CN111471170A - 一种环保聚氨酯全水组合料的制备工艺 - Google Patents

一种环保聚氨酯全水组合料的制备工艺 Download PDF

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CN111471170A
CN111471170A CN202010323229.4A CN202010323229A CN111471170A CN 111471170 A CN111471170 A CN 111471170A CN 202010323229 A CN202010323229 A CN 202010323229A CN 111471170 A CN111471170 A CN 111471170A
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林同起
李政
尚寿坤
柳祖刚
孙忠民
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Beijing Lanyuan Xinxing Technology Development Co ltd
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Abstract

本发明属于聚氨酯全水组合料技术领域，尤其本发明公开了一种环保聚氨酯全水组合料的制备工艺，包括以下步骤，S1，准备原料，由以下重量份的原料组成：蔗糖15‑25份、甘油5‑15份、甲基邻苯二胺4‑10份、小分子二元醇或醇胺3‑8份、碱性催化剂0.6‑1.8份、磷酸15‑25份、磷酸二酯1‑5份、环氧丙烷30‑50份、水1‑5份、阻燃剂0.5‑1.3份。本发明通过官能度较高的蔗糖作为主起始剂，保证了聚醚多元醇的高强度和极佳的尺寸稳定性，同时具有较低的羟值，用其制得的聚氨酯泡沫基材粘结性能好。

