CN117531504A - 一种抗菌除甲醛复合型光触媒及其制备方法和应用 - Google Patents
一种抗菌除甲醛复合型光触媒及其制备方法和应用 Download PDFInfo
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- CN117531504A CN117531504A CN202311539876.9A CN202311539876A CN117531504A CN 117531504 A CN117531504 A CN 117531504A CN 202311539876 A CN202311539876 A CN 202311539876A CN 117531504 A CN117531504 A CN 117531504A
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- composite photocatalyst
- formaldehyde
- antibacterial
- titanium dioxide
- removing composite
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- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
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- LCHWKMAWSZDQRD-UHFFFAOYSA-N silylformonitrile Chemical compound [SiH3]C#N LCHWKMAWSZDQRD-UHFFFAOYSA-N 0.000 claims abstract description 6
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- GBQYMXVQHATSCC-UHFFFAOYSA-N 3-triethoxysilylpropanenitrile Chemical group CCO[Si](OCC)(OCC)CCC#N GBQYMXVQHATSCC-UHFFFAOYSA-N 0.000 claims description 11
- 150000002500 ions Chemical class 0.000 claims description 11
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- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical group [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 150000003624 transition metals Chemical class 0.000 claims description 7
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 6
- 239000012266 salt solution Substances 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
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- 229910052681 coesite Inorganic materials 0.000 description 12
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- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
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- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
