CN103665300A - 一种制备木质素型聚氨酯泡沫材料的方法 - Google Patents

一种制备木质素型聚氨酯泡沫材料的方法 Download PDF

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CN103665300A
CN103665300A CN201310655818.2A CN201310655818A CN103665300A CN 103665300 A CN103665300 A CN 103665300A CN 201310655818 A CN201310655818 A CN 201310655818A CN 103665300 A CN103665300 A CN 103665300A
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曲玉宁
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Abstract

本发明涉及一种木质素聚氨酯泡沫的制备方法。通过一步法将改性后的木质素经超声分散溶解于聚醚多元醇，最后与异氰酸酯等原料复配，得到木质素型聚氨酯发泡材料。本发明所用的木质素反应活性较高，所用的聚醚多元醇既可作为溶剂，又可参与合成反应，对木质素具有良好的溶解性，整个制备过程工艺简单，绿色环保，由于木质素廉价易得，降低了聚氨酯泡沫产品的成本。

Description

一种制备木质素型聚氨酯泡沫材料的方法
技术领域
本发明涉及一种制备木质素型聚氨酯泡沫材料的方法，具体涉及通过一步发泡工艺合成木质素含量不同的木质素型聚氨酯泡沫的方法。
背景技术
聚氨酯泡沫由多元醇和多异氰酸酯在催化剂和发泡剂的作用下缩聚、发泡而形成的。木质素因其改性后含有丰富的羟基含量，可以代替一部分聚醚多元醇参与到反应中去，从而可代替多元醇与多异氰酸酯进行缩聚。在聚氨酯领域，很多研究者利用利用木质素或改性木质素溶解于溶剂并与多元醇混合，在催化剂的作用下生成木质素型聚氨酯，此方法无论是从原料的利用率还是材料的机械强度都有很大的提高，对聚氨酯产业起到很大的作用。木质素是一类含有丰富的醇羟基和酚羟基的天然的高分子化合物，是植物中的第二大组成部分。近年来，随着环境污染和化工原料的紧缺，木质素因其自身的分子结构，而且是可再生的，具有无污染可降解的特点，木质素被广泛的用在聚氨酯等高分子的领域中。由于木质素分子中含有羟基基团，可以作为一种醇类和聚氨酯中的主反应物异氰酸酯作用，代替一部分聚醚多元醇，参与到反应中来，这样不但可以提高聚氨酯的性能，而且节省聚醚多元醇的用量，降低成本，木质素在聚氨酯中的作用主要是交联和填充的作用。专利CN1651478公开了一种高沸醇木质素聚氨酯的制备的方法，具体步骤是将高沸醇木质素或高沸醇木质素衍生物溶于有机溶剂，再与多元醇或多元醇的溶液混合，通过加热或搅拌使它完全混合均匀，然后再加入一定量的多异氰酸酯，加热使它们反应，再加入其他改性添加剂或填料，适当加热使之反应完全。专利CN101696261A公开了一种木质素聚氨酯及其制备方法，该方法包括步骤：将秸秆生产燃料乙醇的残渣中用氢氧化钠抽提分离出的木质素用有机溶剂溶解，除去残渣后用水沉淀，分离木质素，并用环氧化物进行改性，再溶解于多元醇，最后与异氰酸酯等原料复配，得到聚氨酯材料。专利CN1958636一种酶解木质素聚氨酯的原料配方及其制备方法，具体步骤为将酶解木质素或其衍生物溶于有机溶剂再与多元醇或多元醇与有机溶剂的混合液混合，加热或搅拌混合均匀再加入异氰酸酯加热，加入常用的改性添加剂或填料，加热使反应完全减压蒸出溶剂得棕色固体，水洗烘干得酶解木质素聚氨酯。专利CN103183801A公开了CIMV小麦秸秆木质素聚氨酯薄膜的制备方法，具体步骤为：CIMV小麦秸秆木质素和聚醚多元醇的混合；CIMV小麦秸秆木质素聚氨酯薄膜的形成；CIMV小麦秸秆木质素聚氨酯薄膜的熟化。专利CN1406258公开了一种聚氨酯泡沫材料及其制造方法，采用此方法聚氨酯泡沫具有优良的耐压缩变定性，该可热成型的聚氨酯泡沫材料在负荷下具有优良耐压缩变定性和形状保持性。
以上专利中，大部分专利利用有机溶剂溶解木质素制备木质素聚氨酯材料，未见公开制备木质素型聚氨酯泡沫的专利。
发明内容
为实现本发明所提供的技术方案是：
(1)白料的制备
首先称取一定量的聚醚多元醇，然后加入改性后的木质素0～1g，超声分散，依次加入发泡剂0.45～0.75，泡沫稳定剂0.3g，然后加入催化剂0.03～0.13g，充分混合均匀，即白料的配制。
(2)称取一定量的异氰酸酯(MDI)，即黑料。
(3)在通风橱中将步骤(1)和步骤(2)的白料和黑料混合，不断搅拌，直至混合液体出现乳白现象，停止搅拌，观察发泡过程，直至不再发泡为止。
为更好理解本发明，下面结合实施例对本发明做进一步地详细说明，但是本发明要求保护的范围并不局限于实施例表示的范围。
实施例1：
(1)白料的制备
首先称取一定量的聚醚多元醇，然后加入改性后的木质素0.5g，超声分散，依次加入发泡剂0.45g，泡沫稳定剂0.3g，然后加入催化剂0.08g，充分混合均匀，即白料的配制。
(2)称取21g的异氰酸酯(MDI)，即黑料。
(3)在通风橱中将步骤(1)和步骤(2)的白料和黑料混合，不断搅拌，直至混合液体出现乳白现象，停止搅拌，观察发泡过程，直至不再发泡为止。发泡时间为4min25s，发泡倍数为39倍。
实施例2：改变催化剂的用量为0.03g，其他步骤同实施例1，得到木质素型聚氨酯泡沫材料的发泡时间3min34s，发泡倍数41倍。
实施例3：改变发泡剂的用量为0.60g，其他步骤同实施例1，得到木质素型聚氨酯泡沫材料的发泡时间3min56s，发泡倍数20倍。
实施例4：改变木质素的用量为1g，其他步骤同实施例1，得到木质素型聚氨酯泡沫的发泡时间3min3s，发泡倍数40倍。

