CN114835971A - 一种高弹、透气艾草粉发泡复合材料及其制备方法、应用 - Google Patents
一种高弹、透气艾草粉发泡复合材料及其制备方法、应用 Download PDFInfo
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Abstract
本发明涉及一种高弹、透气艾草粉发泡复合材料及其制备方法、应用。首先将艾草粉碎并加水制成艾草糊，然后利用碳酸钠调节艾草糊的pH至6.5～8.5，再加入偏磷酸钠进行反应，接着加入醋酸酐继续反应，由此得到的改性艾草粉与DEDB混合进行包覆增塑，最后与EVA、高弹性橡塑材料、发泡剂、加工助剂等混合，经密炼、发泡成型得到高弹、透气的鞋垫等产品。本发明解决了艾草粉与EVA橡塑体系复合时存在的相容性差、易团聚、分散不均等问题，提供的发泡复合材料具有优良的弹性、耐压缩性、抗菌性以及一定的吸湿性，可以制作成鞋垫、拖鞋等各类日常生活用品，具有较好的应用前景和经济效益。
Description
技术领域
本发明涉及发泡复合材料及艾草开发利用技术领域，具体涉及一种高弹、透气艾草粉发泡复合材料及其制备方法、应用。
背景技术
艾草是一种天然的中药材，本身具有抗菌活血、祛湿散寒、理气血、温经等药理特性，除此以外还具有无毒、抗过敏、抗真菌、拥有独特香气等优点，因此艾草在生活中应用很广泛。
中国专利CN113527848A公开了一种艾草粉鞋料，包括以下重量份的原料：5～20份聚酯预聚体A、30～50份聚酯预聚体B、15～35份乙烯-醋酸乙烯共聚物、4～10份艾草粉、2～7份扩链剂、0.5～3份炭黑、0.6～3份疏水剂、0.7～2.2份抗氧剂、0.6～5份交联剂以及0.8～3.5份复合发泡剂，其中聚酯预聚体A和B均为1,4-丁二醇与丁二酸的缩聚产物，其它主料为EVA(乙烯-醋酸乙烯酯共聚物)材料。分析可知该配方中的预聚体A和B均属于硬质材料，其聚合后仍具有很高的极性，这样的简单混合不太可能制备出高弹性的艾草粉复合鞋用材料。
中国专利CN107760052A公开了一种艾草高分子复合材料，包括以下质量百分比的组份：艾草母料23％～27％、橡塑材料55％～65％、树脂8％～12％、交联剂4％～6％，其中艾草母料由艾草粉、橡塑材料加硫制得。该方案直接将未做任何改性处理的艾草粉与橡塑材料混合进行硫化，由于艾草分子结构中不具备硫化所需长链碳、碳碳双键，因此无法通过硫键交联。实际上艾草粉是以填料的形式存在于橡塑材料中，因此如果其用量达到或超过本发明用量16％，是无法制备出高性能鞋用材料的。
类似的专利技术还包括CN113907486A、CN109619764A、CN114098216A、CN112315118A等。综上目前艾草大多以艾草粉的形式与橡塑材料复合应用，然而研究表明艾草的主要活性成分为挥发油、多糖类、黄酮类及酚类物质，这些活性组分都有羟基并且属于极性化合物，很难与普通橡塑材料呈现良好的相容性，即相容性差、艾草粉在橡塑基体中分散困难。因此如何对艾草粉进行改性，并利用其制造出具有高弹、耐弯折、防臭、除味、吸汗、抗菌等优点的艾草基/EVA复合发泡材料成为亟待解决的难题。
发明内容
本发明的目的之一在于提供一种艾草的乙酰化改性方法，包括以下步骤：首先将艾草粉与水混合制成艾草糊，接着调节艾草糊的pH并加入磷酸盐进行反应，然后加入醋酸酐继续反应，最后分离提纯得到乙酰化艾草磷酸酯混合物。
进一步的，改性后的艾草粉含水率不超过5％，且粒径小于200目为宜。对比发现虽然粒径小于100目的艾草粉也可以应用此方法进行改性，但由此制得的产品表面较为粗糙。
