CN110076867B - 基于环氧树脂的木塑复合材料辐射固化方法 - Google Patents
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Abstract
本发明提供了一种基于环氧树脂的木塑复合材料辐射固化方法，包括以下步骤：S1，将植物原料浸没在无机酸或有机酸溶液中浸泡预处理，并过滤去除多余的无机酸或有机酸溶液；S2，将预处理后的植物原料烘干；S3，将烘干后的植物原料加入添加有阳离子引发剂的环氧树脂浸渍；S4，将步骤S3中混合物通过强辐射源进行辐照交联固化得到环氧树脂基木塑复合材料，辐射剂量率1～100kGy/s，辐射总剂量为1～100kGy；S5，将辐射后的环氧树脂基木塑复合材料烘干，得到终产品。
Description
技术领域
本发明涉及一种基于环氧树脂的木塑复合材料辐射固化方法。
背景技术
用辐射方法将液态有机单体迅速转化成固体的手段被称为“辐射固化”，常见辐射源包括激光、紫外光、γ辐射源和EB辐射源。相对传统热固化方式，辐射固化通常有能耗低、污染少、品质高、加工速度快等优点，可应用在涂料、油墨、胶粘剂等高聚物材料固化领域。而木塑复合材料(Wood Plastic Composites,WPC)也属于辐射固化的一个重要分支。所谓WPC是指，指利用聚乙烯、聚丙烯和聚氯乙烯等，代替通常的树脂胶粘剂，与超过50％以上的木粉、稻壳、秸秆等废植物纤维混合成新的木质材料，再经挤压、模压、注射成型等塑料加工工艺，生产出的板材或型材，然后引发浸渍物聚合、交联或接枝反应，最终得到木塑复合材料。通过辐射固化得到的WPC一般能同时具有天然木材和人造高聚物的优点，在力学性能、防腐、阻燃等方面得到不同程度的提高。国外辐射法制造WPC已有较长历史，美国在1975年生产了2000多吨WPC，辐射固化的WPC地板在1973～1980年间也生产了200多平方米。此外日本、加拿大、英国、德国、印度等过都开展了大量关于WPC的研究，均有中试以上的规模的实验或工业化产品推出。
通过浸渍改性木材早已有之，但传统的方法一般需要含有不饱和烯键或环氧官能团的单体/预聚体+热引发剂等成分组成，辐射固化技术由于具有射线可穿透材料、本身可辐射电离产生自由基、辐射剂量易精确控制等特点，它具有传统热引发固化所不具备的优点：(1)固化过程均匀，反应完全，单体残留少；(2)不用或少用引发剂，方便单体回收；(3)常温进行，能耗少，同时减少单体热挥发损失和污染；(4)反应过程更可控。
环氧树脂作为辐射固化原料也有不少报道例子，很多报道都是环氧作为掺杂用料，与烯烃类共混，采用自由基引发聚合，或者采用化学固化剂来引发环氧体系常温自发交联或加热交联。
但是在实际应用中发现几个困难，(1)环氧树脂单独使用时很难通过自由基辐照引发交联固化；(2)环氧树脂与植物原料混合后会引起阳离子辐射引发被阻聚。
发明内容
本发明提供了一种基于环氧树脂的木塑复合材料辐射固化方法，可以有效解决上述问题。
本发明是这样实现的：
一种基于环氧树脂的木塑复合材料辐射固化方法，包括以下步骤：
S1，将植物原料浸没在无机酸或有机酸溶液中浸泡预处理，并过滤去除多余的无机酸或有机酸溶液；
S2，将预处理后的植物原料烘干；
S3，将烘干后的植物原料加入添加有阳离子引发剂的环氧树脂浸渍；
S4，将步骤S3中混合物通过强辐射源进行辐照交联固化得到环氧树脂基木塑复合材料，辐射剂量率1～100kGy/s，辐射总剂量为1～100kGy；
S5，将辐射后的环氧树脂基木塑复合材料烘干，得到终产品。
作为进一步改进的，在步骤S1中，所述植物原料选自纤维、粉末或块状等各类植物原料；所述无机酸或有机酸溶液选自硫酸、草酸或磷酸中的一种或多种。
