CN111350077B - 一种黄变消除剂、其制备方法及防水织物 - Google Patents

一种黄变消除剂、其制备方法及防水织物 Download PDF

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CN111350077B
CN111350077B CN202010326259.0A CN202010326259A CN111350077B CN 111350077 B CN111350077 B CN 111350077B CN 202010326259 A CN202010326259 A CN 202010326259A CN 111350077 B CN111350077 B CN 111350077B
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CN111350077A (zh
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董锋
周宁
方华玉
李天源
卓丽琼
托马斯·沃尔特施密特
姜兴盛
林胜尧
张俊峰
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Putian Dakai New Materials Co ltd
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Abstract

本发明提供的一种不含硅和氟的防水剂及其制备方式，所述交联剂包括以下质量份的组分：15‑30质量份甲基氯丙烯、20‑35质量份氰酸钠、10‑40质量份三羟甲基丙烷，1‑30质量份丙烯酸，所述交联剂的pH值为7‑8。该交联剂配合防水剂，可以提高防水剂的耐洗度，增加防水织物的使用寿命，生产工艺简单，造价低，可大规模应用于工业化生产中。

Description

一种黄变消除剂、其制备方法及防水织物
技术领域
本发明涉及纺织领域，特别涉及一种黄变消除剂、其制备方法及防水织物。
背景技术
全氟辛烷磺酰基化合物(PFOS)和全氟辛酸(PFOA)是C8防水剂中存在的痕量物质，具有难降解、生物累积性及多种毒性，且具备所有持久性有机污染物的共同特性,因而受到严格的限制。对于纺织行业，PFOA与PFOS主要存在于含氟防水防油整理剂处理的织物中。
因此，我司研发了有机硅无氟防水剂，但是在研究中发现有机硅无氟防水剂在经过使用一段时间后，会发生织物色光变化，织物会出现泛黄的情况，影响织物的使用寿命。
发明内容
鉴于背景技术所述的问题，本发明的目的在于提供了一种黄变消除剂、其制备方法及防水织物。该黄变消除剂可以和有机硅无氟防水剂配合使用，降低织物的泛黄情况，提高织物的耐黄变等级。
为达到上述目的，在本发明的第一方面，发明人提供了一种黄变消除剂，所述黄变消除剂的制备包括以下步骤：
向反应釜中投入10-15质量份的醇酯类化合物和1-5质量份的纳米氧化物，80-100℃反应1h后，降温至45-50℃保温1-2h；继续向反应釜中加入加入5-10质量份的酚类抗氧化剂，在80-95℃反应1-2小时后，反应釜降温到40-50℃后再加入2-5质量份的亚磷酸酯，在80-95℃反应1-6小时；最后加入有机溶剂，得到乳化液，调节乳化液的pH值至5-7，得到黄变消除剂。
在本发明的第二方面，发明人提供了一种黄变消除剂，所述黄变消除剂由本发明第一方面所提供方法进行制备。
在本发明的第三方面，发明人提供了一种防水织物，所述防水织物用有机硅无氟防水剂和本发明第一方面所提供的黄变消除剂进行防水处理。
区别于现有技术，本发明至少包括如下所述的有益效果：本发明提供的一种黄变消除剂及其制备方式及防水织物。该黄变消除剂可以和有机硅无氟防水剂配合使用，降低织物的泛黄情况，提高织物的耐黄变等级；对纺织品进行抗黄变处理的同时，不影响纺织品的手感，颜色等。同时，该黄变消除剂的生产工艺简单，造价低，可大规模应用于工业化生产中。
具体实施方式
为详细说明技术方案的技术内容、构造特征、所实现目的及效果，以下结合具体实施例详予说明。
首先说明本发明第一方面的一种黄变消除剂，所述黄变消除剂的制备包括以下步骤：
向反应釜中投入10-15质量份的醇酯类化合物、1-5质量份的纳米氧化物和水，80-100℃反应1h后，降温至45-50℃保温1-2h；继续向反应釜中加入5-10质量份的酚类抗氧化剂，在80-95℃反应1-2小时后，反应釜降温到40-50℃后再加入2-5质量份的亚磷酸酯，在80-95℃反应1-6小时；最后加入有机溶剂，得到乳化液，调节乳化液的pH值至5-7，得到黄变消除剂。
