CN109267329A - 一种涤棉织物自清洁整理剂的制备方法 - Google Patents
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Abstract
本发明提供了一种涤棉织物自清洁整理剂的制备方法,包括以下步骤:将钛酸四丁酯和无水乙醇混合,滴冰醋酸形成A溶液,取正硅酸乙酯和无水乙醇混合形成B溶液;将去离子水滴入B溶液中形成溶胶后加入A溶液中;倒入模具中密封,用无水乙醇浸泡老化;放入正硅酸乙酯醇溶液中,继续老化;洗涤,干燥得复合气凝胶;取纳米氧化锌加蒸馏水搅拌;加γ‑氨丙基三乙氧基硅烷继续搅拌;过滤去除液体,烘干;加复合气凝胶、分散剂、麦饭石粉、抗菌沸石、水性聚氨酯和蒸馏水,混合后剪切;超声即得。本法所制备的涤棉织物自清洁整理剂能够使涤棉织物具有非常好的光催化性能的油污自清洁效果,经向断裂强力没有无明显变化;同时具有很好的透气性和抗菌性能。
Description
技术领域
本发明涉及一种涤棉织物自清洁整理剂的制备方法。
背景技术
自清洁是指具有光催化效应的纳米半导体超细粒子如二氧化钛、氧化锌、硫化镉和三氧化钨等在光的作用下跃迁产生的电子/空穴对,与溶解氧和水发生作用,生成的自由基可以把有机污染物彻底氧化为二氧化碳和水等无机物。光催化氧化技术氧化效率高,反应速度快,对多种有机污染物有良好的处理效果,并且绿色环保,是一种深度氧化技术。而二氧化钛因化学性质稳定、光照后不发生光腐蚀、耐酸碱性好、对生物体无毒、且光催化活性高、反应条件温和等优点备受研究者的青睐。同时,随着全球经济的飞快发展,环境污染也日益严重,从而导致室内空气质量变差,纺织品易受环境中的污物所污染,成为各种细菌繁殖的场所,每年有大批量的纺织品因发霉而废弃,所以人们对纺织品的功能需求不仅仅停留在最基本的性能上,将自清洁技术应用于纺织品上也越来越受到人们的青睐,也无疑将为纺织行业创造巨大的社会和经济效益。
发明内容
要解决的技术问题:本发明的目的是提供一种涤棉织物自清洁整理剂的制备方法,能够使涤棉织物具有非常好的光催化性能的油污自清洁效果,经向断裂强力没有无明显变化;同时具有很好的透气性和抗菌性能。
技术方案:一种涤棉织物自清洁整理剂的制备方法,成分按重量份计,包括以下步骤:
(1)将5-10份钛酸四丁酯和15-30份无水乙醇混合均匀,滴入1-2份冰醋酸,置于磁力搅拌器上充分搅拌均匀,形成A溶液,取4-8份正硅酸乙酯和10-20份无水乙醇混合均匀,置于磁力搅拌器上搅拌,形成B溶液;
(2)将去离子水逐滴滴入B溶液中,充分搅拌待B溶液形成溶胶后,将B溶胶缓慢加入处于搅拌状态的A溶液中继续搅拌2-3min后,加入2-4份甲酰胺继续搅拌5-7min;
(3)倒入模具中,密封,在室温下放置12-24h后用无水乙醇浸泡、老化5d,每天更换1次无水乙醇;
(4)放入正硅酸乙酯醇溶液中,继续在室温下老化6d,每天更换一次正硅酸乙酯醇溶液;
(5)用无水乙醇洗涤,放入小孔聚丙烯容器中,依次在室温、40℃、50℃、60℃、70℃和80℃下各干燥2h即得复合气凝胶;
(6)取0.5-1份纳米氧化锌,加入20-30份蒸馏水,用高剪切分散乳化机在转速15000-16000r/min下搅拌10-15min;
(7)加入0.5-1份γ-氨丙基三乙氧基硅烷,继续搅拌10-15min;
(8)过滤去除液体,烘干;
