CN112376265B - 一种制备纺织品用抗微生物处理剂的方法 - Google Patents

一种制备纺织品用抗微生物处理剂的方法 Download PDF

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CN112376265B
CN112376265B CN202011261192.3A CN202011261192A CN112376265B CN 112376265 B CN112376265 B CN 112376265B CN 202011261192 A CN202011261192 A CN 202011261192A CN 112376265 B CN112376265 B CN 112376265B
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CN112376265A (zh
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蒋婵娟
顾海斌
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Shanghai Pushel Technology Co ltd
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Abstract

本发明提供了一种制备纺织品用抗微生物处理剂的方法，其特征在于，包括以下步骤：S1)提供以下溶液，a)二价铜离子盐，b)氨水或铵盐，c)无机碱性水溶液，d)仅含有碳、氢、氧元素的醇类或糖类有机物，e)水；S2)将上述溶液混合，陈化，以醇类或糖类为催化剂，形成铜铵配合物的复合物。本发明的制备纺织品用抗微生物处理剂的方法，处理剂不含有重金属和可能具有毒性的氮、磷、硫等的有机元素，用于纺织品整理采用的碱性材料不包含非挥发性或有机胺化合物，巧妙地利用以醇类或糖类有机物做为催化剂，铜离子形成配合物过渡，使天然纺织品纤维与铜离子接枝的更牢固，具有安全、环保、耐擦洗和抗菌效力高、持续时间长的优点。

Description

一种制备纺织品用抗微生物处理剂的方法
技术领域
本发明属于抗微生物复合材料技术领域，具体涉及一种制备纺织品用抗微生物处理剂的方法。
背景技术
由于中国消费生活水平的不断提高，对各类纺织品的品质提出了更高的要求。来源天然的棉织物因手感柔软、穿着舒适，但其抗菌防霉性差，易引起微生物孳生，对人的身体健康造成很大的威胁。微生物会在纺织品上寄生并生长，也会降低纺织品的寿命，使之成为微生物传播的载体。纺织品抗微生物处理剂可以降低纺织品上微生物的生长，提高纺织品的耐用性，降低洗涤次数，降低因微生物导致的感染，具有良好的环保性，提高人的健康水平。
由于抗微生物材料往往对自然环境和人体安全具有风险，抗微生物材料本身的环保问题与人体安全问题越来越成为关注的焦点。以银、汞、铅、砷、锡、锌等金属元素的无机抗菌剂和有机+金属抗菌剂会对人体和环境造成污染，特别对土壤、水体产生持久性的极高毒性；以三氯生、百菌清、异噻唑啉酮等有机抗微生物处理剂往往会对人体产生严重的健康影响。
铜离子广泛存在于人体、土壤和水体中，是一种安全环保的抗菌元素。但现有技术中由于铜离子的配合物具有颜色，无法直接作用于织物之上，并在纺织品上没有耐洗涤牢度，其使用受到非常大的限制。
发明内容
为了解决背景技术中存在的技术问题，本发明的发明目的是提供一种制备纺织品用抗微生物处理剂的方法，处理剂不含有重金属和可能具有毒性的氮、磷、硫等的有机元素，用于纺织品整理采用的碱性材料不包含非挥发性或有机胺化合物，巧妙地利用以醇类或糖类有机物做为催化剂，铜离子形成配合物过渡，使天然纺织品纤维与铜离子接枝的更牢固，具有安全、环保、耐擦洗和抗菌效力高、持续时间长的优点。