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- 229940071125 manganese acetate Drugs 0.000 description 1
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 description 1
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- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 1
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- 239000011718 vitamin C Substances 0.000 description 1
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Abstract
本发明属于光降解催化材料及环保技术领域,公开了一种抗菌除甲醛复合型光触媒及其制备方法和应用。所述抗菌除甲醛复合型光触媒由超活性纳米二氧化钛2%~20%,纳米银粉1%~10%,聚乙二醇0.2%~4%和负离子水溶剂组成。所述超活性纳米二氧化钛是采用硅溶胶、氰基硅烷偶联剂和钛酸酯偶联剂经乳液缩合,得到负载TiO2的多孔SiO2微球,再将负载TiO2的多孔SiO2微球浸渍吸附处理过渡金属盐后经煅烧得到。本发明所得超活性纳米二氧化钛具有更多的催化活性位点及显著提高的吸附性能,所得复合型光触媒可显著提高其常温催化降解甲醛等TVOC的效率,并具有良好的抗菌、防霉特性,具有良好的应用前景。
Description
技术领域
本发明属于光降解催化材料及环保技术领域,具体涉及一种抗菌除甲醛复合型光触媒及其制备方法和应用。
背景技术
光触媒也叫光催化剂,是一种以纳米级二氧化钛为代表的具有光催化功能材料的总称。它能在光照射下产生强氧化性的物质(如羟基自由基、氧气等),并且可用于分解有机化合物、部分无机化合物、细菌及病毒等。日常生活中,光触媒能有效地降解空气中有毒有害气体如甲醛等,高效净化空气;同时,能够有效杀灭多种细菌,并能将细菌或真菌释放出的毒素分解及无害化处理。
专利CN 103894215 A公开了一种纳米复合光触媒,其主要组成为:纳米二氧化钛:0.05-97%,硅溶胶20%,特殊纳米材料A:0.05-50%,氯化钠溶液:9%,其余为蒸馏水。该纳米复合光触媒的形态可以是液态或固体,纳米二氧化钛粒子直径范围为5-90nm,特殊纳米材料A的粒子直径范围为5-90nm,硅溶胶的粒子直径范围为6-96nm。特殊纳米材料A为:银、铜、铁的金属单质或其氧化物或其氯化物或含其离子的水溶液。专利CN 104789122 B公开了一种有机硅复合光触媒乳液,由下述原料按所述重量份数比制备而成,无水乙醇、环氧基硅烷、纳米活性炭、纳米硅藻土、纳米二氧化钛、纳米负离子粉、纳米氧化锌、稀散元素、丙三醇、苯甲酸钠、六偏磷酸钠、氨基酸、维生素C、表面活性剂、蒸馏水、羧乙基纤维素。该光触媒可对室内装修后装修材料释放的化学污染物进行有效清除,也可以消灭病毒细菌等生物污染物。专利CN 111841518 A公开了复合光触媒及光触媒材料,各组分及其重量百分比为:改性纳米二氧化钛60~90%、纳米硅藻泥10~30%、纳米银2~10%、香精0.1~1%,且改性纳米二氧化钛粒子的表面包覆有纳米二氧化硅,形成一层多孔包覆层。利用改性纳米二氧化钛在二氧化钛纳米粒子的表面形成一层多孔包覆层,有助于解决纳米二氧化钛易团聚的问题,且纳米硅藻泥的组分也有助于使得改性纳米二氧化钛更加分散。
通过以上现有技术可以看出,提高二氧化钛的分散性是提高其光催化性能的关键,然而目前仍普遍存在负载分散效果不佳的缺陷,其常温光催化性能仍有待进一步提高。
发明内容
针对以上现有技术存在的缺点和不足之处,本发明的首要目的在于提供一种抗菌除甲醛复合型光触媒的制备方法。
