CN107955151A - 一种生物基改性硬泡多元醇的制备方法 - Google Patents

一种生物基改性硬泡多元醇的制备方法 Download PDF

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CN107955151A
CN107955151A CN201711101041.XA CN201711101041A CN107955151A CN 107955151 A CN107955151 A CN 107955151A CN 201711101041 A CN201711101041 A CN 201711101041A CN 107955151 A CN107955151 A CN 107955151A
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李志生
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Guangzhou Friend Poly New Material Co Ltd
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Abstract

本发明公开了一种生物基改性硬泡多元醇的制备方法，首先将亲核试剂与环氧丙烷或环氧乙烷在100‑135℃，压力0‑0.3MPa条件下反应5‑12小时催化剂作用经抽真空脱水过滤制得聚醚多元醇；随后将制得聚醚多元醇与环氧化合物、油脂混合物、助剂在催化剂作用170‑260℃，压力0‑0.2MPa条件下反应5‑20小时，经抽真空脱水过滤制得生物基改性多元醇。本发明以环氧丙烷、环氧乙烷、亲核试剂、环氧化合物、油脂混合物等主要原料进行综合改性，产品生产工艺简单环保，基本没有三废产生，制得生物基改性硬泡多元醇收率高，具有低温抗冻性、粘度适宜流动性好、应用领域广泛的特点，所得聚氨酯硬质泡沫塑料制品泡孔细腻、导热系数低、脆性小、强度高的特性，可替代石油类多元醇。