本发明的具体技术方案是一种制备纺织品用抗微生物处理剂的方法，其特征在于，包括以下步骤：
S1)提供以下溶液，
a)二价铜离子盐，
b)氨水或铵盐，
c)无机碱性水溶液，
d)仅含有碳、氢、氧元素的醇类或糖类有机物，
e)水；
S2)将上述溶液混合，陈化，以醇类或糖类为催化剂，形成铜铵配合物的复合物。
更进一步地，所述的铵盐为氯化铵、硝酸铵、硫酸铵、柠檬酸铵、醋酸铵中的一种或几种。
更进一步地，所述的无机碱性水溶液为碳酸钠、醋酸钠、氢氧化钠、氢氧化钾中的一种或几种的水溶液。
更进一步地，所述的醇类或糖类有机物为甲醇、乙醇、丙二醇、丙三醇、丁醇、聚乙二醇、葡萄糖、低聚糖、高聚糖中的一种或几种。
更进一步地，选用所述的复合物中的四种以上醇类或糖类有机物，来作为催化剂，形成二价铜离子与纺织品具有良好结合牢度的铜离子抗微生物处理剂。
更进一步地，所述的二价铜离子盐的硫酸铜，所述的无机碱性水溶液为氢氧化钠，所述的有机物为乙醇、丙三醇、丙二醇、聚乙二醇、葡萄糖，以下原料份数和百分比按重量计，纺织品为纤维素纤维织物、化纤、涤棉、锦纶、氨纶、腈纶、黏胶、天丝、蚕丝等纤维素织物、化纤织物、再生织物、蛋白质织物等，所述的抗微生物处理剂的原料包括50％硫酸铜水溶液10.1份，28％氢氧化铵2.9份，10％氢氧化钠水溶液0.1份，乙醇：0.3份，丙三醇：1份，丙二醇：3份，聚乙二醇：1份，葡萄糖：1.6，水80份。
本发明的方法的工作原理是：我们知道铜氨溶液能够与天然纤维素中的羟基发生配位配合反应，形成稳定的铜氨离子配合物纤维，具有一定的抗菌功能。织物上牢固结合的铜离子含量是织物抗菌性能的重要指标，但如果铜氨溶液浓度过高，将破坏织物纤维素的力学性能，本发明创造性采用了醇类或糖类的有机物与铜离子形成配合物进行过渡，在不破坏纤维素性能的前提下，使纤维素接枝的铜离子数量大大提高，可以在常温下对织物进行处理，处理过的织物不但具有很高的耐擦洗性，也具有很高的抗菌性能和持续时间。
本发明的有益效果是1)本发明的方法中用于整理或与铜离子形成过渡配合物的碱性铵通过冲洗不保留在纺织品上，原料仅包含碳、氢、氧三种元素，而不包含可能具有毒性的氮、磷、硫的有机元素，不包含可能具有毒性的银、汞、铅、砷、锡等金属元素，具有很高的安全性；2)不包含可能对环境造成影响的非挥发性或有机胺化合物，具有生物活性的金属离子仅包含环境友好的铜离子，而不包含其他具有生物活性的金属离子，具有无毒环保的特性；3)巧妙地利用含有醇类或糖类的有机物与铜离子形成配合物进行过渡，使天然纺织品纤维上铜离子接枝的更牢固，具有很好的耐擦洗和抗菌效力高、持续时间长；4)本发明的方法制备的抗微生物处理剂可以在常温下对织物进行处理，这是现有技术中没有的，无需复杂的处理工艺和条件，就能大幅提高铜离子的结合强度和密度含量。本发明的方法制备的抗微生物处理剂有很高的现场适用度，使用者能够相对简陋的条件环境下对织物进行处理；5)本发明的方法制备的抗微生物处理剂中氢氧化铵的浓度2.9％，并且采用丙三醇、丙二醇、乙醇、聚乙二醇、葡萄糖组合成催化剂能带来洗涤50次测试金黄色葡萄球菌的抑菌率和洗涤20次测试金黄色葡萄球菌的抑菌率都大于99％的效果。
具体实施方式
以下为本发明的一些实施例，除非另有指定，否则下文具体实施例中所阐述的所有分数和百分比均按重量计。
实施例一
硫酸铜(50％)：10.1份，氢氧化铵(28％)：2.9份，氢氧化钠水溶液(10％)：0.1份，乙醇：0.3份，丙三醇：1份，丙二醇：3份，聚乙二醇：1份，葡萄糖：1.6份，水：80份。