本发明的另一目的在于提供一种通过上述方法制备得到的抗菌除甲醛复合型光触媒。
本发明的再一目的在于提供上述抗菌除甲醛复合型光触媒在家具家装、汽车装饰等材料抗菌、防霉、除甲醛的应用。
本发明目的通过以下技术方案实现:
一种抗菌除甲醛复合型光触媒的制备方法,包括如下制备步骤:
(1)超活性纳米二氧化钛的制备:
将硅溶胶与氰基硅烷偶联剂和钛酸酯偶联剂搅拌混合均匀后调节pH值至2~4,将所得混合液加入到油相中,加入乳化剂均质得到乳液,然后加入氨水调节pH值至9~11,搅拌混合均匀后静置老化,产物经洗涤、干燥,得到负载TiO2的多孔SiO2微球;将所得负载TiO2的多孔SiO2微球加入到过渡金属盐溶液中浸渍吸附处理,取出后洗涤、干燥、煅烧、粉碎,得到过渡金属氧化物掺杂负载型超活性纳米二氧化钛;
(2)复合型光触媒的制备:
将步骤(1)所得超活性纳米二氧化钛与纳米银粉和聚乙二醇加入到负离子水中搅拌分散均匀,得到抗菌除甲醛复合型光触媒。
优选地,步骤(1)中所述氰基硅烷偶联剂为2-氰乙基三乙氧基硅烷,2-氰乙基三乙氧基硅烷的加入量为硅溶胶固含量的20%~50%。
优选地,步骤(1)中所述钛酸酯偶联剂为钛酸四乙酯或钛酸四丁酯,钛酸酯偶联剂的加入量为硅溶胶固含量的10%~80%。
优选地,步骤(1)中所述油相为环己烷和乙酸乙酯的混合溶剂;所述乳化剂为聚氧乙烯脂肪酸酯乳化剂。
优选地,步骤(1)中所述过渡金属盐溶液是指Mn、Cu、Ni、Fe、Ce、Co中至少一种金属的可溶性盐溶液。
优选地,步骤(1)中所述干燥是指在80~120℃下真空干燥;所述煅烧是指在500~600℃空气条件下煅烧。
优选地,步骤(1)中所述粉碎是指粉碎至粒径为10~200nm。
优选地,步骤(2)中所述纳米银粉的粒径为10~200nm。
优选地,步骤(2)中所述聚乙二醇的分子量为600~6000。
优选地,步骤(2)中所述负离子水是指经电解水阴极产生的碱性水。
一种抗菌除甲醛复合型光触媒,通过上述方法制备得到。
优选地,所述抗菌除甲醛复合型光触媒中各组分质量百分含量如下:
超活性纳米二氧化钛2%~20%,纳米银粉1%~10%,聚乙二醇0.2%~4%,负离子水,余量。
上述抗菌除甲醛复合型光触媒在家具家装、汽车装饰等材料抗菌、防霉、除甲醛中的应用,所述应用方法为:将抗菌除甲醛复合型光触媒喷涂于待处理物体表面,然后通风晾干即可。
与现有技术相比,本发明的有益效果是:
(1)本发明的超活性纳米二氧化钛以多孔SiO2微球作为载体,能够显著改善二氧化钛的分散及增强其活性位点,提高其常温催化降解甲醛等TVOC的效率。
(2)本发明的超活性纳米二氧化钛通过进一步掺杂Mn、Cu、Ni、Fe、Ce、Co等过渡金属的氧化物,可进一步降低TiO2常温光催化氧化降解甲醛等TVOC所需要的反应活化能,显著提高其常温降解效率。
(3)本发明的超活性纳米二氧化钛进一步采用氰基硅烷偶联剂进行改性,可显著提高载体对过渡金属的吸附负载能力,且能显著提高其比表面积及对甲醛等TVOC的吸附性能,并最终大大提高其常温催化降解甲醛等TVOC的效率。
实施方式
下面结合实施例对本发明作进一步详细的描述,但本发明的实施方式不限于此。
实施例
一种抗菌除甲醛复合型光触媒的制备方法,包括如下制备步骤:
(1)超活性纳米二氧化钛的制备:
将硅溶胶与2-氰乙基三乙氧基硅烷和钛酸四乙酯搅拌混合均匀后用硝酸溶液调节pH值至3,其中2-氰乙基三乙氧基硅烷的加入量为硅溶胶固含量的30%,钛酸四乙酯的加入量为硅溶胶固含量的40%。将所得混合液加入到环己烷和乙酸乙酯的混合油相中,加入乳化剂吐温-80均质得到乳液,然后加入氨水调节pH值至10,搅拌混合均匀后静置过夜老化,产物经乙醇洗涤、真空干燥,得到负载TiO2的多孔SiO2微球;将所得负载TiO2的多孔SiO2微球加入质量分数为8.65%的醋酸锰溶液中浸渍吸附处理过夜,抽滤后去离子水洗涤、90℃真空干燥、560℃空气煅烧,纳米级粉碎机粉碎至D90粒径<100nm,得到MnO2掺杂多孔SiO2微球负载型超活性纳米二氧化钛。根据氮吸附BET测试结果显示,所得负载型超活性纳米二氧化钛的比表面积为582 m2/g,孔体积为1.96 cm3/g。
