CN108035148B - 一种氨基改性TiO2皮革纤维的制备方法 - Google Patents
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Abstract
本发明提供了一种氨基改性TiO2皮革纤维的制备方法,先利用硅烷偶联剂对TiO2进行表面化学修饰,使TiO2表面带有氨基,再利用氯乙酸钠对皮革纤维进行羧基化,使得皮革纤维具有更多活性基团,最后利用硫酸锆作为连接剂,将改性TiO2与改性皮革纤维进行交联,使改性后的皮革具有增强的抗紫外性能。
Description
技术领域
本发明涉及功能材料领域,具体是一种氨基改性TiO2皮革纤维的制备方法。
背景技术
随着人们生活水平的提高,皮革类产品在我们日常生活中占据着重要角色,如我们所使用鞋、衣服和皮包,这些产品大多数由皮革制造而成。然而,日常生活中紫外线无处不在,长期的紫外线照射可使皮革胶原蛋白链段发生交联和降解,进而影响其使用价值。
在最近几年,纳米材料在皮革领域应用越来越广泛,通过使用纳米材料赋予皮革或涂饰膜具有自清洁,抗紫外线,抗菌、超亲水性等性能。其中纳米二氧化钛由于粒径小,活性大,既能反射、散射紫外线,又能吸收紫外线,从而对紫外线有更强的阻隔能力。目前,在皮革抗紫外研究中,主要以皮革涂饰剂为主,通过涂饰剂赋予皮革抗紫外性能,但涂饰剂本身存在老化问题,且TiO2的加入也主要是对涂饰剂起抗紫外作用,并没有对皮革本身起到抗紫外作用。
发明内容
本发明为了解决现有技术的问题,提供了一种氨基改性TiO2皮革纤维的制备方法,可以使皮革纤维本身具备抗紫外性能。
本发明提供了一种氨基改性TiO2皮革纤维的制备方法,包括以下步骤:
1)利用硅烷偶联剂(3-氨丙基三乙氧基硅烷)对TiO2进行表面化学修饰,使TiO2表面带有氨基:将3-5g TiO2加入体积分数为0.5-1%的硅烷偶联剂,混合搅拌2-3h,温度控制在60-80℃,反应结束后,过滤,于110℃下干燥10-20min。
2)利用氯乙酸钠对皮革纤维进行羧基化,使得皮革纤维具有更多活性基团:
2.1)在三口烧瓶中加入氯乙酸20-30g,水15-20mL,搅拌溶解,同时滴加30-50%氢氧化钠溶液中和,得到氯乙酸钠;
2.2)将3-5g皮革浸与100-200mL去离子水中,浸泡10-12h,再放于水浴恒温振荡器中振荡4-6h;
2.3)将步骤2.1)得到的氯乙酸钠加入步骤2.2)得到的回湿皮革中进行反应,温度为40-50℃,用NaHCO3调节体系PH值保持在7-8,反应5-8h。
3)利用硫酸锆作为连接剂,将步骤1)得到的改性TiO2与步骤2)得到的改性皮革纤维进行交联,使改性后的皮革具有增强的抗紫外性能:将改性TiO2与改性皮革纤维放于100mL烧杯中,加入0.02-0.08g/mL的硫酸锆溶液,体系PH为1.5-2.5,搅拌反应 3-6h,反应结束后,过滤、去离子水洗涤3-5次,干燥。
本发明有益效果在于:
通过硅烷偶联剂对TiO2表面进行化学修饰,使其表面带有大量氨基,再通过氯乙酸钠对皮革纤维进行羧基化,在酸性条件下,硫酸锆中的Zr4+与TiO2表面-NH2的N原子、改性皮革纤维中的-COO及-CONH-中的C=O形成螯合物,与皮革纤维和二氧化钛以氢键连接相比稳定性更强,耐摩擦牢度增大,TiO2不易从皮革纤维上脱落,使皮革纤维本身具备更好的抗紫外性能。
具体实施方式
下面结合具体实施方式对本发明做进一步说明。
本发明提供了一种氨基改性TiO2皮革纤维的制备方法,包括以下步骤:
1)利用硅烷偶联剂(3-氨丙基三乙氧基硅烷)对TiO2进行表面化学修饰,使TiO2表面带有氨基:将3-5g TiO2加入体积分数为0.5-1%的硅烷偶联剂,混合搅拌2-3h,温度控制在60-80℃,反应结束后,过滤,于110℃下干燥10-20min。
2)利用氯乙酸钠对皮革纤维进行羧基化,使得皮革纤维具有更多活性基团:
2.1)在三口烧瓶中加入氯乙酸20-30g,水15-20mL,搅拌溶解,同时滴加30-50%氢氧化钠溶液中和,得到氯乙酸钠;
2.2)将3-5g皮革浸与100-200mL去离子水中,浸泡10-12h,再放于水浴恒温振荡器中振荡4-6h;
2.3)将步骤2.1)得到的氯乙酸钠加入步骤2.2)得到的回湿皮革中进行反应,温度为40-50℃,用NaHCO3调节体系PH值保持在7-8,反应5-8h。
3)利用硫酸锆作为连接剂,将步骤1)得到的改性TiO2与步骤2)得到的改性皮革纤维进行交联,使改性后的皮革具有增强的抗紫外性能:将改性TiO2与改性皮革纤维放于100mL烧杯中,加入0.02-0.08g/mL的硫酸锆溶液,体系PH为1.5-2.5,搅拌反应 3-6h,反应结束后,过滤、去离子水洗涤3-5次,干燥。
所制备而得的皮革样品与TiO2含量相同的改性丙烯酸树脂涂饰剂处理过的皮革(自制)经下述操作处理,比较其UPF、耐摩擦牢度及染色牢度:
a.通过紫外-可见光连续分光光度计分析,测定其UPF值。
b.用摩擦牢度试验仪,按照GB/T3920--1997进行测试,随后采用评定变色用灰色样卡(GB/T251-1984)进行评级。
c.染色皮革在浓度为1-5g/L的肥皂溶液中皂洗,温度为30-80℃,时间为10-50min, 浴比为30:1-70:1,取出水洗,烘干。用评定变色用灰色样卡(GB/T251-1984)进行评级。
实施例1
(1)将3g TiO2加入体积分数为0.5%的硅烷偶联剂,混合搅拌3h,温度控制在60℃,反应结束后,过滤、于110℃下干燥15min。
(2)在三口烧瓶中加入氯乙酸20g,水15mL,搅拌溶解,同时滴加30%氢氧化钠溶液中和,得到氯乙酸钠。再将3g皮革浸与100mL去离子水中,浸泡10h,再放于水浴恒温振荡器中振荡4h。将氯乙酸钠加入回湿皮革中进行反应,温度为45℃,用NaHCO3调节体系PH值保持在7.5,反应6h。
(3)将上述(1)和上述(2)制备得到产物放于100mL烧杯中,加入0.05g/mL的硫酸锆溶液,体系PH为1.5,搅拌反应3h。反应结束后,过滤、去离子水洗涤5次,干燥。
(4)自制含3g TiO2改性丙烯酸树脂涂饰剂处理过的皮革与上述皮革样品经下述操作处理,比较其UPF、耐摩擦牢度及染色牢度:
a.通过紫外-可见光连续分光光度计分析,测定其UPF值。
b.用摩擦牢度试验仪,按照GB/T3920--1997进行测试,随后采用评定变色用灰色样卡(GB/T251-1984)进行评级。
c.染色皮革在浓度为1g/L的肥皂溶液中皂洗,温度为50℃,时间为20min,浴比为70:1,取出水洗,烘干。用评定变色用灰色样卡(GB/T251-1984)进行评级。结果如下:
实施例2
(1)将5g TiO2加入体积分数为1%的硅烷偶联剂,混合搅拌3h,温度控制在60℃,反应结束后,过滤、于110℃下干燥15min。
(2)在三口烧瓶中加入氯乙酸22g,水15mL,搅拌溶解,同时滴加30%氢氧化钠溶液中和,得到氯乙酸钠。再将3g皮革浸与100mL去离子水中,浸泡10h,再放于水浴恒温振荡器中振荡4h。将氯乙酸钠加入回湿皮革中进行反应,温度为45℃,用NaHCO3调节体系PH值保持在8,反应6h。
(3)将上述(1)和上述(2)制备得到产物放于100mL烧杯中,加入0.07g/mL的硫酸锆溶液,体系PH为1.5,搅拌反应4h。反应结束后,过滤、去离子水洗涤5次,干燥。
(4)自制含5g TiO2改性丙烯酸树脂涂饰剂处理过的皮革与上述皮革样品经下述操作处理,比较其UPF、耐摩擦牢度及染色牢度:
a.通过紫外-可见光连续分光光度计分析,测定其UPF值。
b.用摩擦牢度试验仪,按照GB/T3920--1997进行测试,随后采用评定变色用灰色样卡(GB/T251-1984)进行评级。
c.染色皮革在浓度为2g/L的肥皂溶液中皂洗,温度为50℃,时间为30min,浴比为70:1,取出水洗,烘干。用评定变色用灰色样卡(GB/T251-1984)进行评级。结果如下:
通过紫外-可见光连续分光光度计分析,上述实验所得到的皮革UPF值为56.2。
实施例3
(1)将4g TiO2加入体积分数为0.7%的硅烷偶联剂,混合搅拌3h,温度控制在60℃,反应结束后,过滤、于110℃下干燥15min。
(2)在三口烧瓶中加入氯乙酸21g,水15mL,搅拌溶解,同时滴加30%氢氧化钠溶液中和,得到氯乙酸钠。再将3g皮革浸与100mL去离子水中,浸泡10h,再放于水浴恒温振荡器中振荡4h。将氯乙酸钠加入回湿皮革中进行反应,温度为45℃,用NaHCO3调节体系PH值保持在7.5,反应6h。
(3)将上述(1)和上述(2)制备得到产物放于100mL烧杯中,加入0.06g/mL的硫酸锆溶液,体系PH为1.5,搅拌反应4h。反应结束后,过滤、去离子水洗涤5次,干燥。
(4)自制含4g TiO2改性丙烯酸树脂涂饰剂处理过的皮革与上述皮革样品经下述操作处理,比较其UPF、耐摩擦牢度及染色牢度:
a.通过紫外-可见光连续分光光度计分析,测定其UPF值。
b.用摩擦牢度试验仪,按照GB/T3920--1997进行测试,随后采用评定变色用灰色样卡(GB/T251-1984)进行评级。
c.染色皮革在浓度为2g/L的肥皂溶液中皂洗,温度为70℃,时间为30min,浴比为60:1,取出水洗,烘干。用评定变色用灰色样卡(GB/T251-1984)进行评级。结果如下:
本发明具体应用途径很多,以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以作出若干改进,这些改进也应视为本发明的保护范围。
Claims (3)
1.一种氨基改性TiO2 皮革纤维的制备方法,其特征在于包括以下步骤:
1)利用硅烷偶联剂3-氨丙基三乙氧基硅烷对TiO2 进行表面化学修饰;
2)利用氯乙酸钠对皮革纤维进行羧基化;
3)利用硫酸锆作为连接剂,将步骤1)得到的改性TiO2与步骤2)得到的改性皮革纤维进行交联,具体过程为改性TiO2与改性皮革纤维放于100mL烧杯中,加入0.02-0.08g/mL的硫酸锆溶液,体系pH 为1.5-2.5,搅拌反应3-6h,反应结束后,过滤、去离子水洗涤3-5次,干燥。
2.根据权利要求1所述的氨基改性TiO2皮革纤维的制备方法,其特征在于步骤1)所述的TiO2 表面化学修饰过程具体如下:将3-5g TiO2 加入体积分数为0.5-1%的硅烷偶联剂,混合搅拌2-3h,温度控制在60-80℃,反应结束后,过滤,于110℃下干燥10-20min。
3.根据权利要求1所述的氨基改性TiO2皮革纤维的制备方法,其特征在于步骤2)所述的皮革纤维羧基化过程具体如下:
2.1)在三口烧瓶中加入氯乙酸20-30g,水15-20 mL,搅拌溶解,同时滴加30-50%氢氧化钠溶液中和,得到氯乙酸钠;
2.2)将3-5g皮革浸与100-200 mL去离子水中,浸泡10-12h,再放于水浴恒温振荡器中振荡4-6h;
2.3)将步骤2.1)得到的氯乙酸钠加入步骤2.2)得到的回湿皮革中进行反应,温度为40-50℃,用NaHCO3调节体系pH 值保持在7-8,反应5-8h。
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CN104357595A (zh) * | 2014-11-07 | 2015-02-18 | 陕西科技大学 | 赋予皮革屏蔽紫外线功能的皮革加脂剂及其制备方法 |
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CN103266418A (zh) * | 2013-05-16 | 2013-08-28 | 上海博格工业用布有限公司 | 原生态废革胶原蛋白纤维非织造布的制造工艺 |
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