为:
或
本发明所述的方法,具体步骤为:
(1)将多元醇于110-130℃中真空干燥1-5h,除去体系中的水;
(2)向真空干燥后的体系中加入异山梨醇缩水甘油醚和催化剂,在65-95℃下反应3-8h;
其中,所述异山梨醇缩水甘油醚:催化剂:多元醇的摩尔比为1:0.002~0.01:0.5~20。
本发明所述的方法,其中,所述多元醇为聚醚多元醇或聚酯多元醇。聚醚多元醇是指含有醚键的多元醇,如4110等;聚酯多元醇是指含有酯键的多元醇,如3202等。
本发明所述的方法,其中,所述催化剂为氢氧化钾、氢氧化钠、醇纳、醇钾、乙酸钙、醋酸镁、氯化锡、氯化铝、五氯化锑、高氯酸、三氟乙酸、三氟甲硫酸中的一种或几种混合物。
本发明所述的改性的多元醇混合物在合成聚氨酯泡沫材料中的应用。即,利用异山梨醇改性的多元醇混合物与异氰酸酯、发泡剂、催化剂、稳泡剂混合反应,产生聚氨酯泡沫。
本发明的有益效果在于:
(1)通过异山梨醇缩水甘油醚改性多元醇制备获得的聚氨酯硬质泡沫与未改性的多元醇制备的聚氨酯硬质泡沫相比,抗压强度提高8-31%,密度降低5-9%。尺寸稳定性提高了32-60%。因此,本方法可提高聚氨酯泡沫的力学性能和结构稳定性。
(2)该方法所获得的聚氨酯泡沫材料具有不改变原生产工艺、价格适中、性能优异等优点。
(3)本发明可能的技术原理在于:异山梨醇缩水甘油醚是以异山梨醇为原料生产的一种高反应活性的化合物,将刚性结构的异山梨醇引入到聚氨酯结构中,其特殊的分子结构应该可以从分子层次为聚氨酯材料提供优异的力学性能和结构稳定性。
具体实施方式
下面结合具体实例对本发明所述工艺及材料进行详细说明。
本发明对所制备的改性多元醇的羟值,按照国标GB/T12008.3-2009测定;本发明中的黏度使用上海方瑞仪器有限公司生产的NDJ-8S型粘度计测定。
实施例1
将50g市售多元醇4110,购自红宝丽集团股份有限公司,装入三口烧瓶中,于110℃真空干燥3h,将三口烧瓶放入65℃的油浴锅中,加入异山梨醇缩水甘油醚10g,氢氧化钾0.02g反应进行7h。反应结束后,最终得到多元醇的羟值为432.3mgKOH/g,黏度为6500mPa·s。
实施例2
将100g市售多元醇8635,购自红宝丽集团股份有限公司,装入三口烧瓶中,于130℃真空干燥1h,将三口烧瓶放入80℃的油浴锅中,加入异山梨醇缩水甘油醚50g,氢氧化钠0.15g反应进行4.5h。反应结束后,最终得到多元醇的羟值为442.6mgKOH/g,黏度为11530mPa·s。
实施例3
将80g市售多元醇6020,购自红宝丽集团股份有限公司,装入三口烧瓶中,于115℃真空干燥4h,将三口烧瓶放入95℃的油浴锅中,加入异山梨醇缩水甘油醚50g,乙醇钠0.11g反应进行3h。反应结束后,最终得到多元醇的羟值为433.5mgKOH/g,黏度为13100mPa·s。
实施例4
将70g市售多元醇9211,购自红宝丽集团股份有限公司,装入三口烧瓶中,于120℃真空干燥3.5h,将三口烧瓶放入70℃的油浴锅中,加入异山梨醇缩水甘油醚5g,乙醇钾0.09g反应进行6h。反应结束后,最终得到多元醇的羟值为458.6mgKOH/g,黏度为3020mPa·s。
实施例5
将150g市售多元醇4820,购自红宝丽集团股份有限公司,装入三口烧瓶中,于130℃真空干燥8h,将三口烧瓶放入80℃的油浴锅中,加入异山梨醇缩水甘油醚150g,乙酸钙1.06g反应进行8h。反应结束后,最终得到多元醇的羟值为444.6mgKOH/g,黏度为9100mPa·s。