作为进一步改进的，在步骤S1中，所述将植物原料浸没在无机酸或有机酸溶液中浸泡预处理的步骤包括：
S11，将植物原料浸没在0.1～1mol/l的硫酸、草酸或磷酸溶液中，浸泡12～36h。
作为进一步改进的，在步骤S2中，所述将预处理后的植物原料烘干的步骤包括：
S21，将预处理后的植物原料在45～100度加热并烘干3～6小时。
作为进一步改进的，在步骤S3中，所述环氧树脂与阳离子引发剂按照质量比100～1000：1混合。
作为进一步改进的，在步骤S3中，所述将烘干后的植物原料加入添加有阳离子引发剂的环氧树脂浸渍的步骤包括：
S31，将烘干后的植物原料加入添加有阳离子引发剂的环氧树脂中，加压0～1MPa浸渍1～4小时。
作为进一步改进的，在步骤S4中，辐射总剂量为10～60kGy。
作为进一步改进的，在步骤S4中，所述将步骤S3中的混合物通过强辐射源进行辐照交联固化得到环氧树脂基木塑复合材料的步骤包括：
S41，将步骤S3中的混合物取出后用模具盛装或拭干后进行辐照交联固化得到环氧树脂基木塑复合材料。
本发明的有益效果是：本发明经过实验，采用对植物原料酸液浸泡过滤多余酸液后烘干，再与环氧树脂混合，发现此时就可以克服植物原料成分对环氧阳离子聚合过程的阻聚效应，同过中低辐射剂量的伽马辐射或电子束辐射，在少量阳离子引发剂帮助下即可引发环氧树脂-植物原料混合体系聚合固化。
附图说明
为了更清楚地说明本发明实施方式的技术方案，下面将对实施方式中所需要使用的附图作简单地介绍，应当理解，以下附图仅示出了本发明的某些实施例，因此不应被看作是对范围的限定，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他相关的附图。
图1是本发明实施例提供的基于环氧树脂的木塑复合材料辐射固化方法的流程图。
具体实施方式
为使本发明实施方式的目的、技术方案和优点更加清楚，下面将结合本发明实施方式中的附图，对本发明实施方式中的技术方案进行清楚、完整地描述，显然，所描述的实施方式是本发明一部分实施方式，而不是全部的实施方式。基于本发明中的实施方式，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施方式，都属于本发明保护的范围。因此，以下对在附图中提供的本发明的实施方式的详细描述并非旨在限制要求保护的本发明的范围，而是仅仅表示本发明的选定实施方式。基于本发明中的实施方式，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施方式，都属于本发明保护的范围。
参照图1所示，一种基于环氧树脂的木塑复合材料辐射固化方法，包括以下步骤：
S1，将植物原料浸没在无机酸或有机酸溶液中浸泡预处理，并过滤去除多余的无机酸或有机酸溶液；
S2，将预处理后的植物原料烘干；
S3，将烘干后的植物原料加入添加有阳离子引发剂的环氧树脂浸渍；
S4，将步骤S3中混合物通过强辐射源进行辐照交联固化得到环氧树脂基木塑复合材料，辐射剂量率1～100kGy/s，辐射总剂量为1～100kGy；
S5，将辐射后的环氧树脂基木塑复合材料烘干，得到终产品。
步骤S1中，所述植物原料选自竹粉或木粉。植物原料也不仅限于特定木材，可以是木材，竹材，灌木，草本等各类可用的植物的块状、刨花、纤维、粉末等原料。
所述无机酸或有机酸溶液选自硫酸、草酸或磷酸中的一种或多种。
所述将植物原料浸没在无机酸或有机酸溶液中浸泡预处理的步骤包括：
S11，将植物原料浸没在0.1～1mol/l的硫酸、草酸或磷酸溶液中，浸泡12～36h。
在步骤S2中，所述将预处理后的植物原料烘干的步骤包括：
S21，将预处理后的植物原料在45～100度加热并真空烘干3～6小时。