(9)加入复合气凝胶、5-8份分散剂、1-2份麦饭石粉、1-3份抗菌沸石、10-15份水性聚氨酯和400-500份蒸馏水,混合均匀后用高速剪切乳化机在剪切速率3000r/min下剪切20-25min;
(10)用超声波细胞粉碎机在超声功率1500-2000W下超声20-25min即得。
进一步的,所述分散剂聚乙二醇、三乙醇胺、月桂醇硫酸钠、月桂酰基谷氨酸或六偏磷酸钠中的一种或几种。
进一步的,所述麦饭石粉的粒径为1-10μm。
进一步的,所述抗菌沸石的粒径≤20μm。
有益效果:
1. 复合气凝胶中能够有效改善紫外线对涤棉织物的损害,尤其以二氧化硅气凝胶效果更好,同时利用气凝胶比表面积大的优势,充分发挥二氧化钛光催化降解性能,提高自清洁效果,同时具有优异的抗紫外线性能。
2. 经本发明方法所制备的整理剂对棉织物进行处理后,棉织物具有非常好的光催化性能的油污自清洁效果,经过24h的自然光照射后,残留于整理样上的油污全部降解;整理后的织物试样经光催化后的经向断裂强力和未经整理的织物试样相比没有无明显变化,其透气量高达600.2L/(m2·s),具有很好的透气效果,同时还具有一定的抗菌性,其对大肠杆菌有很好的抑制效果。
具体实施方式
实施例1
一种涤棉织物自清洁整理剂的制备方法,成分按重量份计,包括以下步骤:
(1)将5份钛酸四丁酯和15份无水乙醇混合均匀,滴入1份冰醋酸,置于磁力搅拌器上充分搅拌均匀,形成A溶液,取4份正硅酸乙酯和10份无水乙醇混合均匀,置于磁力搅拌器上搅拌,形成B溶液;
(2)将去离子水逐滴滴入B溶液中,充分搅拌待B溶液形成溶胶后,将B溶胶缓慢加入处于搅拌状态的A溶液中继续搅拌2min后,加入2份甲酰胺继续搅拌5min;
(3)倒入模具中,密封,在室温下放置12h后用无水乙醇浸泡、老化5d,每天更换1次无水乙醇;
(4)放入正硅酸乙酯醇溶液中,继续在室温下老化6d,每天更换一次正硅酸乙酯醇溶液;
(5)用无水乙醇洗涤,放入小孔聚丙烯容器中,依次在室温、40℃、50℃、60℃、70℃和80℃下各干燥2h即得复合气凝胶;
(6)取0.5份纳米氧化锌,加入20份蒸馏水,用高剪切分散乳化机在转速15000r/min下搅拌10min;
(7)加入0.5份γ-氨丙基三乙氧基硅烷,继续搅拌10min;
(8)过滤去除液体,烘干;
(9)加入复合气凝胶、5份三乙醇胺、1份麦饭石粉、1份抗菌沸石、10份水性聚氨酯和400份蒸馏水,混合均匀后用高速剪切乳化机在剪切速率3000r/min下剪切20min;
(10)用超声波细胞粉碎机在超声功率1500W下超声20min即得。
实施例2
一种涤棉织物自清洁整理剂的制备方法,成分按重量份计,包括以下步骤:
(1)将8份钛酸四丁酯和28份无水乙醇混合均匀,滴入1.5份冰醋酸,置于磁力搅拌器上充分搅拌均匀,形成A溶液,取6份正硅酸乙酯和15份无水乙醇混合均匀,置于磁力搅拌器上搅拌,形成B溶液;
(2)将去离子水逐滴滴入B溶液中,充分搅拌待B溶液形成溶胶后,将B溶胶缓慢加入处于搅拌状态的A溶液中继续搅拌2.5min后,加入3份甲酰胺继续搅拌6min;
(3)倒入模具中,密封,在室温下放置18h后用无水乙醇浸泡、老化5d,每天更换1次无水乙醇;
(4)放入正硅酸乙酯醇溶液中,继续在室温下老化6d,每天更换一次正硅酸乙酯醇溶液;
(5)用无水乙醇洗涤,放入小孔聚丙烯容器中,依次在室温、40℃、50℃、60℃、70℃和80℃下各干燥2h即得复合气凝胶;
(6)取0.8份纳米氧化锌,加入25份蒸馏水,用高剪切分散乳化机在转速15500r/min下搅拌13min;