Description

一种生物基改性硬泡多元醇的制备方法
技术领域
本发明涉及生物技术领域，具体为一种生物基改性硬泡多元醇的制备方法。
背景技术
聚氨酯工业起源于德国，半个多世纪以来在欧、美、日迅速发展，目前已达到千万吨级的产业规模。随着低碳生活方式越来越为人们所接受，中国的硬泡在建筑节能、太阳能热水器、仿木家具、管道保温、工程应用等领域有巨大的发展空间，中国目前已成为并将保持为世界最大的聚氨酯硬泡市场。
随着石油消耗量增加,人类面临着石油资源的日益短缺和原油价格的不断上涨,用可再生资源生产生物材料、化工原料和燃料越来越吸引人们的重视。用生物基产品替代石油原料生产聚氨酯是未来发展的必然趋势，将含羟基的植物油或羟基化的植物油作为多元醇制备聚氨酯完全符合环保要求。
据有关资料报道，生物质多元醇与石油类多元醇相比能耗降低23％，非可再生资源消耗降低61％，向大气排放温室气体减少36％。每使用1kg生物基聚氨酯能够减排二氧化碳1.2kg因此，进一步推广生物质可再生资源在聚氨酯泡沫塑料中的应用，提高植物油基多元醇、纤维素改性多元醇、木质素多元醇等在聚氨酯硬泡中的使用，被列为我国聚氨酯工业“十三五”规划的重要内容之一。
然而，在目前制备生物基多元醇的众多技术工艺中，所得到的产品存在产品抗冻性差粘度高、相容性差、羟值低等诸多缺点，直接导致生产发泡使用过程中存在配方调试难度大、工艺操控难度高等问题，所得的发泡制品泡沫脆性大、强度低等缺点，不利于家电、板材、喷涂等聚氨酯硬泡领域的推广应用，制约着生物基多元醇的发展。
发明内容
本发明的目的在于提供一种生物基改性硬泡多元醇的制备方法，产品生产工艺简单环保，基本没有三废产生，制得生物基改性硬泡多元醇具有低温抗冻性、粘度适宜流动性好、相容性好、应用领域广泛的特点，以解决上述背景技术中提出的问题。
为实现上述目的，本发明提供如下技术方案：
申请人经研究发现，采用一种生物基改性硬泡多元醇的制备方法，包括以下步骤：
S1：将亲核试剂与环氧丙烷或环氧乙烷在催化剂作用100-135℃，压力0-0.3MPa条件下反应5-12小时，经抽真空脱水过滤制得聚醚多元醇；
S2：将制得聚醚多元醇与环氧化合物、油脂混合物、助剂在催化剂作用170-260℃，压力0-0.2MPa条件下反应5-20小时，经抽真空脱水过滤制得生物基改性多元醇；
优选的，所述步骤S1中亲核试剂为三乙醇胺、丙三醇、二甘醇、三羟甲基丙烷。
优选的，催化剂为氢氧化钠、氢氧化钾、甲醇钠、甲基咪唑。
优选的，所述步骤S2中环氧化合物为环氧大豆油、环氧地沟油、环氧潲水油。
优选的，所述步骤S2中油脂混合物为棕榈油、地沟油、潲水油。
优选的，步骤S2中助剂为匀泡剂AK8805。
优选的，所述亲核试剂与环氧丙烷或环氧乙烷用量(重量)比例为1：(0.7-2)
优选的，制得聚醚多元醇与环氧化合物、油脂混合物、助剂用量(重量)比例为1：(1-1.5)：(0-0.1)：(0-0.05)。
优选的，所述步骤S1或S2中中催化剂用量占总重量比例的0.05-0.2％
与现有技术相比，本发明的有益效果是：
本生物基改性硬泡多元醇的制备方法，以环氧丙烷、环氧乙烷、亲核试剂、环氧化合物、油脂混合物等主要原料进行综合改性，产品生产工艺简单环保，基本没有三废产生，制得生物基改性硬泡多元醇收率高，具有低温抗冻性、粘度适宜流动性好、相容性好、应用领域广泛的特点，所得聚氨酯硬质泡沫塑料制品泡孔细腻、导热系数低、脆性小、强度高的特性，可替代石油类多元醇。
附图说明
图1为本发明步骤一反应原理图；
图2为本发明步骤二反应原理图。
图中：R为-CH2-CH2-O-CH2-CH2-OH。
具体实施方式
下面将结合本发明实施例中的附图，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：
将400g三乙醇胺加入搅拌反应装置内，抽真空氮气置换3次，加入催化剂甲醇钠1.2g，关闭阀门开搅拌升温至100℃，然后逐步滴加环氧乙烷300g，在110～120℃反应5小时，压力小于等于0.25MPa。待反应压力为0时，升温至125～130℃熟化1小时，然后抽真空脱水，制得聚醚多元醇。将制得聚醚多元醇300g、催化剂甲醇钠1.2g、环氧大豆油300g、棕榈油20g依次加入搅拌反应装置内。氮气置换2次后常压条件下程序化逐步升温至180℃反应6小时，然后降温抽真空脱水过滤，制得生物基改性硬泡多元醇Ⅰ，产品收率为99.85％。经检测其水分0.05％，羟值355mgKOH/g，粘度3550cps，冷冻浊点3℃。
实施例2：
将400g二甘醇加入搅拌反应装置内，抽真空氮气置换3次，加入催化剂氢氧化钠2g，关闭阀门开搅拌升温至100℃，然后逐步滴加环氧丙烷320g，在110～120℃反应5小时，压力小于等于0.25MPa。待反应压力为0时，升温至125～130℃熟化1小时，然后抽真空脱水，制得聚醚多元醇。将制得聚醚多元醇350g、催化剂甲醇钠1.1g、环氧地沟油360g、潲水油10g依次加入搅拌反应装置内。氮气置换2次后常压条件下程序化逐步升温至210℃反应10小时，然后抽真空脱水过滤，制得生物基改性硬泡多元醇Ⅱ，产品收率为99.88％。经检测其水分0.04％，羟值373mgKOH/g，粘度2640cps，冷冻浊点0℃。
实施例3：
将50g二甘醇、400g甘油加入搅拌反应装置内，抽真空氮气置换3次，加入催化剂甲醇钠2g，关闭阀门开搅拌升温至100℃，然后逐步滴加环氧丙烷450g，在110～120℃反应6小时，压力小于等于0.25MPa。待反应压力为0时，升温至125～130℃熟化1小时，然后抽真空脱水，制得聚醚多元醇。将制得聚醚多元醇400g、催化剂甲基咪唑2g、环氧潲水油450g、地沟油25g，依次加入搅拌反应装置内。氮气置换2次后常压条件下逐步升温至230℃反应7小时，然后降温加入20g助剂AK8805搅拌抽真空脱水过滤，制得生物基改性硬泡多元醇Ⅲ，产品收率为99.81％。经检测其水分0.07％，羟值410mgKOH/g，粘度 4640cps，冷冻浊点2℃。
各实施例均按以下方法制备：将各原料按表1中所给的份额投入容器内搅拌均匀(将聚醚多元醇、催化剂、泡沫稳定剂和水加入并混匀)，得到硬泡组合聚醚。将该组合聚醚与甲苯二异氰酸酯按组合聚醚：异氰酸酯＝1：(1～1.3)的重量比进行高速混合反应，其中，反应温度为20-25℃，搅拌速度为3000r/min(在起始时间搅拌即可)，乳白时间为9±3s，发泡时间为100±30s，制成硬质聚氨酯泡沫塑料。
表1 各实施例的原料配比及所得产品的性能表
注：1.聚醚多元醇4110，羟值430mgKOH/g，生产厂家为为绍兴恒丰聚氨酯实业有限公司；三乙烯二胺，生产厂家为江都市大江化工厂；环己胺，生产厂家为空气化工产品(上海)有限公司；匀泡剂AK-8811，AK8830生产厂家为南京美思德新材料有限公司；异氰酸酯PM-200，生产厂家为万华化学集团股份有限公司；环戊烷，生产厂家为锦化化工集团有限责任公司；2.上表中原料均按质量份额计算；3.泡沫表观芯密度按国家标准GB/T 6343-2009进行测试；导热系数按国家标准GB/T 10294-2008进行测试；压缩强度按国家标准GB/T8813-2008进行测试；尺寸稳定性按国家标准GB/T 8811-2008进行测试；
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 (10)