Description

一种环保聚氨酯全水组合料的制备工艺
技术领域
本发明涉及聚氨酯全水组合料技术领域，尤其涉及一种环保聚氨酯全水组合料的制备工艺。
背景技术
聚氨酯硬质泡沫以其优异的性能广泛应用于保温、制冷、建筑行业，但随着其应用范围广泛拓展，其对环境的负面影响给人们敲响了警钟。其中聚氨酯喷涂料主要应用于建筑保温行业，采用的发泡剂主要是HCFC-141b和水。HCFC等发泡剂皆为氟利昂类发泡剂，氟利昂的使用会消耗大气臭氧层，造成对大气臭氧层的破坏，导致紫外线照射增强并威胁到人类及其它地球生物的生存，是目前人类面临的最为严重的环境问题之一。
现有的聚氨酯全水组合料阻燃效率还是不够好，当高温环境下，阻燃剂容易氧化分解，从而导致阻燃失效，阻燃时间短，且现有的聚氨酯全水组合料环保性差，容易造成大气臭氧层的破坏，为此，本发明提出一种环保聚氨酯全水组合料的制备工艺。
发明内容
本发明的目的是为了解决现有技术中存在的缺点，而提出的一种环保聚氨酯全水组合料的制备工艺。
为了实现上述目的，本发明采用了如下技术方案：
一种环保聚氨酯全水组合料的制备工艺，包括以下步骤，
S1，准备原料，由以下重量份的原料组成：蔗糖15-25份、甘油5-15份、甲基邻苯二胺4-10份、小分子二元醇或醇胺3-8份、碱性催化剂0.6-1.8份、磷酸15-25份、磷酸二酯1-5份、环氧丙烷30-50份、水1-5份、阻燃剂0.5-1.3份；
S2，将上述重量份的蔗糖、甘油、甲基邻苯二胺、小分子二元醇或醇胺和碱性催化剂放入反应罐中反应，反应温度控制在50-100℃，反应6-8小时，得到多羟基混合物；
S3，向S2中制得的溶液中加入上述重量份的环氧丙烷、水和阻燃剂，140-160℃下反应4-5小时，充分搅拌使其充分反应，得到环保聚氨酯全水组合料；
S4，向环保聚氨酯全水组合料中加入磷酸、磷酸二酯，混合均匀，80-110℃下反应5-7小时，过滤后得到环保聚氨酯全水组合料。
优选的，所述S1中，准备原料，由以下重量份的原料组成：蔗糖15份、甘油5份、甲基邻苯二胺4份、小分子二元醇或醇胺3份、碱性催化剂0.6份、磷酸15份、磷酸二酯1份、环氧丙烷30份、水1份、阻燃剂0.5份。
优选的，所述S1中，准备原料，由以下重量份的原料组成：蔗糖20份、甘油10份、甲基邻苯二胺7份、小分子二元醇或醇胺5.5份、碱性催化剂1.2份、磷酸21份、磷酸二酯3.5份、环氧丙烷42份、水3.2份、阻燃剂0.9份。
优选的，所述S1中，准备原料，由以下重量份的原料组成：蔗糖25份、甘油15份、甲基邻苯二胺10份、小分子二元醇或醇胺8份、碱性催化剂1.8份、磷酸25份、磷酸二酯5份、环氧丙烷50份、水5份、阻燃剂1.3份。
优选的，所述小分子二元醇或醇胺为乙二醇、二乙二醇、丙二醇、二丙二醇、乙醇胺、二乙醇胺中的一种。
优选的，所述的碱性催化剂为氢氧化钾、氢氧化钠、乙醇钠中的一种或者两种。
优选的，所述磷酸二酯为磷酸二甲酯、磷酸二乙酯和磷酸二丙酯中的一种或者两种。
优选的，所述阻燃剂为聚磷酸铵、季戊四醇、三聚氰胺按照质量比4～6：1～2：1的复配物。
与现有技术相比，本发明的有益效果是：通过官能度较高的蔗糖作为主起始剂，保证了聚醚多元醇的高强度和极佳的尺寸稳定性，同时具有较低的羟值，用其制得的聚氨酯泡沫基材粘结性能好，制备过程中将环氧丙烷加入，在较低温度下加入环氧丙烷顺利激活聚合反应，避免了直接进行高温反应副产物的生成，更有利于聚醚多元醇合成指标的稳定性，而且制备聚氨酯泡沫的各项性能更加优良。通过特制的阻燃剂加入，由于阻燃剂内含有醇类，不仅可以产生很好的阻燃效果，而且还可以促进本发明的结构更加稳定，本发明在高温下也能很好的稳定存在，避免高温对阻燃剂造成影响，进而提高本发明的使用寿命。
具体实施方式
下面将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。
实施例一
一种环保聚氨酯全水组合料的制备工艺，包括以下步骤，
S1，准备原料，由以下重量份的原料组成：蔗糖15份、甘油5份、甲基邻苯二胺4份、小分子二元醇或醇胺3份、碱性催化剂0.6份、磷酸15份、磷酸二酯1份、环氧丙烷30份、水1份、阻燃剂0.5份；
S2，将上述重量份的蔗糖、甘油、甲基邻苯二胺、小分子二元醇或醇胺和碱性催化剂放入反应罐中反应，反应温度控制在50℃，反应6小时，得到多羟基混合物；
S3，向S2中制得的溶液中加入上述重量份的环氧丙烷、水和阻燃剂，140℃下反应4小时，充分搅拌使其充分反应，得到环保聚氨酯全水组合料；
S4，向环保聚氨酯全水组合料中加入磷酸、磷酸二酯，混合均匀，80℃下反应5小时，过滤后得到环保聚氨酯全水组合料。
实施例二
一种环保聚氨酯全水组合料的制备工艺，包括以下步骤，
S1，准备原料，由以下重量份的原料组成：蔗糖20份、甘油10份、甲基邻苯二胺7份、小分子二元醇或醇胺5.5份、碱性催化剂1.2份、磷酸21份、磷酸二酯3.5份、环氧丙烷42份、水3.2份、阻燃剂0.9份；
S2，将上述重量份的蔗糖、甘油、甲基邻苯二胺、小分子二元醇或醇胺和碱性催化剂放入反应罐中反应，反应温度控制在75℃，反应7小时，得到多羟基混合物；
S3，向S2中制得的溶液中加入上述重量份的环氧丙烷、水和阻燃剂，150℃下反应4.5小时，充分搅拌使其充分反应，得到环保聚氨酯全水组合料；
S4，向环保聚氨酯全水组合料中加入磷酸、磷酸二酯，混合均匀，90℃下反应6小时，过滤后得到环保聚氨酯全水组合料。
实施例三
一种环保聚氨酯全水组合料的制备工艺，包括以下步骤，
S1，准备原料，由以下重量份的原料组成：蔗糖25份、甘油15份、甲基邻苯二胺10份、小分子二元醇或醇胺8份、碱性催化剂1.8份、磷酸25份、磷酸二酯5份、环氧丙烷50份、水5份、阻燃剂1.3份；
S2，将上述重量份的蔗糖、甘油、甲基邻苯二胺、小分子二元醇或醇胺和碱性催化剂放入反应罐中反应，反应温度控制在100℃，反应8小时，得到多羟基混合物；
S3，向S2中制得的溶液中加入上述重量份的环氧丙烷、水和阻燃剂，160℃下反应5小时，充分搅拌使其充分反应，得到环保聚氨酯全水组合料；
S4，向环保聚氨酯全水组合料中加入磷酸、磷酸二酯，混合均匀，110℃下反应7小时，过滤后得到环保聚氨酯全水组合料。
聚氨酯全水组合料产品指标：
Figure BDA0002462231940000061
聚氨酯组合料与PAPI(多亚甲基多苯基多异氰酸酯)混合后的反应特性：
Figure BDA0002462231940000062
聚氨酯组合料与PAPI(多亚甲基多苯基多异氰酸酯)混合后生成泡沫的模塑特性：
Figure BDA0002462231940000063
本发明，通过官能度较高的蔗糖作为主起始剂，保证了聚醚多元醇的高强度和极佳的尺寸稳定性，同时具有较低的羟值，用其制得的聚氨酯泡沫基材粘结性能好，制备过程中将环氧丙烷加入，在较低温度下加入环氧丙烷顺利激活聚合反应，避免了直接进行高温反应副产物的生成，更有利于聚醚多元醇合成指标的稳定性，而且制备聚氨酯泡沫的各项性能更加优良。通过特制的阻燃剂加入，由于阻燃剂内含有醇类，不仅可以产生很好的阻燃效果，而且还可以促进本发明的结构更加稳定，本发明在高温下也能很好的稳定存在，避免高温对阻燃剂造成影响，进而提高本发明的使用寿命。
以上所述，仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，根据本发明的技术方案及其发明构思加以等同替换或改变，都应涵盖在本发明的保护范围之内。