(7)加入0.8份γ-氨丙基三乙氧基硅烷,继续搅拌13min;
(8)过滤去除液体,烘干;
(9)加入复合气凝胶、7份聚乙二醇、1.5份麦饭石粉、2份抗菌沸石、13份水性聚氨酯和450份蒸馏水,混合均匀后用高速剪切乳化机在剪切速率3000r/min下剪切23min;
(10)用超声波细胞粉碎机在超声功率1800W下超声23min即得。
实施例3
一种涤棉织物自清洁整理剂的制备方法,成分按重量份计,包括以下步骤:
(1)将10份钛酸四丁酯和30份无水乙醇混合均匀,滴入2份冰醋酸,置于磁力搅拌器上充分搅拌均匀,形成A溶液,取8份正硅酸乙酯和20份无水乙醇混合均匀,置于磁力搅拌器上搅拌,形成B溶液;
(2)将去离子水逐滴滴入B溶液中,充分搅拌待B溶液形成溶胶后,将B溶胶缓慢加入处于搅拌状态的A溶液中继续搅拌3min后,加入4份甲酰胺继续搅拌7min;
(3)倒入模具中,密封,在室温下放置24h后用无水乙醇浸泡、老化5d,每天更换1次无水乙醇;
(4)放入正硅酸乙酯醇溶液中,继续在室温下老化6d,每天更换一次正硅酸乙酯醇溶液;
(5)用无水乙醇洗涤,放入小孔聚丙烯容器中,依次在室温、40℃、50℃、60℃、70℃和80℃下各干燥2h即得复合气凝胶;
(6)取1份纳米氧化锌,加入30份蒸馏水,用高剪切分散乳化机在转速16000r/min下搅拌15min;
(7)加入1份γ-氨丙基三乙氧基硅烷,继续搅拌15min;
(8)过滤去除液体,烘干;
(9)加入复合气凝胶、8份月桂酰基谷氨酸、2份麦饭石粉、3份抗菌沸石、15份水性聚氨酯和500份蒸馏水,混合均匀后用高速剪切乳化机在剪切速率3000r/min下剪切25min;
(10)用超声波细胞粉碎机在超声功率2000W下超声25min即得。
对比例1
本实施例与实施例1的差别在于仅为二氧化钛气凝胶,具体为:
一种涤棉织物自清洁整理剂的制备方法,成分按重量份计,包括以下步骤:
(1)将5份钛酸四丁酯和15份无水乙醇混合均匀,滴入1份冰醋酸,置于磁力搅拌器上充分搅拌均匀,形成A溶液;
(2)加入2份甲酰胺继续搅拌5min;
(3)倒入模具中,密封,在室温下放置12h后用无水乙醇浸泡、老化5d,每天更换1次无水乙醇;
(4)放入小孔聚丙烯容器中,依次在室温、40℃、50℃、60℃、70℃和80℃下各干燥2h即得二氧化钛气凝胶;
(5)取0.5份纳米氧化锌,加入20份蒸馏水,用高剪切分散乳化机在转速15000r/min下搅拌10min;
(6)加入0.5份γ-氨丙基三乙氧基硅烷,继续搅拌10min;
(7)过滤去除液体,烘干;
(8)加入二氧化钛气凝胶、5份三乙醇胺、1份麦饭石粉、1份抗菌沸石、10份水性聚氨酯和400份蒸馏水,混合均匀后用高速剪切乳化机在剪切速率3000r/min下剪切20min;
(9)用超声波细胞粉碎机在超声功率1500W下超声20min即得。
对比例2
本实施例与实施例1的差别在于不含有处理后的纳米氧化锌,具体为:
一种涤棉织物自清洁整理剂的制备方法,成分按重量份计,包括以下步骤:
(1)将5份钛酸四丁酯和15份无水乙醇混合均匀,滴入1份冰醋酸,置于磁力搅拌器上充分搅拌均匀,形成A溶液,取4份正硅酸乙酯和10份无水乙醇混合均匀,置于磁力搅拌器上搅拌,形成B溶液;
(2)将去离子水逐滴滴入B溶液中,充分搅拌待B溶液形成溶胶后,将B溶胶缓慢加入处于搅拌状态的A溶液中继续搅拌2min后,加入2份甲酰胺继续搅拌5min;