1.一种生物基改性硬泡多元醇的制备方法，其特征在于，包括以下步骤：
S1：将亲核试剂与环氧丙烷或环氧乙烷在催化剂作用100-135℃，压力0-0.3MPa条件下反应5-12小时，经抽真空脱水过滤制得聚醚多元醇；
S2：将制得聚醚多元醇与环氧化合物、油脂混合物、助剂在催化剂作用170-260℃，压力0-0.2MPa条件下反应5-20小时，经抽真空脱水过滤制得生物基改性多元醇。
2.根据权利要求1所述的一种生物基改性硬泡多元醇的制备方法，其特征在于，所述步骤S1中亲核试剂为一乙醇胺、二乙醇胺、三乙醇胺、乙二胺、甲苯二胺、丙二醇、乙二醇、丙三醇、二甘醇、三羟甲基丙烷、季戊四醇、木糖醇、山梨醇、蔗糖、聚酯多元醇中的一种或几种。
3.根据权利要求1所述的一种生物基改性硬泡多元醇的制备方法，其特征在于，所述催化剂为氢氧化钠、氢氧化钾、甲醇钠、乙醇钠、甲醇钾、乙醇钾、咪唑、甲基咪唑中的一种或几种。
4.根据权利要求1所述的一种生物基改性硬泡多元醇的制备方法，其特征在于，所述步骤S2中环氧化合物为环氧地沟油、环氧潲水油、环氧大豆油、环氧棉籽油、环氧棕榈油、环氧菜籽油、环氧脂肪酸甲酯、环氧亚麻油中的一种或几种，其环氧化合物的环氧值2%-7%。
5.根据权利要求1所述的一种生物基改性硬泡多元醇的制备方法，其特征在于，所述步骤S2中油脂混合物为地沟油、潲水油、大豆油、棉籽油、棕榈油、菜籽油、脂肪酸甲酯、亚麻油中的一种或几种。
6.根据权利要求1所述的一种生物基改性硬泡多元醇的制备方法，其特征在于，所述步骤S2中助剂为匀泡剂硅油AK8805、AK8811、AK8830、AK8863中的一种或几种。
7.根据权利要求1所述的一种生物基改性硬泡多元醇的制备方法，其特征在于，所述步骤S2中反应温度在170-260℃压力0-0.2MPa条件下反应5-20小时，反应过程为程序化控制分阶段逐步进行升温。
8.根据权利要求1或2所述的一种生物基改性硬泡多元醇的制备方法，其特征在于，所述亲核试剂与环氧丙烷或环氧乙烷用量（重量）比例为1：（0.5-4）。
9.根据权利要求1或4或5所述的一种生物基改性硬泡多元醇的制备方法，其特征在于，制得聚醚多元醇与环氧化合物、油脂混合物、助剂用量（重量）比例为1：（0.7-1.5）：（0-0.2）：（0-0.1）。
10.根据权利要求1或3所述的一种生物基改性硬泡多元醇的制备方法，其特征在于，所述步骤S1或S2中中催化剂用量占总重量比例的0.01-0.4％。
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CN111286019A (zh) * 2020-02-24 2020-06-16 滨化集团股份有限公司 一种高粘结力发泡用硬质聚醚多元醇的制备方法
CN113637221A (zh) * 2021-09-24 2021-11-12 长春工业大学 一种废聚氨酯泡沫液化制备多元醇的方法
CN113717374A (zh) * 2021-09-24 2021-11-30 长春工业大学 一种生物基阻燃聚醚多元醇的制备方法及用途
CN115160556A (zh) * 2022-08-04 2022-10-11 江苏华大新材料有限公司 一种生物基聚醚酯多元醇及其制备方法

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Publication number Priority date Publication date Assignee Title
CN111286019A (zh) * 2020-02-24 2020-06-16 滨化集团股份有限公司 一种高粘结力发泡用硬质聚醚多元醇的制备方法
CN113637221A (zh) * 2021-09-24 2021-11-12 长春工业大学 一种废聚氨酯泡沫液化制备多元醇的方法
CN113717374A (zh) * 2021-09-24 2021-11-30 长春工业大学 一种生物基阻燃聚醚多元醇的制备方法及用途
CN115160556A (zh) * 2022-08-04 2022-10-11 江苏华大新材料有限公司 一种生物基聚醚酯多元醇及其制备方法
CN115160556B (zh) * 2022-08-04 2024-03-26 江苏华大新材料有限公司 一种生物基聚醚酯多元醇及其制备方法

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