(2)复合型光触媒的制备:
按质量份计,将步骤(1)所得超活性纳米二氧化钛12份与纳米银粉(平均粒径为50nm)6份和2份聚乙二醇-2000加入到80份负离子水(电解水阴极产生的碱性水)中搅拌溶解分散均匀,得到抗菌除甲醛复合型光触媒。
实施例
一种抗菌除甲醛复合型光触媒的制备方法,包括如下制备步骤:
(1)超活性纳米二氧化钛的制备:
将硅溶胶与2-氰乙基三乙氧基硅烷和钛酸四丁酯搅拌混合均匀后用硝酸溶液调节pH值至4,其中2-氰乙基三乙氧基硅烷的加入量为硅溶胶固含量的20%,钛酸四丁酯的加入量为硅溶胶固含量的60%。将所得混合液加入到环己烷和乙酸乙酯的混合油相中,加入乳化剂吐温-80均质得到乳液,然后加入氨水调节pH值至11,搅拌混合均匀后静置过夜老化,产物经乙醇洗涤、真空干燥,得到负载TiO2的多孔SiO2微球;将所得负载TiO2的多孔SiO2微球加入质量分数为8%的硫酸铜溶液中浸渍吸附处理过夜,抽滤后去离子水洗涤、100℃真空干燥、600℃空气煅烧,纳米级粉碎机粉碎至D90粒径<100nm,得到CuO掺杂多孔SiO2微球负载型超活性纳米二氧化钛。根据氮吸附BET测试结果显示,所得负载型超活性纳米二氧化钛的比表面积为561 m2/g,孔体积为1.91 cm3/g。
(2)复合型光触媒的制备:
按质量份计,将步骤(1)所得超活性纳米二氧化钛5份与纳米银粉(平均粒径为50nm)2份和1份聚乙二醇-1200加入到92份负离子水(电解水阴极产生的碱性水)中搅拌溶解分散均匀,得到抗菌除甲醛复合型光触媒。
实施例
一种抗菌除甲醛复合型光触媒的制备方法,包括如下制备步骤:
(1)超活性纳米二氧化钛的制备:
将硅溶胶与2-氰乙基三乙氧基硅烷和钛酸四丁酯搅拌混合均匀后用硝酸溶液调节pH值至2,其中2-氰乙基三乙氧基硅烷的加入量为硅溶胶固含量的50%,钛酸四丁酯的加入量为硅溶胶固含量的20%。将所得混合液加入到环己烷和乙酸乙酯的混合油相中,加入乳化剂吐温-80均质得到乳液,然后加入氨水调节pH值至9,搅拌混合均匀后静置过夜老化,产物经乙醇洗涤、真空干燥,得到负载TiO2的多孔SiO2微球;将所得负载TiO2的多孔SiO2微球加入质量分数为8.1%的氯化铁溶液中浸渍吸附处理过夜,抽滤后去离子水洗涤、100℃真空干燥、500℃空气煅烧,纳米级粉碎机粉碎至D90粒径<100nm,得到Fe2O3掺杂多孔SiO2微球负载型超活性纳米二氧化钛。根据氮吸附BET测试结果显示,所得负载型超活性纳米二氧化钛的比表面积为596 m2/g,孔体积为2.03 cm3/g。
(2)复合型光触媒的制备:
按质量份计,将步骤(1)所得超活性纳米二氧化钛20份与纳米银粉(平均粒径为50nm)10份和4份聚乙二醇-800加入到66份负离子水(电解水阴极产生的碱性水)中搅拌溶解分散均匀,得到抗菌除甲醛复合型光触媒。
对以上实施例1~3所得抗菌除甲醛复合型光触媒进行安全性及性能测试如下:
(1)多次皮肤刺激性/腐蚀性(《消毒技术规范》2002 年版,第二部分,2.3.3)、急性经口毒性试验(《消毒技术规范》2002 年版,第二部分,2.3.1)。
测试结果显示受试物对新西兰免多次皮肤刺激试验结果为无刺激性;受试物对SPF级KM小急性经口毒性LD50>5000mg/kg·BW,属于实际无毒。
(2)甲醛去除率(QB/T 2761-2006),测试效果如下表1所示。
(3)抗菌性能(GB/T 30706-2014 可见光照射下光催化抗菌材料及制品抗菌测试方法及评价),测试效果显示实施例1~3所得复合型光触媒对大肠杆菌和金黄色葡萄球菌的抗菌率均>99.99%。
(4)耐霉菌性能(GB/T 1741-2007),测试效果显示实施例1~3所得复合型光触媒的防霉等级均为0级(在放大约 50倍下无明显长霉)。
对比例1
本对比例与实施例1相比,超活性纳米二氧化钛未掺杂MnO2,直接采用负载TiO2的多孔SiO2微球制备复合型光触媒,其余相同。
本对比例所得负载型超活性纳米二氧化钛的比表面积为590 m2/g,孔体积为2.02cm3/g。
本对比例所得复合型光触媒的甲醛去除率结果显示甲醛去除率为78.2%,苯去除率为72.3%,TVOC去除率为73.8%。