发明人在研究中发现，醇酯类化合物、酚类抗氧化剂的配比会影响黄变消除剂的去黄效果。
酚类抗氧剂是一类在苯环上羟基(-OH)的一侧或两侧有取代基的化合物。由于-OH受到空间障碍，H原子容易从分子上脱落下来，与过氧化自由基(ROO-)、烷氧自由基(RO-)、羟自由基(-OH)等结合使之失去活性，从而使热氧老化的链反应终止。
优选的，所述醇酯类化合物包括聚己内酯二元醇和聚己二酸乙二醇酯；所述聚己内酯二元醇和聚己二酸乙二醇酯的质量比为6-7:4-6。
优选的，所述纳米氧化物的直径为100nm以内，所述纳米氧化物包括纳米氧化锌、纳米氧化铝，所述纳米氧化锌、纳米氧化铝的质量比为4-5：5-6。
优选的，所述有机溶剂为乙醇，乙醇的加入量为10-15g/L交联剂。
优选的，用pH调节剂调节乳化液的pH值，所述pH调节助剂包括柠檬酸、氢氧化钠、柠檬酸钠。
其次，说明本发明第二方面的一种黄变消除剂，由本发明第一方面的制备方法进行制备。
再次，说明本发明第三方面的一种防水织物，所述防水织物用有机硅无氟防水剂和本发明第二方面所提供的黄变消除剂进行防水处理；所述有机硅无氟防水剂包括以下质量份的组分：60-70质量份有机硅聚合物、1-10质量份交联混合物、1-5质量份表面活性剂；所述有机硅聚合物包括氨基硅烷和改性硅油，所述氨基硅烷与改性硅油的质量比为50-60:40-50；所述交联混合物包括丙烯酸和环氧硅烷，所述丙烯酸与环氧硅烷的质量比为30-60:40-70；所述有机硅无氟防水剂的pH值为5-7。
一种有机硅无氟防水剂的制备方法，包括以下步骤：
先将水投入反应釜中，再向反应釜中依次投入60-70质量份有机硅聚合物、1-10质量份交联混合物、1-5质量份表面活性剂，搅拌乳化，得到乳状液；调节乳状液的温度至55-70℃，加入乙醇助溶、调节乳状液的pH值至5-7，70-80℃保温2-3h，得到有机硅无氟防水剂；
所述有机硅聚合物包括氨丙基三乙氧基硅烷和羧基硅油，所述氨丙基三乙氧基硅烷和羧基硅油的质量比为50-60:40-50；所述交联混合物包括丙烯酸和乙烯基三乙氧基硅烷，所述丙烯酸和乙烯基三乙氧基硅烷的质量比为30-60:40-70；所述表面活性剂包括AEO-9、AEO-1303和AEO-1307，所述AEO-9、AEO-1303、AEO-1307的质量比为2:1:1；乙醇的加入量为10-15g/L非硅无氟防水剂。
本发明的黄变消除剂配合有机硅防水剂混合后，可与织物紧密结合，不影响纺织品的手感，颜色和防水性能。
实施例1一种黄变消除剂：
向反应釜中投入12kg的醇酯类化合物(聚己内酯二元醇7kg、聚己二酸乙二醇酯5kg)、4kg的纳米氧化物(纳米氧化锌2kg、纳米氧化铝2kg)和70kg的水，80℃反应1h后，降温至50℃保温2h；继续向反应釜中加入6kg的酚类抗氧化剂，在80℃反应1小时后，反应釜降温到40℃后再加入4kg的亚磷酸酯，在80℃反应3小时；最后加入乙醇(乙醇加入量为15g/L黄变消除剂)，得到乳化液，调节乳化液的pH值至7，得到黄变消除剂。
实施例2一种黄变消除剂：
向反应釜中投入12kg的醇酯类化合物(聚己内酯二元醇7kg、聚己二酸乙二醇酯5kg)、4kg的纳米氧化物(纳米氧化锌2kg、纳米氧化铝2kg)和70kg的水，90-95℃反应1h后，降温至45-50℃保温1-2h；继续向反应釜中加入3kg的酚类抗氧化剂，在90-95℃反应1小时后，反应釜降温到40-45℃后再加入2kg的亚磷酸酯，在90-95℃反应3小时；最后加入乙醇(乙醇加入量为15g/L黄变消除剂)，得到乳化液，调节乳化液的pH值至7，得到黄变消除剂。
实施例3一种黄变消除剂：
向反应釜中投入10kg的醇酯类化合物(聚己内酯二元醇6kg、聚己二酸乙二醇酯4kg)、1kg的纳米氧化物(纳米氧化锌0.4kg、纳米氧化铝0.6kg)和70kg的水，90-95℃反应1h后，降温至45-50℃保温1-2h；继续向反应釜中加入5kg的酚类抗氧化剂，在90-95℃反应1小时后，反应釜降温到40-45℃后再加入2kg的亚磷酸酯，在90-95℃反应3小时；最后加入乙醇(乙醇加入量为10g/L黄变消除剂)，得到乳化液，调节乳化液的pH值至7，得到黄变消除剂。
实施例4一种黄变消除剂：
