CN108385368A - 一种纳米二氧化钛有机无机杂化抗紫外整理剂的制备方法及其应用 - Google Patents
一种纳米二氧化钛有机无机杂化抗紫外整理剂的制备方法及其应用 Download PDFInfo
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Abstract
本申请提供了一种基于纳米二氧化钛的有机无机杂化抗紫外整理剂的制备方法:将无水乙醇和去离子水混合,调节溶液pH值至8‑9,加入金红石型纳米二氧化钛,经超声分散后,滴入γ‑(甲基丙烯酰氧)丙基三甲氧基硅烷(KH570)的乙醇溶液,在室温下搅拌反应;反应结束后,用乙醇洗沉淀物三次并高速离心,烘干;得到KH570‑TiO2杂化的抗紫外整理剂。本申请将单体整理到涤纶织物上,并采取了传统的轧烘焙工艺(PDC)和电子束辐射工艺(EB)两种整理手段,可制备出具有优异抗紫外性能的纺织品。
Description
技术领域
本发明涉及抗紫外整理纺织品技术领域,尤其是涉及一种基于纳米二氧化钛有机无机杂化抗紫外整理剂的制备方法及其在涤纶织物中的应用。
背景技术
当今世界经济日益发展,人们生活质量水平逐渐提高,伴随而来的环境污染问题日益严重。涤纶作为合成纤维的一大分支,具有举足轻重的地位。长期的紫外线照射,会使织物变黄,如何提高织物的抗紫外能力就显得十分重要了。
近年来纳米科技迅速发展,人们对于纳米TiO2的研究及其应用的兴趣也增加了,尤其是对较常规TiO2具有极高的吸收和屏蔽紫外光能力、较高的折射率(2.6-2.9)、良好的透明性等优异性能的金红石型纳米TiO2。利用现代科技研制出的纳米TiO2,粒径较小,只有10-50nm,对波长为200-400nm的UVA和UVB紫外线有很好的屏蔽作用,且亲水性较好、安全无毒、化学稳定性较高。目前,抗紫外技术主要有两大类,有机类紫外吸收剂的吸收作用和无机类紫外整理剂的遮盖作用,一类是对紫外线具有较强反射作用而达到屏蔽紫外线效果的无机涂料,如二氧化钛,一类是对紫外线具有吸收作用的紫外线吸收剂,如苯并***类。
纳米TiO2是一种传统的无机型紫外整理剂,具有环保、无毒副作用、稳定性好、抗紫外线能力强、耐化学腐蚀性强等优点,被广泛地应用于工业、纺织、医学等领域。由于二氧化钛折光性和光活性比较高的特点,是防晒剂的良好选择。但纳米TiO2的比表面能大、极性强、难以分散、易团聚等缺点,影响了它的实际应用效果。涤纶纤维分子结构比较规整紧密,但是大分子中缺乏亲水性的基团,只有两个端醇羟基,所以导致其亲水性差,而TiO2虽有亲水性,但是吸湿性不强,故而用纳米TiO2对涤纶织物改性存在一定的困难。
CN106496562A提供了一种有机硅-二氧化钛杂化微球的制备方法及应用。这种微球主要是利用钛原子和有机硅之间的化学键连接,采用的是钛酸酯与有机硅氧烷单体的水解-缩聚反应,而本发明是利用二氧化钛表面水化出羟基,然后和KH570表面羟基形成氢键连接。但是该杂化微球需要控制其粒径大小和粒径分布等参数,具有一定的难度。
CN102134447A提供了一种端甲基丙烯酰氧基倍半硅氧烷/二氧化钛纳米防腐保护膜。该防腐保护膜采用的是溶胶-凝胶法,将原料混合进行水解缩合制备的,但是对于不同大小的着膜物需要采取不同的整理方式,比较复杂,不具有普适性。
鉴于此,研究出一种基于纳米二氧化钛有机无机杂化抗紫外整理剂和兼具有优良抗紫外性能、良好抗老化性能的抗紫外功能纺织品,具有十分重要的意义。
发明内容