通过本对比例与实施例1~3的比较结果可以看出,本发明通过进一步掺杂过渡金属的氧化物,可显著提高常温条件下光触媒对甲醛等TVOC的降解效率。其原因可能在于过渡金属氧化物的掺杂可进一步降低TiO2常温光催化氧化降解甲醛等TVOC所需要的反应活化能。
对比例2
本对比例与实施例1相比,超活性纳米二氧化钛的制备过程中未加入2-氰乙基三乙氧基硅烷,其余相同。
本对比例所得负载型超活性纳米二氧化钛的比表面积为425 m2/g,孔体积为1.49cm3/g。
本对比例所得复合型光触媒的甲醛去除率结果显示甲醛去除率为80.6%,苯去除率为66.2%,TVOC去除率为69.5%。
通过本对比例与实施例1~3的比较结果可以看出,通过氰乙基改性可以显著提高所得负载型超活性纳米二氧化钛的比表面积,和显著提高其常温催化降解甲醛等TVOC的效率。其原因可能在于经氰乙基改性后的载体其吸附负载过渡金属的能力更强,且在后续空气煅烧过程中产生挥发性N、C氧化物气体生成更多的孔隙,其具有更多的催化活性位点及对TVOC污染物的吸附降解能力。
上述实施例为本发明较佳的实施方式,但本发明的实施方式并不受上述实施例的限制,其它的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本发明的保护范围之内。
Claims (10)
1.一种抗菌除甲醛复合型光触媒的制备方法,其特征在于,包括如下制备步骤:
(1)超活性纳米二氧化钛的制备:
将硅溶胶与氰基硅烷偶联剂和钛酸酯偶联剂搅拌混合均匀后调节pH值至2~4,将所得混合液加入到油相中,加入乳化剂均质得到乳液,然后加入氨水调节pH值至9~11,搅拌混合均匀后静置老化,产物经洗涤、干燥,得到负载TiO2的多孔SiO2微球;将所得负载TiO2的多孔SiO2微球加入到过渡金属盐溶液中浸渍吸附处理,取出后洗涤、干燥、煅烧、粉碎,得到过渡金属氧化物掺杂负载型超活性纳米二氧化钛;
(2)复合型光触媒的制备:
将步骤(1)所得超活性纳米二氧化钛与纳米银粉和聚乙二醇加入到负离子水中搅拌分散均匀,得到抗菌除甲醛复合型光触媒。
2.根据权利要求1所述的一种抗菌除甲醛复合型光触媒的制备方法,其特征在于,步骤(1)中所述氰基硅烷偶联剂为2-氰乙基三乙氧基硅烷,2-氰乙基三乙氧基硅烷的加入量为硅溶胶固含量的20%~50%。
3.根据权利要求1所述的一种抗菌除甲醛复合型光触媒的制备方法,其特征在于,步骤(1)中所述钛酸酯偶联剂为钛酸四乙酯或钛酸四丁酯,钛酸酯偶联剂的加入量为硅溶胶固含量的10%~80%。
4.根据权利要求1所述的一种抗菌除甲醛复合型光触媒的制备方法,其特征在于,步骤(1)中所述油相为环己烷和乙酸乙酯的混合溶剂;所述乳化剂为聚氧乙烯脂肪酸酯乳化剂。
5.根据权利要求1所述的一种抗菌除甲醛复合型光触媒的制备方法,其特征在于,步骤(1)中所述过渡金属盐溶液是指Mn、Cu、Ni、Fe、Ce、Co中至少一种金属的可溶性盐溶液。
6.根据权利要求1所述的一种抗菌除甲醛复合型光触媒的制备方法,其特征在于,步骤(1)中所述干燥是指在80~120℃下真空干燥;所述煅烧是指在500~600℃空气条件下煅烧;所述粉碎是指粉碎至粒径为10~200nm。
7.根据权利要求1所述的一种抗菌除甲醛复合型光触媒的制备方法,其特征在于,步骤(2)中所述纳米银粉的粒径为10~200nm;所述聚乙二醇的分子量为600~6000;所述负离子水是指经电解水阴极产生的碱性水。
8.一种抗菌除甲醛复合型光触媒,其特征在于,通过权利要求1~7任一项所述的方法制备得到。
9.根据权利要求8所述的一种抗菌除甲醛复合型光触媒,其特征在于,所述抗菌除甲醛复合型光触媒中各组分质量百分含量如下:
超活性纳米二氧化钛2%~20%,纳米银粉1%~10%,聚乙二醇0.2%~4%,负离子水,余量。
10.权利要求8或9所述的抗菌除甲醛复合型光触媒在家具家装、汽车装饰等材料抗菌、防霉、除甲醛中的应用,其特征在于,所述应用方法为:将抗菌除甲醛复合型光触媒喷涂于待处理物体表面,然后通风晾干即可。
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