进一步的，艾草糊在调节pH前需先升温至60～75℃，在加入醋酸酐前需降温至40～50℃。这是因为温度是艾草改性过程中的一个重要影响因素，加入醋酸酐会使得艾草糊温度升高，而醋酸酐与艾草糊乙酰化反应的最佳温度约45℃，因此中间需要进行降温处理。
进一步的，反应前利用碳酸钠或其水溶液调节艾草糊的pH至6.5～8.5，反应过程中利用碱试剂(如氢氧化钠或其水溶液)维持体系的pH在6.5～8.5之间。
进一步的，所述磷酸盐具体为偏磷酸钠，磷酸盐的加入量相当于艾草粉质量的0.5％～3％，优选为1.0％～2.0％。碳酸钠只是起中和作用，而偏磷酸钠能够参与反应获得磷酸化中间体。
进一步的，艾草粉、醋酸酐的质量比为100:6～10，优选为100:7～9。
进一步的，反应完先用稀盐酸调节溶液的pH至6.0～7.0，接着过滤并用水洗涤，所得固体干燥、粉碎后过200目筛网，得到乙酰化艾草磷酸酯混合物。
进一步的，制得的乙酰化艾草磷酸酯混合物还需与二乙二醇二苯甲酸酯(DEDB)混合搅拌进行包覆增塑，乙酰化艾草磷酸酯混合物与DEDB的质量比为8～12:1，优选为9～11:1。
本发明的目的之二在于提供一种高弹、透气艾草粉发泡复合材料，其按照重量份数计的配方包括：EVA 100份，高弹性橡塑材料20～25份，增塑过的乙酰化艾草磷酸酯混合物1～35份，发泡剂(偶氮二甲酰胺，AC)1～7份，加工助剂23～49份。
进一步的，所述高弹性橡塑材料包括EAA(乙烯-丙烯酸共聚物)1～3份，SEBS(苯乙烯-乙烯-丁烯-苯乙烯嵌段共聚物)10～22份，EVM(VA含量高于50％的EVA)5～5份。
进一步的，所述加工助剂包括硬脂酸1～5份，氧化锌1～8份，硬脂酸锌1～5份，无机粉填料19～31份，交联剂(过氧化二异丙苯，DCP)0.3～0.9份。
本发明的目的之三在于提供上述高弹、透气艾草粉发泡复合材料的制备方法，该方法包括以下步骤：按照配方准备好原料，将EVA、高弹性橡塑材料混合后加热至95～120℃密炼，再加入增塑过的乙酰化艾草磷酸酯混合物继续密炼，接着加入加工助剂、发泡剂再次密炼，密炼完压片并裁切成需要的粒料，最后将粒料加入成型设备中发泡成型即可。
本发明的目的之四在于利用上述高弹、透气艾草粉发泡复合材料制造高弹性鞋垫、中底、拖鞋、坐垫、瑜伽垫、爬行垫等产品，在这些产品的局部可以设置透气孔。
检索并未发现艾草粉化学改性的先例，发明人团队利用醋酸酐、DEDB等物质先后对艾草粉进行了乙酰化改性和增塑处理，使其与EVA等橡塑材料具有较好的相容性，具体的原理如下：艾草的化学结构中含有大量羟基，利用偏磷酸钠将艾草粉磷酸化成为磷酸酯后，能与醋酸酐发生乙酰化反应，因而乙酰化改性容易进行下去；改性后的艾草粉由于乙酰基的存在降低了亲水性，从而增加了其与EVA橡塑材料的相容性；再通过DEDB及体系中EAA等物质的增容作用，使得改性艾草粉在混炼过程中更容易分散，避免了团聚现象的发生。
改性后的艾草基本保留了原有的药理特性和独特香味，使得产品兼具天然艾草香味以及良好的抗菌性。相对于一般EVA发泡材料而言，发明人在复合材料配方中引入了高弹性橡塑材料，有利于增加产品的拉伸强度、撕裂强度、弹性并降低压缩变形，此外还大幅提高了产品的耐弯折性和透气性。
本发明的有益效果体现在以下几点：(1)成功开发了一种艾草粉改性方法，通过化学接枝艾草粉并与DEDB混合增塑，解决了艾草粉的团聚和分散不均匀问题；(2)采用高弹性材料与EVA基材共混造粒后发泡，使其具有优良的弹性、耐压缩性、抗菌性以及一定的吸湿性；(3)复合材料应用面较广，可以制作成鞋垫、中底、拖鞋、瑜伽垫、爬行垫等各类产品，其中的艾草成分不仅赋予了产品独特的颜色和香味，而且能够吸附异味，拖鞋类产品有助于防止蚊虫叮咬，抗菌性能良好。