按以上配比制成硫酸铜、氢氧化铵、氢氧化钠、丙二醇、丙三醇、聚乙二醇试剂，将试剂分别溶解陈化10小时后，混合，保持30-35℃，搅拌，继续陈化24小时，获得抗微生物处理剂。其中，乙醇、丙三醇、丙二醇、聚乙二醇、葡萄糖的比例是0.3:1:3:1:1.6先预混合纯化1小时，得到醇类有机物，来做催化剂，很好地稳定铜离子，做一个过渡。
实施例二
硫酸铜(50％)：10.1份，氢氧化铵(28％):2.9份，氢氧化钠水溶液(10％)：0.1份，乙醇：3份，丙三醇：3份，丙二醇：4份，聚乙二醇：3份，葡萄糖：9.9份，水：64份。
按以上配比制成硫酸铜、氢氧化铵、氢氧化钠、丙二醇、丙三醇、聚乙二醇试剂，将试剂分别溶解陈化10小时后，混合，保持30-35℃，搅拌，继续陈化24小时，获得抗微生物处理剂。其中，乙醇、丙三醇、丙二醇、聚乙二醇、葡萄糖的比例是3:1:5:1:9.9。
实施例三
硫酸铜(50％)：10.1份，氢氧化铵(28％):2.9份，氢氧化钠水溶液(10％)：0.1份，乙醇：1.9份，丙三醇：3份，丙二醇：20份，聚乙二醇：3份，葡萄糖：10份，水：49份。
按以上配比制成硫酸铜、氢氧化铵、氢氧化钠、丙二醇、丙三醇、聚乙二醇试剂，将试剂分别溶解陈化10小时后，混合，保持30-35℃，搅拌，继续陈化24小时，获得抗微生物处理剂。其中，乙醇、丙三醇、丙二醇、聚乙二醇、葡萄糖的比例是1.9:3:20:3:10。
实施例四
硫酸铜(50％)：10.1份，氢氧化铵(28％):4.8份，氢氧化钠水溶液(10％)：0.1份，乙醇：2份，丙三醇：3份，丙二醇：13份，聚乙二醇：3份，葡萄糖：10份，水：54份。
硫酸铜、氢氧化铵、氢氧化钠、丙二醇、丙三醇、聚乙二醇，将试剂分别溶解陈化10小时后，混合，保持30-35℃，搅拌，继续陈化24小时，获得抗微生物处理剂。其中，乙醇、丙三醇、丙二醇、聚乙二醇、葡萄糖的比例是2:3:13:3:10。
用本发明的方法制备的抗微生物处理剂进行处理的纺织品为纤维素纤维织物、化纤、可再生纤维、黏胶等等。具体处理工艺有浸渍、浸轧、喷涂、涂层、泡沫涂层加工。1)浸渍：也可以叫浸泡，面料前处理、染色水洗完成，在常温或者40℃，将微生物处理剂加入到常温常压缸染缸，保持运行10分钟即可出缸、脱水、烘干；2)浸轧：面料染色、水洗、烘干后，通过一浸一轧的方法，在压力1.8-4公斤之间，把微生物处理剂均匀的带到织物上，通过定型，烘干，烘干温度100℃-150℃，让织物和微生物处理剂发生反应，完成织物的微生物处理剂的加工；3)喷涂：针对特殊产品，无法进行浸泡或者浸轧，只能采用喷涂的工艺，比如填充，采用雾化喷头，通过喷涂后，烘干，烘干温度100-150℃完成；4)涂层工艺：针对需要通过涂层工艺完成的制品，配置需要的量和涂层浆料一起，刮涂到织物表面，再通过烘干进行交联；5)泡沫涂层：泡沫涂层可以节省水的使用，采用发泡剂，抗微生物处理剂发泡成泡沫，再通过刮涂，烘干，烘干温度100℃-150℃完成，此工艺可以节省大量的水，减少能源的浪费。
以上4个实施例中，本发明方法制得的抗微生物处理剂中，当氢氧化铵的浓度增加，微生物处理剂和织物结合的耐洗牢度下降。采用不同氢氧化铵的浓度，其他保持不变，织物经过3％抗微生物处理剂处理后做洗涤，测试金黄色葡萄球菌的抑菌率，见下表：
Figure BDA0002774685630000061
另外，选用葡萄糖作为催化剂，有利于微生物处理剂和织物的耐洗涤牢度，选用不同或组合的催化剂，有利于微生物处理剂和织物结合的耐洗牢度，其他保持不变，织物经过微生物处理剂3％处理后做洗涤，测试金黄色葡萄球菌的抑菌率，见下表。
Figure BDA0002774685630000062
