CN111851079B - 一种微囊化的含艾草精油的驱蚊面料整理剂及驱蚊面料整理方法 - Google Patents
一种微囊化的含艾草精油的驱蚊面料整理剂及驱蚊面料整理方法 Download PDFInfo
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Abstract
本发明公开一种微囊化的含艾草精油的驱蚊面料整理剂，通过如下方法制得：依次配制阿拉伯胶、含可聚合阴离子表面活性剂、艾草精油、肉桂油和薄荷油的预聚合乳液，含可聚合酯类单体、可聚合羧酸类单体和氧化还原法制得的石墨烯粉末的单体预乳液，然后室温条件下，于氧化还原催化体系中由预聚合乳液制得胶囊种子乳液；再滴加单体预乳液和剩余的还原剂溶液，制得微囊化的含艾草精油的驱蚊面料整理剂，稀释后整理经阳离子改性的面料。整理后的面料，后期无需高温固着，不会破坏微胶囊结构，保证微胶囊稳定性和持久性。
Description
技术领域
本发明属于纺织整理技术领域，具体涉及一种微囊化的含艾草精油的驱蚊面料整理剂及驱蚊面料整理方法。
背景技术
夏季，天气炎热、蚊虫较多，为了防止蚊虫叮咬，开发出了具有驱蚊效果的服装面料，但是现有技术中的驱蚊面料多为多层结构，包括基布层、面料层和设置在基布层与面料层之间的驱蚊层，如中国专利文献(申请号为201410428554.1)公开了一种驱蚊吸湿面料，再如中国专利文献(申请号为201510284983.0)公开的一种效果好的抗菌驱蚊面料及其制备方法，均存在料层多、透汽难、闷热不耐水洗的缺陷。
发明内容
为了克服背景技术中的问题，本发明提供一种微囊化的含艾草精油的驱蚊面料整理剂及驱蚊面料整理方法。通过本发明方法将艾叶精油微胶囊化，并同时引入肉桂油和薄荷油，获得驱蚊面料整理剂，即可赋予面料驱蚊止痒功能，有可增加面料清凉舒适感，特别适用于夏季衣物。
为了实现本发明目的，所采用的技术方案为：一种微囊化的含艾草精油的驱蚊面料整理剂，所述整理剂由如下步骤制得：
步骤1，将阿拉伯胶溶于去离子水中，再加入可聚合阴离子表面活性剂、薄荷油、艾草精油和肉桂油，制得预聚合乳液，各组分的质量百分含量为：可聚合阴离子表面活性剂5％-10％，艾草精油15％-20％，薄荷油2％-5％，肉桂油2％-5％，阿拉伯胶为5％-10％，余量为去离子水；
步骤2，将平平加O-30溶于去离子水中，再加入可聚合酯类单体、可聚合羧酸类单体和氧化还原法制得的石墨烯粉末，制得单体预乳液，各组分质量百分含量为：可聚合酯类单体25％-45％，可聚合羧酸类单体3％-10％，石墨烯粉末0.05％-0.2％，平平加O-30为1％-6％，余量为去离子水；石墨烯粉末的片径＜1μm，层数＜5层；
步骤3，将过硫酸铵溶于去离子水中，配制氧化剂溶液，过硫酸铵用量为可聚合阴离子表面活性剂、可聚合酯类单体和可聚合羧酸类单体总摩尔数的1-3％；将维生素C溶于去离子水中，配制还原剂溶液，维生素C的用量为可聚合阴离子表面活性剂、可聚合酯类单体和可聚合羧酸类单体总摩尔数的0.01-0.1％；
步骤4，室温条件下，边搅拌边向步骤1制得的预聚合乳液中同时滴加1/5步骤3中配制的氧化剂溶液和还原剂溶液，控制氧化剂溶液的滴加速度在5-10min内滴完，还原剂溶液的滴加速度在30-60min内滴完，滴加结束后继续反应10-30min；保温结束后，加入剩余氧化剂溶液，再向其中滴加所述的单体预乳液和剩余的还原剂溶液，1.5-3h内滴加完，滴加结束后继续反应0.5-1.5h，制得所述微囊化的含艾草精油的驱蚊面料整理剂。