附图说明
图1为利用本发明艾草粉发泡复合材料制得的鞋垫产品。
图2为利用本发明艾草粉发泡复合材料制得的拖鞋产品。
具体实施方式
为使本领域普通技术人员充分理解本发明的技术方案和有益效果，以下结合具体实施例及附图进行进一步说明。
本发明所使用的原料和试剂均为市售工业品。
实施例1
一、艾草粉的化学改性：量取400mL去离子水倒入容量为1000mL的三颈烧瓶中，再加入180g艾草粉搅拌均匀得到浓度为31％的艾草粉糊状液。将艾草粉糊状液加热升温至65℃，用碳酸钠溶液调节糊状液的pH至6.5～8.5，再加入1.6g偏磷酸钠搅拌120min后降温至45℃，接着加入14.4g醋酸酐继续反应，期间用质量分数为3％的NaOH溶液维持反应体系的pH稳定在6.5～8.5之间。反应120min后用质量分数为5％的稀HCl调节溶液的pH至6.5，过滤后用水洗涤，所得固体产物转入烘箱中于105℃下干燥24h，待其自然冷却后取出粉碎并过200目筛网，得到含水率在5％以下的乙酰化艾草磷酸酯混合物。
二、改性艾草粉的增塑：室温下将500g乙酰化艾草磷酸酯混合物投入密闭高速剪切机中，再加入50g DEDB搅拌5min，得到DEDB包覆增塑的乙酰化艾草磷酸酯混合物备用。
三、炼胶：将100g EVA、2g丙烯酸树脂EAA、18g SEBS216、5gEVM50加入到密炼机中于105℃下炼制5min，接着加入25g增塑后的改性乙酰化艾草磷酸酯混合物炼制8分钟，再加入2.5g硬脂酸、3.5g氧化锌、2g硬脂酸锌、25g滑石粉、5g发泡剂偶氮二甲酰胺AC和0.9g交联剂过氧化二异丙苯DCP继续密炼5min，最后压片并裁切成需要的料粒。
四、发泡成型：按照模具大小将规定量的粒料放入模板中，合模后发泡模压成型得到改性艾草基复合发泡产品，模压发泡条件为：时间400s，温度175℃，压力10MPa。
根据模具的不同，制得的鞋垫、拖鞋产品实物如图1～2所示，其中在鞋垫产品的脚掌部位分布有很多小孔，最外侧的小孔距离鞋垫边缘2～3mm。
对比例1
将150g EVA加入到密炼机中于105℃下炼制5min，接着加入2.5g硬脂酸、3.5g氧化锌、2g硬脂酸锌、25g滑石粉、4g发泡剂偶氮二甲酰胺AC和0.7g交联剂过氧化二异丙苯DCP继续密炼3min，最后压片并裁切成需要的料粒。
按照模具大小将规定量的粒料放入模板中，合模后发泡模压成型得到普通EVA发泡产品，模压发泡条件为：时间420s，温度180℃，压力10MPa。
对比例2
将100g EVA、2g丙烯酸树脂EAA、18g SEBS216、5g EVM50加入到密炼机中于105℃下炼制5min，接着加入25g艾草粉(与实施例1同批次，但未做任何改性处理)炼制8分钟，再加入2.5g硬脂酸、3.5g氧化锌、2g硬脂酸锌、25g滑石粉、5g发泡剂偶氮二甲酰胺AC和0.9g交联剂过氧化二异丙苯DCP继续密炼5min，最后压片并裁切成需要的料粒。
按照模具大小将规定量的粒料放入模板中，合模后发泡模压成型得到艾草基复合发泡产品，模压发泡条件为：时间350s，温度172℃，压力10MPa。对比可知，该配方下的发泡条件发生了明显改变。