Claims (8)

1.一种环保聚氨酯全水组合料的制备工艺，其特征在于，包括以下步骤，
S1，准备原料，由以下重量份的原料组成：蔗糖15-25份、甘油5-15份、甲基邻苯二胺4-10份、小分子二元醇或醇胺3-8份、碱性催化剂0.6-1.8份、磷酸15-25份、磷酸二酯1-5份、环氧丙烷30-50份、水1-5份、阻燃剂0.5-1.3份；
S2，将上述重量份的蔗糖、甘油、甲基邻苯二胺、小分子二元醇或醇胺和碱性催化剂放入反应罐中反应，反应温度控制在50-100℃，反应6-8小时，得到多羟基混合物；
S3，向S2中制得的溶液中加入上述重量份的环氧丙烷、水和阻燃剂，140-160℃下反应4-5小时，充分搅拌使其充分反应，得到环保聚氨酯全水组合料；
S4，向环保聚氨酯全水组合料中加入磷酸、磷酸二酯，混合均匀，80-110℃下反应5-7小时，过滤后得到环保聚氨酯全水组合料。
2.根据权利要求1所述的一种环保聚氨酯全水组合料的制备工艺，其特征在于，所述S1中，准备原料，由以下重量份的原料组成：蔗糖15份、甘油5份、甲基邻苯二胺4份、小分子二元醇或醇胺3份、碱性催化剂0.6份、磷酸15份、磷酸二酯1份、环氧丙烷30份、水1份、阻燃剂0.5份。
3.根据权利要求1所述的一种环保聚氨酯全水组合料的制备工艺，其特征在于，所述S1中，准备原料，由以下重量份的原料组成：蔗糖20份、甘油10份、甲基邻苯二胺7份、小分子二元醇或醇胺5.5份、碱性催化剂1.2份、磷酸21份、磷酸二酯3.5份、环氧丙烷42份、水3.2份、阻燃剂0.9份。
4.根据权利要求1所述的一种环保聚氨酯全水组合料的制备工艺，其特征在于，所述S1中，准备原料，由以下重量份的原料组成：蔗糖25份、甘油15份、甲基邻苯二胺10份、小分子二元醇或醇胺8份、碱性催化剂1.8份、磷酸25份、磷酸二酯5份、环氧丙烷50份、水5份、阻燃剂1.3份。
5.根据权利要求1所述的一种环保聚氨酯全水组合料的制备工艺，其特征在于，所述小分子二元醇或醇胺为乙二醇、二乙二醇、丙二醇、二丙二醇、乙醇胺、二乙醇胺中的一种。
6.根据权利要求1所述的一种环保聚氨酯全水组合料的制备工艺，其特征在于，所述的碱性催化剂为氢氧化钾、氢氧化钠、乙醇钠中的一种或者两种。
7.根据权利要求1所述的一种环保聚氨酯全水组合料的制备工艺，其特征在于，所述磷酸二酯为磷酸二甲酯、磷酸二乙酯和磷酸二丙酯中的一种或者两种。
8.根据权利要求1所述的一种环保聚氨酯全水组合料的制备工艺，其特征在于，所述阻燃剂为聚磷酸铵、季戊四醇、三聚氰胺按照质量比4～6：1～2：1的复配物。
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CN105315450A (zh) * 2015-11-25 2016-02-10 山东一诺威新材料有限公司 全水型聚氨酯硬泡用聚醚多元醇的制备方法
CN106008951A (zh) * 2016-07-01 2016-10-12 句容宁武新材料股份有限公司 一种利用环氧大豆油制备生物基阻燃聚醚多元醇的方法
CN110643030A (zh) * 2019-10-21 2020-01-03 滨化集团股份有限公司 一种全水发泡用硬泡阻燃聚醚多元醇的制备方法

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US3442888A (en) * 1962-05-17 1969-05-06 Allied Chem Sucrose - glycerol - alkyleneoxide polyol compositions and process for preparing same
CN105315450A (zh) * 2015-11-25 2016-02-10 山东一诺威新材料有限公司 全水型聚氨酯硬泡用聚醚多元醇的制备方法
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