以下处理实例为本发明方法制得的抗微生物处理剂(实施例一)对各种织物的处理，并与现有技术中的处理剂处理织物性能进行的比较。
实例1：如对棉纱处理，浸渍工艺，在副缸里加入2％(o.w.f)的药剂，100公斤纱线需要2公斤抗菌剂。
Figure BDA0002774685630000071
实例2：袜子、棉针织面料、内衣、T恤面料采用浸渍工艺。在副缸里加入2％(o.w.f)的药剂，100公斤面料需要2公斤抗菌剂。常温加入(工厂常温一般在35℃-40℃)，保温10分钟。
本发明抗微生物处理剂
耐洗性(FZ/T73023) 洗涤50次
抑菌圈 0
50次洗后抗菌率(GB/T20944.3) 金葡大肠大于99.9％
实例3：毛巾采用浸渍工艺。在副缸里加入2％(o.w.f)的药剂，100公斤面料需要2公斤抗菌剂。常温加入(工厂常温一般在35℃-40℃)，保温10分钟。
Figure BDA0002774685630000072
实例4：家纺面料,如棉、黏胶、涤纶、尼龙等以及混纺面料采用浸轧工艺。面料添加量为2％(o.w.f)的药剂，计算轧液率后，来配置浓度，100公斤面料需要2公斤抗菌剂。通过浸轧工艺、烘干定型，完成。
本发明抗微生物处理剂
执行标准FZ/T73023-AAA 洗涤50次
抑菌圈 0
50次洗后抗菌率(GB/T20944.3) 金葡大肠大于99.9％
实例5：运动服面料，如棉、黏胶、涤纶、尼龙采用浸轧工艺。面料添加量为2％(o.w.f)的药剂，计算轧液率后，来配置浓度，100公斤面料需要2公斤抗菌剂。通过浸轧工艺、烘干定型，完成。
测试：洗涤50次后，抗菌率：金黄色葡萄球菌、大肠杆菌都为99％
实例6：工装面料采用浸轧工艺。如棉、黏胶、涤纶、尼龙采用浸轧工艺。面料添加量为2％(o.w.f)的药剂，计算轧液率后，来配置浓度，100公斤面料需要2公斤抗菌剂。通过浸轧工艺、烘干定型，完成。
测试：洗涤50次后，抗菌率：采用AATCC100-2019测试金黄色葡萄球菌、肺炎克雷伯都为99％
实例7：口罩针织面料采用浸轧工艺。在副缸里加入2％(o.w.f)的药剂，100公斤面料需要2公斤抗菌剂。常温加入(工厂常温一般在35℃-40℃)，保温10分钟。出缸、脱水、烘干，浸轧三防，完成抗菌加三防功能。
测试：抗菌效果：AATCC135洗涤30次后，抗菌率：采用AATCC100-2019测试金黄色葡萄球菌、肺炎克雷伯都为99％.
三防效果：防水洗前100分，30次洗后75分。油洗前5级，洗后3.5级。
此案例解决了以往抗菌和三防冲突引起的无法达到几万米的大生产工艺，同时缸里完成抗菌不增加工厂成本，以往抗菌加三防，需要定型两次，引起能源浪费，生产效率低的问题。
实例8：衬衫面料采用浸轧工艺。如棉、黏胶、涤纶、尼龙采用浸轧工艺。面料添加量为2％(o.w.f)的药剂，计算轧液率后，来配置浓度，100公斤面料需要2公斤抗菌剂。通过浸轧工艺、烘干定型，完成。
测试：洗涤50次后，抗菌率：采用AATCC100-2019测试金黄色葡萄球菌、肺炎克雷伯都为99％
此案例：衬衫白色偏多，以往采用银离子抗菌剂，面料在存储过程中容易黄变，三氯生抗菌剂存在安全性问题，有机硅季铵盐抗菌剂耐洗性达不到等问题。本发明抗微生物处理剂，处理完成后，储存颜色变化小，无抑菌剂，可以达到50次耐洗涤。
实例9：牛仔面料采用浸轧工艺。成分如棉、黏胶、涤纶、尼龙采用浸轧工艺。面料添加量为2％(o.w.f)的药剂，计算轧液率后，来配置浓度，100公斤面料需要2公斤抗菌剂。通过浸轧工艺、烘干定型，完成。还可以在牛仔纱线上浆时同时涂上抗微生物处理剂，和纱线浆料一起加入。
测试：洗涤50次后，抗菌率：采用ISO20743-2013测试金黄色葡萄球菌、肺炎克雷伯都为99％