实施例6
将60g市售多元醇3202,购自红宝丽集团股份有限公司,装入三口烧瓶中,于130℃真空干燥1h,将三口烧瓶放入90℃的油浴锅中,加入异山梨醇缩水甘油醚90g,醋酸镁0.315g反应进行5h。反应结束后,最终得到多元醇的羟值为380.4mgKOH/g,黏度为4500mPa·s。
实施例7
将80g市售多元醇3162,购自恒丰聚氨酯实业有限公司,装入三口烧瓶中,于115℃真空干燥5h,将三口烧瓶放入90℃的油浴锅中,加入异山梨醇缩水甘油醚6g,氯化锡0.106g反应进行3h。反应结束后,最终得到多元醇的羟值为502.8mgKOH/g,黏度为7800mPa·s。
实施例8
将110g市售多元醇380,购自恒丰聚氨酯实业有限公司,装入三口烧瓶中,于125℃真空干燥4h,将三口烧瓶放入70℃的油浴锅中,加入异山梨醇缩水甘油醚30g,氯化铝0.216g反应进行5h。反应结束后,最终得到多元醇的羟值为381.9mgKOH/g,黏度为10080mPa·s。
实施例9
将90g市售多元醇640,购自恒丰聚氨酯实业有限公司,装入三口烧瓶中,于125℃真空干燥2h,将三口烧瓶放入90℃的油浴锅中,加入异山梨醇缩水甘油醚15g,三氟乙酸0.221g反应进行4h。反应结束后,最终得到多元醇的羟值为459.8mgKOH/g,黏度为11000mPa·s。
实施例10
将130g市售多元醇835,购自恒丰聚氨酯实业有限公司,装入三口烧瓶中,于120℃真空干燥4h,将三口烧瓶放入80℃的油浴锅中,加入异山梨醇缩水甘油醚150g,三氟甲硫酸0.852g反应进行5h。反应结束后,最终得到多元醇的羟值为488.3mgKOH/g,黏度为7260mPa·s
实施例11
本发明对异山梨醇缩水甘油醚改性多元醇制备的聚氨酯硬质泡沫的测定方法如下:
根据GB/T6343-2009测定聚氨酯硬质泡沫的密度;
根据GB /8813-2008测定聚氨酯硬质泡沫的压缩强度,取发泡垂直方向截面为压缩面。
取上述实施例中制备的异山梨醇缩水甘油醚改性多元醇,与水、稳泡剂AK8818(江苏美思德)、三乙烯二胺、辛酸亚锡、异氰酸酯(万华化学)反应进行发泡,即可制备出聚氨酯硬质泡沫,垂直压缩强度较未改性的提高8-31%,材料密度较未改性的降低5-9%。尺寸稳定性提高32-60%。
Claims (5)
1.一种改性多元醇的方法,其特征在于,将异山梨醇缩水甘油醚与聚合多元醇混合,在催化剂作用下进行接枝反应改性,获得异山梨醇缩水甘油醚改性的多元醇混合物。
2.根据权利要求1所述的方法,方法具体步骤为:
(1)将多元醇于110-130℃中真空干燥1-5h,除去体系中的水;
(2)向真空干燥后的体系中加入异山梨醇缩水甘油醚和催化剂,在65-95℃下反应3-8h;
其特征在于,所述异山梨醇缩水甘油醚:催化剂:多元醇的摩尔比为1:0.002~0.01:0.5~20。
3.根据权利要求1所述的方法,其特征在于,所述多元醇为聚醚多元醇或聚酯多元醇。
4.根据权利要求1所述的方法,其特征在于,所述催化剂为氢氧化钾、氢氧化钠、醇纳、醇钾、乙酸钙、醋酸镁、氯化锡、氯化铝、五氯化锑、高氯酸、三氟乙酸、三氟甲硫酸中的一种或几种的混合物。
5.权利要求1所述的改性的多元醇混合物在合成聚氨酯泡沫材料中的应用。
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