进一步的，步骤2中所述可聚合酯类单体为甲基丙烯酸乙酯、甲基丙烯酸丙酯、甲基丙烯酸丁酯、丙烯酸甲酯、丙烯酸乙酯、丙烯酸丙酯、丙烯酸丁酯、丙烯酸羟乙酯、丙烯酸羟丙酯、甲基丙烯酸羟乙酯或甲基丙烯酸羟丙酯中的任意一种或多种。
进一步的，步骤2中所述可聚合羧酸类单体为丙烯酸、甲基丙烯酸中的任意一种。
进一步的，步骤1中所述可聚合阴离子表面活性剂为ABM、MAPM、MAEM、VBM或VBS中的任意一种，结构式为：
ABM CH2＝CHCOO(CH2)4OCOCH＝CHCOOH
MAPM CH2＝CH(CH3)COOCH2CH(CH3)OCOCH＝CHCOOH
MAEM CH2＝CH(CH3)COO(CH2)2OCOCH＝CHCOOH
VBM CH2＝CHC6H4CH2OCOCH＝CHCOOH
VBS CH2＝CHC6H4CH2OCOCH2CH2COOH。
一种驱蚊面料整理方法，包括如下步骤：
步骤a，将面料浸扎含有双(3-氯-2-羟丙基)四甲基二氯化乙二铵的溶液，然后烘干，再浸扎氢氧化钠溶液，焙烘后冷却，制得阳离子改性面料；
步骤b，将如上所述的微囊化的含艾草精油的驱蚊面料整理剂用去离子水稀释，然后将步骤a中制得的阳离子改性面料浸泡在稀释后的微囊化的含艾草精油的驱蚊面料整理剂中，浸扎后脱水烘干，制得驱蚊面料。
进一步的，所述面料由70％再生纤维素纤维的纱线、20％棉纤维和10％的氨纶纤维制造而成。
相比于现有技术，本发明所取得的技术效果为：
以含有阿拉伯胶和可聚合阴离子表面活性剂的预聚合乳液，在氧化还原体系下制备精油种子乳液，种子乳液中阿拉伯胶包裹在精油表面，进而初步囊化，结合阴离子表面活性剂，促进相容性，便于进一步形成微囊化的的含艾草精油的驱蚊面料整理剂。
微囊化的含艾草精油的驱蚊面料整理剂于室温制得，反应温度低，减少艾叶精油有效成分的损失，保持艾叶精油的新鲜感和驱蚊效果。
引入丙烯酸类单体，可以赋予微囊化的含艾草精油的驱蚊面料整理剂的胶黏特性，与面料表面的季铵盐阳离子结合，大大提升了整理剂在面料上的附着率和附着力，后期整理无需高温固着，不会破坏微胶囊结构，保证微胶囊稳定性和持久驱蚊止痒效果。
氧化还原法制备的石墨烯表面具有少量缺陷，在缺陷附近的双键具有反应活性，可以参与到自由基聚合反应中，从而接枝到微胶囊。通过引入石墨烯，可以提高微胶囊壁的屏蔽性，降低微胶囊内薄荷油的释放速率。石墨烯还可以提高微胶囊的机械强度，且石墨烯表面残留的羧基基团可与面料接枝的季铵盐结合成化学键，增强其在面料上的附着力，从而提高其在纤维表面的寿命；此外，加入石墨烯可以提高面料的抑菌能力。
本发明的整理剂含羧基等阴离子基团与面料上接枝的阳离子基团，形成化学键，提高了整理剂在面料上的附着密度，保证面料较好的驱蚊、止痒效果，及较好的透气性和凉爽舒适性。
说明书附图
图1为本发明各实施例制得的微囊化的含艾草精油的驱蚊面料整理剂整理面料后的缓释性能图。
图2为本发明各实施例制得的微囊化的含艾草精油的驱蚊面料整理剂整理面料后的耐水洗性能图。
具体实施方式
本发明下面结合实施例作进一步详述：
实施例1