针对现有技术存在的上述问题,本申请提供了一种纳米二氧化钛有机无机杂化抗紫外整理剂的制备方法及其应用。本发明原料廉价易得、每一流程产物产量都较高,由该法合成的抗紫外整理剂屏蔽紫外线的能力比强、稳定性高、毒性低,可制备出具有优异抗紫外性能的涤纶纺织品。
本发明的技术方案如下:
本申请提供了一种KH570-TiO2杂化的抗紫外整理剂,所述杂化的抗紫外整理剂为式(I)所示结构的化合物:
本申请还提供了一种权利要求1所述的杂化的紫外整理剂的制备方法,具体步骤如下:
将无水乙醇和去离子水混合,调节溶液pH值至8-9,加入金红石型纳米二氧化钛,经超声分散后,滴入γ-(甲基丙烯酰氧)丙基三甲氧基硅烷即KH570的乙醇溶液,在室温下搅拌反应10~13个小时.反应结束后,用乙醇洗沉淀物并高速离心,烘干,即得到KH570-TiO2杂化的抗紫外整理剂。
优选的,加入KH570的乙醇溶液时,边搅拌边缓慢地滴加。
本申请还提供了所述的紫外整理剂在制备抗紫外涤纶织物中的应用,采用轧烘焙工艺,具体步骤为:
用丙酮溶液将涤纶织物洗涤烘干并称取重量,引发剂BPO和抗紫外整理剂在室温条件下,用无水乙醇溶液溶解,浴比1:30,二浸二轧,轧余率100%,先在65~70℃条件下预烘5~8min,后在120~130℃条件下焙烘3~5min,用无水乙醇溶液充分洗涤,烘干至恒重,制得抗紫外涤纶织物。
本申请还提供了另一种所述的紫外整理剂在制备抗紫外涤纶织物中的应用,采用电子束辐射工艺,具体步骤为:
用丙酮溶液将涤纶织物洗涤烘干并称取重量,紫外整理剂在室温条件下,用无水乙醇溶液溶解,浴比1:30,二浸二轧,轧余率100%,在电子束控制***的辐照室中辐射后取出焙烘,用无水乙醇溶液充分洗涤烘干至恒重,制得抗紫外涤纶织物。优选的,辐射量大小为32.5、65、130、195、260kGy。
上述步骤中,加入纳米二氧化钛之后,需要超声分散,分散成均一稳定的乳浊液。水与乙醇混合之后需要调节溶液的pH值。向烧瓶中加入硅烷偶联剂KH570的乙醇溶液时,需要搅拌并且尽可能缓慢的滴加,防止KH570加入量过多时,形成多层包覆或者KH570水解自聚。反应后需要对产物进行清洗。
上述轧烘焙工艺处理需要预烘,先提供一定的能量使引发剂BPO产生自由基,与织物和单体自由基焙烘过程完成接枝反应。
处理之后的织物应该尽快清洗焙烘,使反应更加稳固。
本申请所述浴比是指织物与染液的质量比。
本发明有益的技术效果在于:
本发明制备得到的抗紫外涤纶纺织品在紫外线照射的条件下,二氧化钛会吸收近紫外光波,价电子激发至导带,产生空穴和自由电子。TiO2和水作用在其表面形成大量的羟基,这些羟基可以捕获空穴,而自由电子可以结合氧气产生能将周围的细菌与病毒杀死的超氧自由基由该法合成的紫外屏蔽剂,对于紫外线的屏蔽效果非常好,比原涤纶织物的UPF值提高了3-5倍。
本发明在制备过程中使用的原料常见,可以极大程度地节约生产成本;本发明方法仅需一步合成单体,过程简单,耗时耗能少,产率高,制备简便。通过本发明应用工艺制得的抗紫外纺织品具有优异的抗紫外性能,抗紫外效率高,UPF值由原涤纶的45分别上升到202、141。
附图说明
图1为本发明制备方法的原理示意图。
图2为引发剂BPO浓度一定时,不同的抗紫外整理剂浓度条件下按照应用例1所述轧烘焙工艺进行抗紫外整理的测试结果。
图3为抗紫外整理剂终浓度为15%时,不同的BPO终浓度条件下按照应用例1所述轧烘焙工艺进行抗紫外整理的测试结果。
图4为抗紫外整理剂浓度一定时,不同的辐射量条件下按照应用例3所述电子束工艺进行抗紫外整理的测试结果。
