CN112774716A - 一种含有蛭石的TiO2-C3N4光触媒剂及其制备方法 - Google Patents
一种含有蛭石的TiO2-C3N4光触媒剂及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种含有蛭石的TiO2‑C3N4光触媒剂及其制备方法,所述光触媒剂具体包括如下以重量份数计的原料:蛭石10‑20份、异丙醇钛3‑7份、尿素5‑10份、柠檬酸2‑5份、稀盐酸0.5‑3份、碳酸钠0.2‑3份、聚乙二醇‑82‑5份以及适量去离子水。该材料是结合物理化学吸附以及光催化降解技术,由蛭石与TiO2‑C3N4催化剂共同作用的一种光触媒剂,其不仅具有良好的净化空气以及降解有机物的能力,还具有绿色环保、性质稳定、抗菌抗紫外线等特点。
Description
技术领域
本发明涉及水质净化、空气净化以及光催化技术领域,特别是涉及一种含有蛭石的TiO2-C3N4光触媒剂及其制备方法。
背景技术
随着社会经济的迅猛发展,环境问题也日益凸显出来,其中废水和有害气体大量排放,严重影响了生活环境,所以开发一种有效的废水和有害气体治理手段俨然已成为了人们研究工作中的首要任务。近年来,为了实现科技创新与绿色环保理念的结合,水处理剂和催化剂的研究都朝向环保、实用的理念进行,不仅要给企业带来高效收益,还要为社会创造同步的效益。
蛭石是一种具有独特层状结构的天然、无毒的水铝硅酸盐矿物物质,其化学式为(Mg,Fe,Al)3[(Si,Al)4O10(OH)2].4H2O。蛭石受热易膨胀,其失水造成体积猛增,使得它具有良好的离子交换性、吸附性以及化学稳定性,将其与绿色的光催化技术结合起来,共同处理废水和有害气体,这不仅实现了绿色净化的目的,并且对性能也会有一个质的提升。例如,CN106111104B公开了一种片状锌硅层状双羟基复合氢氧化物光催化剂制备方法及应用,该催化剂以蛭石为基底,采用连续外延的生长方式制备而成,可有效光催化降解4-氯苯酚;CN102658106B公开了一种制备酸化剥离蛭石负载光催化剂的方法,采用水热法制备出一种海绵状三元混相TiO2纳米颗粒,解决了材料不易回收的问题,并且对亚甲基蓝溶液的降解实现了吸附-光催化一体式的处理。然而上述发明所制备的催化剂在实际应用中,降解有机污染物时,都容易产生吸附损失、磨损及脱落的弊端。所以将其做成一种粘合型光触媒剂,尤其是在处理有机污染物及有害气体的时候,将会使催化剂发挥巨大的作用。
发明内容
本发明主要目的是解决上述问题,致力于环保型水处理以及空气净化的研究。本发明提供一种含有蛭石的TiO2-C3N4光触媒剂及其制备方法,该光触媒剂具体包括如下以份数计的原料:蛭石10-20份、异丙醇钛3-7份、尿素5-10份、柠檬酸2-5份、稀盐酸0.5-3份、碳酸钠0.2-3份、聚乙二醇-82-5份以及适量去离子水。
优选地,所述的光触媒剂的浓度为50-250mg/L。
本发明还提供了一种含有蛭石的TiO2-C3N4光触媒剂的制备方法,具体技术方案包括如下步骤:
(1)蛭石的处理:清洗蛭石,用搅碎机将蛭石破碎,然后采用球磨机将蛭石块研磨粉碎,加入1-3mol/L的稀盐酸,持续搅拌过程中升温至55-85℃,并继续搅拌保温0.5h,再进行过滤、干燥,再转移到马弗炉中煅烧,然后将产物研磨细碎,命名为P1;
(2)TiO2的制备:将碳酸钠和去离子水混合均匀,然后在磁力搅拌下,逐滴加入异丙醇钛,搅拌10-20min,转移至反应釜中,进行水热反应;反应结束后,将其洗涤、离心、干燥;
(3)TiO2-C3N4分散液的制备:将尿素、柠檬酸以及去离子水混合均匀,然后加入步骤(2)所制备的二氧化钛,超声10-20min,然后转移至反应釜中,进行水热反应;反应结束后,将固体产物超声、离心、洗涤、干燥;然后将其置于管式炉中,通入氮气并进行煅烧;然后将煅烧所得产物加入到去离子水中,并反复超声处理,将所得混合液命名为P2;