向反应釜中投入15kg的醇酯类化合物(聚己内酯二元醇8kg、聚己二酸乙二醇酯7kg)、1kg的纳米氧化物(纳米氧化锌0.4kg、纳米氧化铝0.6kg)和70kg的水，90-95℃反应1h后，降温至45-50℃保温1-2h；继续向反应釜中加入10kg的酚类抗氧化剂，在90-95℃反应2小时后，反应釜降温到40-45℃后再加入5kg的亚磷酸酯，在90-95℃反应3小时；最后加入乙醇(乙醇加入量为10g/L黄变消除剂)，得到乳化液，调节乳化液的pH值至5，得到黄变消除剂。
对比例1一种黄变消除剂
向反应釜中投入6kg的醇酯类化合物(聚己内酯二元醇3kg、聚己二酸乙二醇酯3kg)、4kg的纳米氧化物(纳米氧化锌2kg、纳米氧化铝2kg)和70kg的水，80℃反应1h后，降温至50℃保温2h；继续向反应釜中加入12kg的酚类抗氧化剂，在80℃反应1小时后，反应釜降温到40℃后再加入4kg的亚磷酸酯，在80℃反应3小时；最后加入乙醇(乙醇加入量为15g/L黄变消除剂)，得到乳化液，调节乳化液的pH值至7，得到黄变消除剂。
对比例2一种黄变消除剂
向反应釜中投入18kg的醇酯类化合物(聚己内酯二元醇10kg、聚己二酸乙二醇酯8kg)、4kg的纳米氧化物(纳米氧化锌2kg、纳米氧化铝2kg)和70kg的水，80℃反应1h后，降温至50℃保温2h；继续向反应釜中加入4kg的酚类抗氧化剂，在80℃反应1小时后，反应釜降温到40℃后再加入4kg的亚磷酸酯，在80℃反应3小时；最后加入乙醇(乙醇加入量为15g/L黄变消除剂)，得到乳化液，调节乳化液的pH值至7，得到黄变消除剂。
实施例1-2和对比实施例1-2参与防水织物的制备，包括以下步骤：
工作液配制：将实施例和对比实施例所配制的黄变消除剂稀释为浓度5-10g/L的工作液，和浓度为10-40g/L(含水量不同)的有机硅无氟防水剂混合，得到工作液；
一浸一轧：将化纤织物浸泡于工作液中20-100s后用轧车扎一次，所述轧车压力为1-3Kg/cm2,带液率为75-100％，
烘干：将一浸一轧后的织物在150-180℃烘45-120秒，得到防黄变防水织物。
有机硅无氟防水剂的制备：先将600kg水投入反应釜中，再向反应釜中依次投入150kg份有机硅聚合物(氨丙基三乙氧基硅烷8kg，羧基硅油70kg)、40kg交联剂、(丙烯酸20kg，乙烯基三乙氧基硅烷20kg)20kg表面活性剂(AEO-9:1303:1307＝2:1:1)，搅拌乳化，得到乳状液；调节乳状液的温度至60℃，加入15g/L乳状液的乙醇，调节乳状液的pH值至6，80℃保温2h，得到有机硅无氟防水剂。
将实施例1-2黄变消除剂分别配合上述配置的非硅无氟防水剂和有机硅无氟防水剂，所制备的防水织物和对比实施例1-2配合相同防水剂、相同工艺所制备的防水织物，与未经处理的化纤织物按照GB250-1995标准对纺织品耐黄变等级进行测试：试样在紫外光下照射一定时间后，与未经照射的样品进行对比，用评定变色用灰色样卡评定变色程度，从而判定纺织材料在紫外光线照射下耐光黄变的能力，对测试后的织物进行评级结果如下表所述：
编号 空白 实施例1 实施例2 对比例1 对比例2
耐黄变等级 1 5 5 3 3
实施例1-2黄变消除剂处理过的织物的耐黄变等级达到5级，明显高于对比例。醇酯类化合物、酚类抗氧化剂的配比会影响黄边消除剂的去黄效果。
同时，本发明的黄变消除剂配合防水剂可与织物紧密结合，不影响纺织品的手感，颜色和防水性能，在紫外光下不易氧化变色。
需要说明的是，在本文中，诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来，而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且，术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含，从而使得包括一系列要素的过程、方法、物品或者终端设备不仅包括那些要素，而且还包括没有明确列出的其他要素，或者是还包括为这种过程、方法、物品或者终端设备所固有的要素。在没有更多限制的情况下，由语句“包括……”或“包含……”限定的要素，并不排除在包括所述要素的过程、方法、物品或者终端设备中还存在另外的要素。此外，在本文中，“大于”、“小于”、“超过”等理解为不包括本数；“以上”、“以下”、“以内”等理解为包括本数。
需要说明的是，尽管在本文中已经对上述各实施例进行了描述，但并非因此限制本发明的专利保护范围。因此，基于本发明的创新理念，对本文所述实施例进行的变更和修改，或利用本发明说明书内容所作的等效结构或等效流程变换，直接或间接地将以上技术方案运用在其他相关的技术领域，均包括在本发明的专利保护范围之内。