一种微囊化的含艾草精油的驱蚊面料整理剂，由如下步骤制得：
步骤1，将阿拉伯胶溶于去离子水中，再加入可聚合阴离子表面活性剂、薄荷油、艾草精油和肉桂油，制得预聚合乳液，各组分的质量百分含量为：可聚合阴离子表面活性剂7％，艾草精油15％，薄荷精油5％，肉桂油5％，阿拉伯胶为7％，余量为去离子水。
步骤2，将平平加O-30溶于去离子水中，再加入可聚合酯类单体、可聚合羧酸类单体和氧化还原法制得的石墨烯粉末，制得单体预乳液，各组分质量百分含量为：可聚合酯类单体45％，可聚合羧酸类单体3％，石墨烯粉末0.05％，平平加O-30为1％，余量为去离子水；石墨烯粉末的片径＜1μm，层数＜5层；
步骤3，将过硫酸铵溶于去离子水中，配制氧化剂溶液，过硫酸铵用量为可聚合阴离子表面活性剂、可聚合酯类单体和可聚合羧酸类单体总摩尔数的1.5％；将维生素C溶于去离子水中，配制还原剂溶液，维生素C的用量为可聚合阴离子表面活性剂、可聚合酯类单体和可聚合羧酸类单体总摩尔数的0.08％；
步骤4，室温条件下，边搅拌边向步骤1制得的预聚合乳液中同时滴加1/5步骤3中配制的氧化剂溶液和还原剂溶液，控制氧化剂溶液的滴加速度在5min内滴完，还原剂溶液的滴加速度在40min内滴完，滴加结束后继续反应30min；保温结束后，加入剩余氧化剂溶液，再向其中滴加所述的单体预乳液和剩余的还原剂溶液，3h内滴加完，滴加结束后继续反应0.5h，制得含微囊化的含艾草精油的驱蚊面料整理剂的乳液。
可聚合酯类单体为质量比为1:1:1:1的甲基丙烯酸乙酯、甲基丙烯酸丙酯、丙烯酸甲酯和丙烯酸羟丙酯，可聚合羧酸类单体为丙烯酸，可聚合阴离子表面活性剂为ABM。
一种驱蚊面料整理方法，包括如下步骤：
步骤a，将面料浸扎含有双(3-氯-2-羟丙基)四甲基二氯化乙二铵的溶液，然后烘干，再浸扎氢氧化钠溶液，焙烘后冷却，制得阳离子改性面料；
步骤b，将如上所述的微囊化的含艾草精油的驱蚊面料整理剂用去离子水稀释至微胶囊的质量含量为15％，然后将步骤a中制得的阳离子改性面料浸泡在稀释后的微囊化的含艾草精油的驱蚊面料整理剂中，浸扎后脱水烘干，制得驱蚊面料。面料与稀释后的微囊化的含艾草精油的驱蚊面料整理剂的质量比为3％，控制轧余率90％。其中面料由70％再生纤维素纤维的纱线、20％棉纤维和10％的氨纶纤维制造而成。
实施例2
一种薄荷清香凉感再生纤维素纤维的氨纶面料的整理方法，包括如下步骤：
步骤1，将阿拉伯胶溶于去离子水中，再加入可聚合阴离子表面活性剂、薄荷油、艾草精油和肉桂油，制得预聚合乳液，各组分的质量百分含量为：可聚合阴离子表面活性剂5％，艾草精油18％，薄荷油4％，肉桂油3％，平阿拉伯胶为8％，余量为去离子水；
步骤2，将平平加O-30溶于去离子水中，再加入可聚合酯类单体、可聚合羧酸类单体和氧化还原法制得的石墨烯粉末，制得单体预乳液，各组分质量百分含量为：可聚合酯类单体25％，可聚合羧酸类单体10％，石墨烯粉末0.1％，平平加O-30为6％，余量为去离子水；石墨烯粉末的片径＜1μm，层数＜5层；
步骤3，将过硫酸铵溶于去离子水中，配制氧化剂溶液，过硫酸铵用量为可聚合阴离子表面活性剂、可聚合酯类单体和可聚合羧酸类单体总摩尔数的1.5％；将维生素C溶于去离子水中，配制还原剂溶液，维生素C的用量为可聚合阴离子表面活性剂、可聚合酯类单体和可聚合羧酸类单体总摩尔数的0.03％；