(3)倒入模具中,密封,在室温下放置12h后用无水乙醇浸泡、老化5d,每天更换1次无水乙醇;
(4)放入正硅酸乙酯醇溶液中,继续在室温下老化6d,每天更换一次正硅酸乙酯醇溶液;
(5)用无水乙醇洗涤,放入小孔聚丙烯容器中,依次在室温、40℃、50℃、60℃、70℃和80℃下各干燥2h即得复合气凝胶;
(6)加入5份三乙醇胺、1份麦饭石粉、1份抗菌沸石、10份水性聚氨酯和400份蒸馏水,混合均匀后用高速剪切乳化机在剪切速率3000r/min下剪切20min;
(7)用超声波细胞粉碎机在超声功率1500W下超声20min即得。
对比例3
本实施例与实施例1的差别在于不含有水性聚氨酯,具体为:
一种涤棉织物自清洁整理剂的制备方法,成分按重量份计,包括以下步骤:
(1)将5份钛酸四丁酯和15份无水乙醇混合均匀,滴入1份冰醋酸,置于磁力搅拌器上充分搅拌均匀,形成A溶液,取4份正硅酸乙酯和10份无水乙醇混合均匀,置于磁力搅拌器上搅拌,形成B溶液;
(2)将去离子水逐滴滴入B溶液中,充分搅拌待B溶液形成溶胶后,将B溶胶缓慢加入处于搅拌状态的A溶液中继续搅拌2min后,加入2份甲酰胺继续搅拌5min;
(3)倒入模具中,密封,在室温下放置12h后用无水乙醇浸泡、老化5d,每天更换1次无水乙醇;
(4)放入正硅酸乙酯醇溶液中,继续在室温下老化6d,每天更换一次正硅酸乙酯醇溶液;
(5)用无水乙醇洗涤,放入小孔聚丙烯容器中,依次在室温、40℃、50℃、60℃、70℃和80℃下各干燥2h即得复合气凝胶;
(6)取0.5份纳米氧化锌,加入20份蒸馏水,用高剪切分散乳化机在转速15000r/min下搅拌10min;
(7)加入0.5份γ-氨丙基三乙氧基硅烷,继续搅拌10min;
(8)过滤去除液体,烘干;
(9)加入复合气凝胶、5份三乙醇胺、1份麦饭石粉、1份抗菌沸石和400份蒸馏水,混合均匀后用高速剪切乳化机在剪切速率3000r/min下剪切20min;
(10)用超声波细胞粉碎机在超声功率1500W下超声20min即得。
将棉织物浸渍与本发明整理剂中,超声处理10 min,振荡30 min后二浸二轧(轧余率80%-85%),在80℃下烘干,冷却测定其性能指标。
以红色辣椒油作为油污污渍对整理后的织物进行局部滴定观察,在保证每天自然光光照(气温28℃,晴天) 一定时间的基础上测定织物上红辣椒油污表观色深值K/S变化的方法来评价自清洁效果。
断裂强力根据ASTM D5035—2011《纺织品断裂强力和伸长率试验方法( 条样法)》进行测定。
透气性测试根据国家标准 GB/T5453-8 规定的测试方法,采用数字式透气量仪进行测试。
抑菌性的测定:利用滤纸片抑菌圈法测定面料对供试菌的抑制效果,将供试菌接入无菌液体培养基中,在37℃、120 r/min 的恒温摇床内活化培育 24 h。吸取一部分活化后的菌种液接入无菌水中,充分振荡后制成 107 cfu/m L的初始菌液。
将灭过菌的LB固体培养基在室温下放置,冷却至适宜温度后倒至无菌培养皿,待培养基凝固后备用。吸取0.1 mL初始菌液接种至LB培养基,用灭过菌的玻璃涂布棒将菌液分散均匀。
剪取一块直径为6 mm的织物,贴于含有供试菌的培养基上,把平板倒扣放置于温度为37℃的培养箱中 24 h。培养结束后,抑菌圈直径使用游标卡尺量出。
表1 涤棉织物自清洁整理剂的部分性能
产品名称 | 24h自然光照射<i>K/S</i>值 | 经向断裂强力(N) | 透气量(L/(m<sup>2</sup>·s)) | 大肠杆菌抑菌圈(mm) |