图5为辐射量为130kGy时,不同的抗紫外整理剂浓度条件下按照应用例3所述电子束工艺进行抗紫外整理的测试结果。
具体实施方式
下面结合附图和实施例,对本发明进行具体描述。
实施例1:
将90mL无水乙醇和10mL去离子水在250mL烧杯中混合,用pH计调节溶液pH值至8,加入10g的金红石型纳米二氧化钛,经超声分散后倒入250mL平底烧瓶中,滴入2g的γ-(甲基丙烯酰氧)丙基三甲氧基硅烷(KH570)的乙醇(10mL)溶液,在室温下搅拌反应11个小时.反应结束后,用乙醇洗沉淀物三次并高速离心,置于干燥箱中烘干,得白色产物8.04g,收率80.40%。
实施例2:
将95mL无水乙醇和10mL去离子水在250mL烧杯中混合,用pH计调节溶液pH值至8.5,加入9g的金红石型纳米二氧化钛,经超声分散后倒入250mL平底烧瓶中,滴入3g的γ-(甲基丙烯酰氧)丙基三甲氧基硅烷(KH570)的乙醇(5mL)溶液,在室温下搅拌反应12个小时.反应结束后,用乙醇洗沉淀物三次并高速离心,置于干燥箱中烘干,得白色产物8.04g,收率82.35%。
实施例3:
将100mL无水乙醇和10mL去离子水在250mL烧杯中混合,用pH计调节溶液pH值至9,加入8g的金红石型纳米二氧化钛,经超声分散后倒入250mL平底烧瓶中,滴入4g的γ-(甲基丙烯酰氧)丙基三甲氧基硅烷(KH570)溶液,在室温下搅拌反应13个小时.反应结束后,用乙醇洗沉淀物三次并高速离心,置于干燥箱中烘干,得白色产物8.04g,收率81.60%。
应用例1:
用丙酮溶液将用涤纶布洗涤烘干并称取重量,引发剂(BPO)和实施例1制得的抗紫外整理剂在室温条件下,用无水乙醇溶液溶解,浴比1:30,二浸二轧,轧余率100%,先在70℃条件下预烘5min,后在130℃条件下焙烘3min,用无水乙醇溶液充分洗涤,烘干至恒重,制得抗紫外涤纶织物,测得其UPF值为202。
应用例2:
用丙酮溶液将用涤纶布洗涤烘干并称取重量,引发剂(BPO)和实施例1制得的抗紫外整理剂在室温条件下,用无水乙醇溶液溶解,浴比1:30,二浸二轧,轧余率100%,先在60℃条件下预烘5min,后在120℃条件下焙烘5min,用无水乙醇溶液充分洗涤,烘干至恒重,制得抗紫外涤纶织物,测得其UPF值为198。
应用例3:
用丙酮溶液将涤纶布洗涤烘干并称取重量,实施例1制得的抗紫外整理剂在室温条件下,用无水乙醇溶液溶解,浴比1:30,二浸二轧,轧余率100%,在电子束控制***的辐照室中辐射后取出在130℃条件下焙烘3min,用无水乙醇溶液充分洗涤烘干至恒重,制得抗紫外涤纶织物,测得其UPF值为141。
应用例4:
用丙酮溶液将涤纶布洗涤烘干并称取重量,实施例1制得的抗紫外整理剂在室温条件下,用无水乙醇溶液溶解,浴比1:30,二浸二轧,轧余率100%,在电子束控制***的辐照室中辐射后取出在120℃条件下焙烘5min,用无水乙醇溶液充分洗涤烘干至恒重,制得抗紫外涤纶织物,测得其UPF值为137。
测试例1:整理后涤纶织物抗紫外性能
图2为引发剂BPO浓度一定时,不同的抗紫外整理剂浓度条件下按照应用例1所述轧烘焙工艺进行抗紫外整理的测试结果。图3为抗紫外整理剂终浓度为15%时,不同的BPO终浓度条件下按照应用例1所述轧烘焙工艺进行抗紫外整理的测试结果。
图2和图3表明,本发明所制得的抗紫外涤纶织物具有优良的抗紫外性能,紫外吸收性能比较好;用15%的抗紫外整理剂和2%浓度的引发剂BPO整理的涤纶织物UPF值可以达到202。