步骤4，室温条件下，边搅拌边向步骤1制得的预聚合乳液中同时滴加1/5步骤3中配制的氧化剂溶液和还原剂溶液，控制氧化剂溶液的滴加速度在10min内滴完，还原剂溶液的滴加速度在30min内滴完，滴加结束后继续反应10min；保温结束后，加入剩余氧化剂溶液，再向其中滴加所述的单体预乳液和剩余的还原剂溶液，2h内滴加完，滴加结束后继续反应1h，制得含微囊化的含艾草精油的驱蚊面料整理剂的乳液；
一种驱蚊面料整理方法，包括如下步骤：
步骤a，将面料浸扎含有双(3-氯-2-羟丙基)四甲基二氯化乙二铵的溶液，然后烘干，再浸扎氢氧化钠溶液，焙烘后冷却，制得阳离子改性面料；
步骤b，将如上所述的含微囊化的含艾草精油的驱蚊面料整理剂的乳液用去离子水稀释至微胶囊的质量浓度为15％，然后将步骤a中制得的阳离子改性面料浸泡在稀释后的微囊化的含艾草精油的驱蚊面料整理剂中，浸扎后脱水烘干，制得驱蚊面料。面料与稀释后的微囊化的含艾草精油的驱蚊面料整理剂的质量比为3％，控制轧余率90％。其中面料由70％再生纤维素纤维的纱线、20％棉纤维和10％的氨纶纤维制造而成。
可聚合酯类单体为质量比为1:1:2:2:1的甲基丙烯酸丙酯、甲基丙烯酸丁酯、丙烯酸甲酯、丙烯酸乙酯、甲基丙烯酸羟乙酯和甲基丙烯酸羟丙酯，可聚合羧酸类单体为甲基丙烯酸，可聚合阴离子表面活性剂为MAPM。
实施例3
一种微囊化的含艾草精油的驱蚊面料整理剂，由如下步骤制得：
步骤1，将阿拉伯胶溶于去离子水中，再加入可聚合阴离子表面活性剂、薄荷油、艾草精油和肉桂油，制得预聚合乳液，各组分的质量百分含量为：可聚合阴离子表面活性剂10％，艾草精油18％，薄荷油2％，肉桂油5％，阿拉伯胶为10％，余量为去离子水；
步骤2，将平平加O-30溶于去离子水中，再加入可聚合酯类单体、可聚合羧酸类单体和氧化还原法制得的石墨烯粉末，制得单体预乳液，各组分质量百分含量为：可聚合酯类单体30％，可聚合羧酸类单体5％，石墨烯粉末0.1％，平平加O-30为2％，余量为去离子水；石墨烯粉末的片径＜1μm，层数＜5层；
步骤3，将过硫酸铵溶于去离子水中，配制氧化剂溶液，过硫酸铵用量为可聚合阴离子表面活性剂、可聚合酯类单体和可聚合羧酸类单体总摩尔数的3％；将维生素C溶于去离子水中，配制还原剂溶液，维生素C的用量为可聚合阴离子表面活性剂、可聚合酯类单体和可聚合羧酸类单体总摩尔数的0.05％；
步骤4，室温条件下，边搅拌边向步骤1制得的预聚合乳液中同时滴加1/5步骤3中配制的氧化剂溶液和还原剂溶液，控制氧化剂溶液的滴加速度在8min内滴完，还原剂溶液的滴加速度在60min内滴完，滴加结束后继续反应20min；保温结束后，加入剩余氧化剂溶液，再向其中滴加所述的单体预乳液和剩余的还原剂溶液，3h内滴加完，滴加结束后继续反应1h，制得含微囊化的含艾草精油的驱蚊面料整理剂的乳液；
一种驱蚊面料整理方法，包括如下步骤：
步骤a，将面料浸扎含有双(3-氯-2-羟丙基)四甲基二氯化乙二铵的溶液，然后烘干，再浸扎氢氧化钠溶液，焙烘后冷却，制得阳离子改性面料；
步骤b，将如上所述的含微囊化的含艾草精油的驱蚊面料整理剂的乳液用去离子水稀释至微胶囊的质量浓度为15％，然后将步骤a中制得的阳离子改性面料浸泡在稀释后的微囊化的含艾草精油的驱蚊面料整理剂中，浸扎后脱水烘干，制得驱蚊面料。面料与稀释后的微囊化的含艾草精油的驱蚊面料整理剂的质量比为3％，控制轧余率90％。其中面料由70％再生纤维素纤维的纱线、20％棉纤维和10％的氨纶纤维制造而成。