此发明解决了，抗菌剂在纱线里碰到靛蓝染料和硫化染料时抗菌性能失效问题，同时解决了牛仔面料通过酵素洗涤后，抗菌剂80％掉落没有抗菌性问题。
实例10：纱布抹布面料。药剂的加入量为纱布的2％(o.w.f)，100公斤纱布面料需要2公斤抗菌剂。把淀粉浆煮熟后，直接把抗菌剂加入到煮熟的淀粉浆里，浸轧纱布，烘干，完成。
测试：洗涤50次后，抗菌率：采用FZ/T73023-AAA测试金黄色葡萄球菌、大肠杆菌、白色念珠菌都大于99％
此案例解决了以往抗菌剂无法与淀粉浆同浴使用，需要浸轧烘干两次，工艺成本增加较大，降低能源的损耗。
实例11：短纤填充，通过喷涂工艺，药剂的加入量为纱布的2％(o.w.f)，100公斤短纤需要2公斤抗菌剂。计算喷涂率，在配料槽里配置需要的药剂，100公斤短纤需要2公斤抗菌剂。喷涂、烘干。
实例12：棉纤维染色。在染缸的副缸里加入2％(o.w.f)的药剂，100公斤纤维需要2公斤抗菌剂。常温加入(工厂常温一般在35℃-40℃)，保温10分钟。
洗涤50次后，抗菌率：采用FZ/T73023-AAA测试金黄色葡萄球菌、大肠杆菌、白色念珠菌均大于99％。
此案例解决了棉纤维抗菌问题，以往抗菌在纤维里完成容易失效，抗菌不稳定，只能采用涤棉混纺，在涤纶纤维里完成抗菌，棉纤维不做抗菌，此发明可以用100％的处理好的抗菌纤维或者参入50％未抗菌纤维，能达到很好的抗菌性能，从纤维开始处理降低了面料进入染厂，纤维完成后既可以纺纱制造各种成品，节约了运输，同时降低了能源。
实例13：户外服装里的摇粒绒面料。在副缸里加入2％(o.w.f)的药剂，100公斤面料需要2公斤抗菌剂。常温加入(工厂常温一般在35℃-40℃)，保温10分钟。
本发明抗微生物处理剂
10次洗涤后 AATCC100-2019金葡大肠为99.9％
此案例，以往抗菌剂只能使用浸轧工艺，导致太厚的摇粒绒面料很难烘干，需要使用两倍以上的能源才能完成。同时解决了一部分摇粒绒面料工厂烘干设备上没有料槽，无法完成功能附加。
虽然本发明已经以较佳实施例公开如上，但实施例并不是用来限定本发明的。在不脱离本发明之精神和范围内，所做的任何等效变化或润饰，同样属于本发明之保护范围。因此本发明的保护范围应当以本申请的权利要求所界定的内容为标准。

Claims (1)

1.一种制备纺织品用抗微生物处理剂的方法，其特征在于，包括以下步骤：
S1）提供以下溶液，
a）二价铜离子盐，
b）氢氧化铵，
c）无机碱性水溶液，
d）仅含有碳、氢、氧元素的醇类和糖类有机物，
e）水；
S2）将上述溶液混合，陈化，以仅含有碳、氢、氧元素的醇类和糖类有机物为催化剂，形成铜铵配合物的复合物；
其中，纺织品为纤维素织物、涤纶、尼龙或蛋白质织物，所述的二价铜离子盐为硫酸铜，所述的无机碱性水溶液为氢氧化钠，所述的仅含有碳、氢、氧元素的醇类有机物为乙醇、丙三醇、丙二醇和聚乙二醇，所述的仅含有碳、氢、氧元素的糖类有机物为葡萄糖，以下原料份数和百分比按重量计：所述的抗微生物处理剂的原料为：50%硫酸铜10.1份，28%氢氧化铵2.9份，10%氢氧化钠水溶液0.1份，乙醇0.3份，丙三醇1份，丙二醇3份，聚乙二醇1份，葡萄糖1.6份，水80份；或为50%硫酸铜10.1份，28%氢氧化铵2.9份，10%氢氧化钠水溶液0.1份，乙醇1.9份，丙三醇3份，丙二醇20份，聚乙二醇3份，葡萄糖10份，水49份；或为50%硫酸铜10.1份，28%氢氧化铵4.8份，10%氢氧化钠水溶液0.1份，乙醇2份，丙三醇3份，丙二醇13份，聚乙二醇3份，葡萄糖10份，水54份。
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