实施例1 | 1.57 | 605.3 | 599.4 | 13.33 |
实施例2 | 1.57 | 606.1 | 600.2 | 13.35 |
实施例3 | 1.57 | 605.8 | 599.7 | 13.34 |
对比例1 | 1.58 | 581.3 | 600.2 | 13.34 |
对比例2 | 3.21 | 605.2 | 595.8 | 13.14 |
对比例3 | 1.98 | 604.2 | 601.2 | 11.00 |
未整理 | 7.85 | 607.0 | 695.7 | - |
注:未滴红色辣椒油织物的K/S值为1.57
经本发明方法所制备的整理剂对棉织物进行处理后,棉织物具有非常好的光催化性能的油污自清洁效果,经过24h的自然光照射后,残留于整理样上的油污全部降解;整理后的织物试样经光催化后的经向断裂强力和未经整理的织物试样相比没有无明显变化;其透气量高达600.2L/(m2·s),具有很好的透气效果,同时还具有一定的抗菌性,其对大肠杆菌有很好的抑制效果。
Claims (4)
1.一种涤棉织物自清洁整理剂的制备方法,其特征在于:成分按重量份计,包括以下步骤:
将5-10份钛酸四丁酯和15-30份无水乙醇混合均匀,滴入1-2份冰醋酸,置于磁力搅拌器上充分搅拌均匀,形成A溶液,取4-8份正硅酸乙酯和10-20份无水乙醇混合均匀,置于磁力搅拌器上搅拌,形成B溶液;
将去离子水逐滴滴入B溶液中,充分搅拌待B溶液形成溶胶后,将B溶胶缓慢加入处于搅拌状态的A溶液中继续搅拌2-3min后,加入2-4份甲酰胺继续搅拌5-7min;
倒入模具中,密封,在室温下放置12-24h后用无水乙醇浸泡、老化5d,每天更换1次无水乙醇;
放入正硅酸乙酯醇溶液中,继续在室温下老化6d,每天更换一次正硅酸乙酯醇溶液;
用无水乙醇洗涤,放入小孔聚丙烯容器中,依次在室温、40℃、50℃、60℃、70℃和80℃下各干燥2h即得复合气凝胶;
取0.5-1份纳米氧化锌,加入20-30份蒸馏水,用高剪切分散乳化机在转速15000-16000r/min下搅拌10-15min;
加入0.5-1份γ-氨丙基三乙氧基硅烷,继续搅拌10-15min;
过滤去除液体,烘干;
加入复合气凝胶、5-8份分散剂、1-2份麦饭石粉、1-3份抗菌沸石、10-15份水性聚氨酯和400-500份蒸馏水,混合均匀后用高速剪切乳化机在剪切速率3000r/min下剪切20-25min;
用超声波细胞粉碎机在超声功率1500-2000W下超声20-25min即得。
2.根据权利要求 1所述的一种涤棉织物自清洁整理剂的制备方法,其特征在于:所述分散剂聚乙二醇、三乙醇胺、月桂醇硫酸钠、月桂酰基谷氨酸或六偏磷酸钠中的一种或几种。
3.根据权利要求 1所述的一种涤棉织物自清洁整理剂的制备方法,其特征在于:所述麦饭石粉的粒径为1-10μm。
4.根据权利要求 1所述的一种涤棉织物自清洁整理剂的制备方法,其特征在于:所述抗菌沸石的粒径≤20μm。
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CN114592350B (zh) * | 2022-03-07 | 2024-05-14 | 盐城工业职业技术学院 | 一种兼具保暖透气和净化空气双重功能的针织面料及其制备方法 |
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