可聚合酯类单体为质量比为2:1的甲基丙烯酸乙酯和丙烯酸甲酯，可聚合羧酸类单体为丙烯酸，可聚合阴离子表面活性剂为VBS。
对比实施例1
与实施例1不同之处为单体预乳液中石墨烯粉末的含量为0，可聚合羧酸类单体3.05％，其余均与实施例1相同。
对比实施例2
与实施例1不同之处为整理面料未经阳离子改性，其余均与实施例1相同。
效果例
囊化率测定：参考期刊文献：王璐,肖刚,许时英.微胶囊化薄荷油缓释性能的测定[J].食品与发酵工业，1999,26(2):28-31.先测定微胶囊的总含油量，再测定微胶囊表面油含量，囊化率＝(微胶囊的总含油量-微胶囊表面油含量)/微胶囊的总含油量×100％，经测定，实施例1、2、3及对比实施例1制得的微囊化的含艾草精油的驱蚊面料整理剂的囊化率分别为96.5％、95.9％、96.3％、96.4％。
微囊化的含艾草精油的驱蚊面料整理剂整理后面料的缓释性能测试：将上述各实施例及对比实施例1中的微囊化的含艾草精油的驱蚊面料整理剂整理后面料置于100℃的烘箱中，分别测试0、2、4、6、8、10h后织物上的艾叶精油剩余百分含量。具体测试方法如下：取1g上述实施例和对比实施例中微囊化的含艾草精油的驱蚊面料整理剂整理后面料，剪碎置于四口烧瓶中，然后加入5mL 0.809mol/L的HCl溶液，65℃搅拌30min，然后加入15mL乙酸乙酯，搅拌90min后，以4000r/min离心2min，取上清液进行气相色谱分析，气相色谱条件：GC-950型气相色谱，载气：氮气；进样口温度：250℃，进样量：0.2μL，进样方式：分流；柱温：80℃，保持1min，然后以20℃/min的速率升温至150℃，保持3min；FID温度：250℃。测试结果见图1，由图1可以看出添加有石墨烯粉末的微胶囊缓释性能明显提高。
经微囊化的含艾草精油的驱蚊面料整理剂整理后面料的耐水洗性能及驱蚊效果：按GB/T 8629-2017《纺织品试验用家庭洗涤和干燥程序》标准测试，分别测定上述各实施例及对比实施例1中的微囊化的含艾草精油的驱蚊面料整理剂整理后面料经0、2、4、6、8、10次水洗后，面料残留艾叶精油量及面料驱蚊效果。面料残留艾叶精油量采用气相色谱法进行测定，气相色谱条件：GC-950型气相色谱，载气：氮气；进样口温度：250℃，进样量：0.2μL，进样方式：分流；柱温：80℃，保持1min，然后以20℃/min的速率升温至150℃，保持3min；FID温度：250℃。测试结果见图2，从图2中可以看出添加石墨烯粉末后，微囊化的含艾草精油的驱蚊面料整理剂耐水洗性能明显提高。驱蚊面料的驱蚊测试方法具体为：在6个300mm×300mm×300mm的蚊笼内放入准备好的雌性致倦库蚊300只，选择3个人，左手手心平铺准备好的面料(分别为水洗0次、6次和10次的面料)，然后将左右分别同时伸入2个蚊笼内5min，手心向上，观察并记录前来停留和吸血的蚊虫数，右手作为空白对照手有30只以上的蚊虫前来即判蚊虫攻击力合格，左手面料驱蚊效果有效，实验过程中室温为26～27℃，相对湿度60～70％，试验结果见表1：
表1驱蚊效果测试