Claims (4)

1.一种黄变消除剂的制备方法，其特征在于，所述黄变消除剂的制备包括以下步骤：
向反应釜中投入10-15质量份的醇酯类化合物、1-5质量份的纳米氧化物和水，80-100℃ 反应1h后，降温至45-50℃保温1-2h；继续向反应釜中加入5-10质量份的酚类抗氧化剂，在80-95℃反应1-2小时后，反应釜降温到40-50℃后再加入2-5质量份的亚磷酸酯，在80-95℃反应1-6小时；最后加入有机溶剂，得到乳化液，调节乳化液的pH值至5-7，得到黄变消除剂;
所述醇酯类化合物包括聚己内酯二元醇和聚己二酸乙二醇酯；所述聚己内酯二元醇和聚己二酸乙二醇酯的质量比为6-7:4-6;
所述纳米氧化物的直径为100nm以内，所述纳米氧化物包括纳米氧化锌、纳米氧化铝，所述纳米氧化锌、纳米氧化铝的质量比为4-5：5-6；
所述有机溶剂为乙醇，乙醇的加入量为10-15g/L黄变消除剂；
用pH调节剂调节乳化液的pH值，所述pH调节剂包括柠檬酸、氢氧化钠、柠檬酸钠；
所述黄变消除剂和有机硅无氟防水剂配合使用；
所述有机硅无氟防水剂包括以下质量份的组分：60-70质量份有机硅聚合物、1-10质量份交联混合物、1-5质量份表面活性剂；所述有机硅聚合物包括氨基硅烷和改性硅油，所述氨基硅烷与改性硅油的质量比为50-60:40-50；所述交联混合物包括丙烯酸和环氧硅烷，所述丙烯酸与环氧硅烷的质量比为30-60:40-70；所述有机硅无氟防水剂的pH值为5-7。
2.一种黄变消除剂，其特征在于，所述黄变消除剂由权利要求1所述制备方法进行制备。
3.一种防水织物，其特征在于，所述防水织物用权利要求1所述的有机硅无氟防水剂和权利要求2所述的黄变消除剂进行防水处理。
4.根据权利要求3所述的防水织物，其特征在于，所述防水织物为化纤织物。
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