对实施例1及对比例1～2制得的鞋垫样品进行了一系列测试，其中硬度测试按照GB/T 3903.4—2008鞋类通用检验方法硬度试验方法进行；密度测试参照GB/T 6343—2009泡沫塑料及橡胶表观密度的测定进行；回弹性测试参照GB/T 1681—2009硫化橡胶回弹性的测定进行，测试条件：温度2322℃，湿度6525％RH，每个样品随机测定3次，以平均值作为该样品的最终回弹率；压缩变形性测试依据HG/T 2876—2009橡塑鞋微孔材料压缩变形试验方法进行，拉伸强度和伸长率试验按照GB/T 10654—2001高聚物多孔弹性材料拉伸强度和拉断伸长率的测定进行；撕裂强度按照GB/T 10808—2006高聚物多孔弹性材料撕裂强度的测定进行；吸水率试验参考GB/T 8810—2005硬质泡沫塑料吸水率的测定进行，试验条件：三级水温度23±2℃，96h；抗菌性能测试按照QB/T2881—2013鞋类和鞋类部件抗菌性能技术条件附录B菌液吸收法进行。相关测试结果如下表1所示。
表1不同鞋垫产品的性能指标对照表
由表1可以看出，未经过乙酰化改性和增塑的艾草粉直接与EVA橡塑材料复合发泡，所得发泡产品表面极易出现气泡，发泡倍率也会明显减小进而导致硬度增加(由33～42变为48～55)。虽然该产品也可以勉强发泡，但由于弹性、伸长率明显下降以及硬度明显增加，已经不适合作为鞋垫、拖鞋等产品。与未添加艾草粉的产品相比，利用乙酰化改性和DEDB增塑的艾草粉制得的同类产品各项性能更为突出，尤其表现在密度、弹性、耐压缩性、抗菌性、吸湿性等指标。
Claims (9)
1.一种艾草的乙酰化改性方法，其特征在于，该方法包括以下步骤：首先将艾草粉制成艾草糊并调节其pH，然后加入磷酸盐反应，接着加入醋酸酐继续反应，最后分离提纯得到乙酰化艾草磷酸酯混合物。
2.如权利要求1所述的方法，其特征在于：艾草糊在调节pH前需先升温至60～75℃，在加入醋酸酐前需降温至40～50℃。
3.如权利要求1所述的方法，其特征在于：反应前利用碳酸钠或其水溶液调节艾草糊的pH至6.5～8.5，反应过程中利用碱试剂维持体系的pH在6.5～8.5之间；反应完先用酸试剂调节溶液的pH至6.0～7.0，接着过滤并用水洗涤，所得固体干燥、粉碎后过200目筛网，得到乙酰化艾草磷酸酯混合物。
4.如权利要求1所述的方法，其特征在于：所述磷酸盐具体为偏磷酸钠，磷酸盐的加入量相当于艾草粉质量的0.5％～3％，优选为1.0％～2.0％；艾草粉、醋酸酐的质量比为100:6～10，优选为100:7～9。
5.如权利要求1所述的方法，其特征在于：制得的乙酰化艾草磷酸酯混合物进一步与DEDB混合搅拌进行包覆增塑，乙酰化艾草磷酸酯混合物与DEDB的质量比为8～12:1，优选为9～11:1。
6.一种高弹、透气艾草粉发泡复合材料，其特征在于：该发泡复合材料按照重量份数计的配方包括：EVA 100份，高弹性橡塑材料20～25份，增塑过的乙酰化艾草磷酸酯混合物1～35份，发泡剂1～7份，加工助剂23～49份。
7.如权利要求6所述的发泡复合材料，其特征在于：所述高弹性橡塑材料包括EAA 1～3份，SEBS 10～22份，EVM 5～15份；所述加工助剂包括硬脂酸1～5份，氧化锌1～8份，硬脂酸锌1～5份，无机粉填料19～31份，交联剂0.3～0.9份。
8.权利要求6～7任意一项所述高弹、透气艾草粉发泡复合材料的制备方法，其特征在于，该方法包括以下步骤：按照配方准备好原料，将EVA、高弹性橡塑材料混合后加热至95～120℃密炼，再加入增塑过的乙酰化艾草磷酸酯混合物继续密炼，接着加入加工助剂、发泡剂再次密炼，密炼完压片并裁切成粒料，最后将粒料加入成型设备中发泡成型即可。
9.权利要求6～7任意一项所述高弹、透气艾草粉发泡复合材料在制造高弹性鞋垫、中底、拖鞋、坐垫、瑜伽垫、爬行垫方面的应用。
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