由表1可以看出，水洗十次后实施例1至3获得的驱蚊面料依然具有驱蚊效果，对比实施例1和对比实施例2的驱蚊效果明显下降。
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 (6)
1.一种微囊化的含艾草精油的驱蚊面料整理剂，其特征在于：所述整理剂由如下步骤制得：
步骤1，将阿拉伯胶溶于去离子水中，再加入可聚合阴离子表面活性剂、薄荷油、艾草精油和肉桂油，制得预聚合乳液，各组分的质量百分含量为：可聚合阴离子表面活性剂5％-10％，艾草精油15％-20％，薄荷油2％-5％，肉桂油2％-5％，阿拉伯胶为5％-10％，余量为去离子水；
步骤2，将平平加O-30溶于去离子水中，再加入可聚合酯类单体、可聚合羧酸类单体和氧化还原法制得的石墨烯粉末，制得单体预乳液，各组分质量百分含量为：可聚合酯类单体25％-45％，可聚合羧酸类单体3％-10％，石墨烯粉末0.05％-0.2％，平平加O-30为1％-6％，余量为去离子水；石墨烯粉末的片径＜1μm，层数＜5层；
步骤3，将过硫酸铵溶于去离子水中，配制氧化剂溶液，过硫酸铵用量为可聚合阴离子表面活性剂、可聚合酯类单体和可聚合羧酸类单体总摩尔数的1-3％；将维生素C溶于去离子水中，配制还原剂溶液，维生素C的用量为可聚合阴离子表面活性剂、可聚合酯类单体和可聚合羧酸类单体总摩尔数的0.01-0.1％；
步骤4，室温条件下，边搅拌边向步骤1制得的预聚合乳液中同时滴加1/5步骤3中配制的氧化剂溶液和还原剂溶液，控制氧化剂溶液的滴加速度在5-10min内滴完，还原剂溶液的滴加速度在30-60min内滴完，滴加结束后继续反应10-30min；保温结束后，加入剩余氧化剂溶液，再向其中滴加所述的单体预乳液和剩余的还原剂溶液，1.5-3h内滴加完，滴加结束后继续反应0.5-1.5h，制得所述微囊化的含艾草精油的驱蚊面料整理剂。
2.如权利要求1所述的微囊化的含艾草精油的驱蚊面料整理剂，其特征在于：步骤2中所述可聚合酯类单体为甲基丙烯酸乙酯、甲基丙烯酸丙酯、甲基丙烯酸丁酯、丙烯酸甲酯、丙烯酸乙酯、丙烯酸丙酯、丙烯酸丁酯、丙烯酸羟乙酯、丙烯酸羟丙酯、甲基丙烯酸羟乙酯或甲基丙烯酸羟丙酯中的任意一种或多种。
3.如权利要求1所述的微囊化的含艾草精油的驱蚊面料整理剂，其特征在于：步骤2中所述可聚合羧酸类单体为丙烯酸、甲基丙烯酸中的任意一种。
4.如权利要求1所述的微囊化的含艾草精油的驱蚊面料整理剂，其特征在于：步骤1中所述可聚合阴离子表面活性剂为ABM、MAPM、MAEM、VBM或VBS中的任意一种。
5.一种驱蚊面料整理方法，其特征在于：包括如下步骤：
步骤a，将面料浸扎含有双(3-氯-2-羟丙基)四甲基二氯化乙二铵的溶液，然后烘干，再浸扎氢氧化钠溶液，焙烘后冷却，制得阳离子改性面料；
步骤b，将如权利要求1至4中任一项所述的微囊化的含艾草精油的驱蚊面料整理剂用去离子水稀释，然后将步骤a中制得的阳离子改性面料浸泡在稀释后的微囊化的含艾草精油的驱蚊面料整理剂中，浸扎后脱水烘干，制得驱蚊面料。
6.根据权利要求5所述的驱蚊面料整理方法，其特征在于：所述面料由70％再生纤维素纤维的纱线、20％棉纤维和10％的氨纶纤维制造而成。
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