图4为抗紫外整理剂浓度一定时,不同的辐射量条件下按照应用例3所述电子束工艺进行抗紫外整理的测试结果。图5为辐射量为130kGy时,不同的抗紫外整理剂浓度条件下按照应用例3所述电子束工艺进行抗紫外整理的测试结果。
图4和图5表明,本发明所制得的抗紫外涤纶织物具有优良的抗紫外性能,紫外吸收性能比较好;用终浓度12%的抗紫外整理剂和130kGy的辐射量整理的涤纶织物UPF值可以达到141。
测试例2:抗紫外整理对织物强力的影响
参考标准GB/T 3923-1997《织物的断裂强力和伸长率的测试》,用强力测试仪测试原涤纶织物、应用例1和应用例3改性整理过的涤纶织物经纬向各3块,统一裁剪成长约15cm、宽约6cm的长方形,扯去边纱使之成为5cm,测试结果参见表1。
表1不同老化时间条件下织物的强力
表1的测试数据表明,较原涤纶织物,改性整理过的涤纶织物的经向断裂强力损失约1%,纬向断裂强力损失约为2%,经过24h紫外光照射以后,原涤纶织物的经向断裂强力损失约14%左右,纬向断裂强力损失约为22%,经过24h紫外光照射以后,改性整理过的涤纶织物的经向断裂强力损失约10%,纬向断裂强力损失约为18%,这说明经过改性整理的涤纶织物具有一定的抗紫外性能。且改性整理的织物的经纬向强力损失不大,可见此种工艺并不影响织物的正常使用。
测试例3:抗紫外稳定性测试
将应用例1制备得到的抗紫外涤纶织物保存起来,间隔特定时间测试一次UPF值,结果如表2所示。
表2抗紫外效果随保存时间的变化
从表2的数据可以看到,本发明制备得到的抗紫外涤纶的稳定性好,克服了以往处理方法获得的抗紫外涤纶容易变性、快速失去抗紫外能力的缺陷。
Claims (6)
1.一种KH570-TiO2杂化的抗紫外整理剂,其特征在于所述杂化的抗紫外整理剂为式(I)所示结构的化合物:
2.一种权利要求1所述的杂化抗紫外整理剂的制备方法,其特征在于具体步骤如下:
将无水乙醇和去离子水混合,调节溶液pH值至8-9,加入金红石型纳米二氧化钛,经超声分散后,滴入γ-(甲基丙烯酰氧)丙基三甲氧基硅烷即KH570的乙醇溶液,在室温下搅拌反应10~13个小时.反应结束后,用乙醇洗沉淀物并高速离心,烘干,即得到KH570-TiO2杂化的抗紫外整理剂。
3.根据权利要求2所述的制备方法,其特征在于:加入KH570的乙醇溶液时,边搅拌边缓慢地滴加。
4.权利要求1或2所述的杂化的抗紫外整理剂在制备抗紫外涤纶织物中的应用,其特征在于采用轧烘焙工艺,具体步骤为:
用丙酮溶液将涤纶织物洗涤烘干,引发剂BPO和杂化的抗紫外整理剂在室温条件下,用无水乙醇溶液溶解,浴比1:30,二浸二轧,轧余率100%,先在65~70℃条件下预烘5~8min,后在120~130℃条件下焙烘3~5min,用无水乙醇溶液充分洗涤,烘干至恒重,制得抗紫外涤纶织物。
5.权利要求1或2所述的杂化的抗紫外整理剂在制备抗紫外涤纶织物中的应用,其特征在于采用电子束辐射工艺,具体步骤为:
用丙酮溶液将涤纶织物洗涤烘干,杂化的抗紫外整理剂在室温条件下,用无水乙醇溶液溶解,浴比1:30,二浸二轧,轧余率100%,在电子束控制***的辐照室中辐射后取出焙烘,用无水乙醇溶液充分洗涤烘干至恒重,制得抗紫外涤纶织物。
6.根据权利要求5所述的整理方法,其特征在于:辐射量大小为32.5、65、130、195、260kGy。
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