所述环氧树脂与阳离子引发剂按照质量比1000～100：1混合。所述环氧树脂优选为酚醛-环氧丙烷类常见系列环氧树脂。所述阳离子引发剂也不仅限于硫鎓盐类引发剂，凡各类可在电离辐射下产生阳离子的有机或无机类阳离子引发剂均可。
在步骤S3中，所述将烘干后的植物原料加入添加有阳离子引发剂的环氧树脂浸渍的步骤包括：
S31，将烘干后的植物原料加入添加有阳离子引发剂的环氧树脂中，加压0～1MPa浸渍1～4小时。
在步骤S4中，辐射源可以为电子束或天然放射元素产生的伽马射线源。所述辐射总剂量优选为10～60kGy。
另外，所述将步骤S3中的混合物通过强辐射源进行辐照交联固化得到环氧树脂基木塑复合材料的步骤包括：
S41，将步骤S3中的混合物减压取出后用模具盛装或拭干后进行辐照交联固化得到环氧树脂基木塑复合材料。
实施例1：
取环氧树脂:硫鎓盐质量比为100:1，混合均匀；将木材浸没至0.5mol/l的硫酸溶液中，浸泡24h；木材烘干条件如上；浸渍过程常温加压0.5MPa保压1小时；浸渍后样品直接在空气中辐射，辐射总剂量约50kGy；辐射固化后样品50度真空烘干1小时得成品。
按该例配方和工艺过程所得白松木改性样品，在实验室得到的各项性能为：
(1)木材最后总增重率约70～80％；
(2)24小时吸水率，由未处理前35％降至处理后的约10％，耐水能力提高约3倍；
(3)最大拉伸断裂强度，由未处理前木材的约17MPa,处理后增加至约25MPa，力学强度提高了30％以上。
以上所述仅为本发明的优选实施方式而已，并不用于限制本发明，对于本领域的技术人员来说，本发明可以有各种更改和变化。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 (4)
1.一种基于环氧树脂的木塑复合材料辐射固化方法，其特征在于，包括以下步骤：
S1，将植物原料浸没在无机酸或有机酸溶液中浸泡预处理，并过滤去除多余的无机酸或有机酸溶液；
S2，将预处理后的植物原料烘干；
S3，将烘干后的植物原料加入添加有阳离子引发剂的环氧树脂浸渍；
S4，将步骤S3中混合物通过强辐射源进行辐照交联固化得到环氧树脂基木塑复合材料，辐射剂量率1~99kGy/s；
S5，将辐射后的环氧树脂基木塑复合材料烘干，得到终产品；
在步骤S3中，所述环氧树脂与阳离子引发剂按照质量比100~1000：1混合；
在步骤S3中，所述将烘干后的植物原料加入添加有阳离子引发剂的环氧树脂浸渍的步骤包括：
S31，将烘干后的植物原料加入添加有阳离子引发剂的环氧树脂中，加压0~1MPa浸渍1~4小时；
在步骤S2中，所述将预处理后的植物原料烘干的步骤包括：
S21，将预处理后的植物原料在50~70℃加热并真空烘干3~6小时；
在步骤S4中，辐射总剂量为10~60kGy；辐射源为天然放射元素产生的伽马射线源。
2.如权利要求1所述的固化方法，其特征在于，在步骤S1中，所述植物原料选自竹粉或木粉；所述无机酸或有机酸溶液选自硫酸、草酸或磷酸中的一种或多种。
3.如权利要求2所述的固化方法，其特征在于，在步骤S1中，所述将植物原料浸没在无机酸或有机酸溶液中浸泡预处理的步骤包括：
S11，将植物原料浸没在0.1~1mol/L的硫酸、草酸或磷酸溶液中，浸泡12~36h。
4.如权利要求3所述的固化方法，其特征在于，在步骤S4中，所述将步骤S3中的混合物通过强辐射源进行辐照交联固化得到环氧树脂基木塑复合材料的步骤包括：
S41，将步骤S3中的混合物取出后用模具盛装或拭干后直接进行辐照交联固化得到环氧树脂基木塑复合材料。
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