Claims (4)

1.一种制备木质素型聚氨酯泡沫材料的方法，具体步骤如下：
(1)白料的制备
称取一定量的聚醚多元醇，然后加入改性后的木质素0～1g，超声分散，依次加入发泡剂0.45～0.75，泡沫稳定剂0.3g，然后加入催化剂0.03～0.13g，充分混合均匀，即白料的配制；
(2)称取一定量的异氰酸酯(MDI)，即黑料；
(3)在通风橱中将步骤(1)和步骤(2)的白料和黑料混合，不断搅拌，直至混合液体出现乳白现象，停止搅拌，观察发泡过程，直至不再发泡为止。
2.一种如权利要求1所述的一种制备木质素型聚氨酯泡沫材料的方法，其特征在于：木质素可以是碱木质素、酸性木质素、醇解木质素。
3.一种如权利要求1所述的一种制备木质素型聚氨酯泡沫材料的方法，其特征在于：发泡剂可以是水、环戊烷、正丁烷、异戊烷、氢化氟烷烃等发泡剂。
4.一种如权利要求1所述的一种制备木质素型聚氨酯泡沫材料的方法，其特征在于：催化剂可以是二月硅酸二丁基锡、三乙烯二胺、N，N-二甲基环己胺DMCHA等催化剂。
CN201310655818.2A 2013-12-05 2013-12-05 一种制备木质素型聚氨酯泡沫材料的方法 Pending CN103665300A (zh)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104448186A (zh) * 2014-11-20 2015-03-25 镇江拜因诺生物科技有限公司 一种生物基聚氨酯泡沫保温材料
CN106832173A (zh) * 2015-12-07 2017-06-13 财团法人工业技术研究院 生物多元醇组合物与生物聚氨酯发泡材料
CN107001565A (zh) * 2014-11-25 2017-08-01 Cj第制糖株式会社 硬质聚氨酯泡沫及其制备方法
CN109081900A (zh) * 2018-07-06 2018-12-25 山东圣泉新材料股份有限公司 改性多元醇及制备方法、改性聚氨酯材料及制备方法和应用
CN111072892A (zh) * 2019-11-28 2020-04-28 梅亚萍 隔音隔热铝门用聚氨酯泡沫填充材料
CN111662458A (zh) * 2020-06-01 2020-09-15 浙江高裕家居科技股份有限公司 木质素基嵌段共聚分子级组合聚醚、其制备方法及其在聚氨酯软泡材料制备中的应用

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104448186A (zh) * 2014-11-20 2015-03-25 镇江拜因诺生物科技有限公司 一种生物基聚氨酯泡沫保温材料
CN107001565A (zh) * 2014-11-25 2017-08-01 Cj第制糖株式会社 硬质聚氨酯泡沫及其制备方法
US10604615B2 (en) 2014-11-25 2020-03-31 Cj Cheiljedang Corporation Rigid polyurethane foam and preparation method thereof
CN106832173A (zh) * 2015-12-07 2017-06-13 财团法人工业技术研究院 生物多元醇组合物与生物聚氨酯发泡材料
US10323115B2 (en) 2015-12-07 2019-06-18 Industrial Technology Research Institute Bio-polyol composition and bio-polyurethane foam
CN106832173B (zh) * 2015-12-07 2019-11-05 财团法人工业技术研究院 生物多元醇组合物与生物聚氨酯发泡材料
CN109081900A (zh) * 2018-07-06 2018-12-25 山东圣泉新材料股份有限公司 改性多元醇及制备方法、改性聚氨酯材料及制备方法和应用
CN109081900B (zh) * 2018-07-06 2021-01-26 山东圣泉新材料股份有限公司 改性多元醇及制备方法、改性聚氨酯材料及制备方法和应用
CN111072892A (zh) * 2019-11-28 2020-04-28 梅亚萍 隔音隔热铝门用聚氨酯泡沫填充材料
CN111662458A (zh) * 2020-06-01 2020-09-15 浙江高裕家居科技股份有限公司 木质素基嵌段共聚分子级组合聚醚、其制备方法及其在聚氨酯软泡材料制备中的应用

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