(4)蛭石TiO2-C3N4光触媒剂的制备:将P1和P2混合均匀,加入聚乙二醇-8,反复进行超声震荡,搅拌0.5-1h,再进行微波处理;最后进行冷却、除菌,即得一种含有蛭石的TiO2-C3N4光触媒剂。
优选地,步骤(1)所述的球磨机的转速为32r/min,电机功率为45kw,出料粒度为0.074-0.4mm。
优选地,步骤(1)所述的煅烧为在500-800℃下,煅烧1-5h。
优选地,步骤(2)所述的水热为在180-200℃温度区间加热12-24h。
优选地,步骤(3)所述的水热为在150-200℃温度区间加热6-12h。
优选地,步骤(3)或(4)所述的超声条件为在0-10℃水浴中,采用20-50kHz频率的超声仪,超声20min/次。
优选地,步骤(3)所述的煅烧为以2℃/min的速率升温至200℃,保温30min,然后再以5℃/min的速率升温至550℃,煅烧3-8h。
优选地,步骤(4)所述的微波处理为在300-600W,加热5-30min。
与现有技术相比,本发明的技术方案具有如下有益效果:
(1)本发明制备了一种含有蛭石的TiO2-C3N4光触媒剂,其中蛭石主要起吸附作用以及离子交换作用;而TiO2-C3N4光催化剂在化学反应过程中受光激发,二元协同效应不仅增强了材料的光催化氧化还原能力,使得电子与空穴对部分无机物、有机物以及有害气体分子的捕捉能力增强,并且还使得对细菌的细胞膜和固化病毒的蛋白质的破坏能力增强,这导致其具有优异的降解净化功能以及杀菌作用,并且由于二氧化钛具有优异的紫外光吸收特性,可以使被涂物体表面具有良好的抗紫外线老化作用,可延长被涂物体的使用寿命。
(2)本发明制备的一种含有蛭石的TiO2-C3N4光触媒剂具有无毒无味、绿色安全、性质稳定、长效持久等特点,可安全使用于任何材质物体。
具体实施方式
为能进一步了解本发明的发明内容、特征及其优点,通过以下实施例以及对比例来进一步阐述。
实施例1
一种含有蛭石的TiO2-C3N4光触媒剂及其制备方法,其具体步骤如下:
(1)蛭石的处理:清洗20份蛭石,用搅碎机将蛭石破碎,然后采用球磨机将蛭石块研磨粉碎,加入3份1-3mol/L的稀盐酸稀盐酸,持续搅拌过程中升温至75℃,并继续搅拌保温0.5h;再进行过滤、干燥,再转移到马弗炉中,在700℃下煅烧3h,然后将产物研磨细碎,命名为P1;
(2)TiO2的制备:将3份碳酸钠和45份去离子水混合均匀,然后在磁力搅拌下,逐滴加入7份异丙醇钛,搅拌10min,转移至反应釜中,在200℃下进行24h的水热反应;反应结束后,将其洗涤、离心、干燥;
(3)TiO2-C3N4分散液的制备:将10份尿素、5份柠檬酸以及33份去离子水混合均匀,然后加入2份步骤(2)所制备的二氧化钛,超声20min,然后转移至反应釜中,在150℃下进行12h的水热反应;反应结束后,将固体产物超声、离心、洗涤、干燥;然后将其置于管式炉中,通入氮气并以2℃/min的速率升温至200℃,先进行预热30min,然后再以5℃/min的速率升温至550℃,煅烧4h。
(4)蛭石TiO2-C3N4光触媒剂的制备:将P1和P2混合均匀,加入5份聚乙二醇-8,反复进行超声震荡,搅拌1h,再在500W下进行20min微波加热;最后进行冷却、除菌,即得一种含有蛭石的TiO2-C3N4光触媒剂。
实施例2
一种含有蛭石的TiO2-C3N4光触媒剂及其制备方法,其具体步骤如下:
(1)蛭石的处理:清洗15份蛭石,用搅碎机将蛭石破碎,然后采用球磨机将蛭石块研磨粉碎,加入1.5份1-3mol/L的稀盐酸,持续搅拌过程中升温至75℃,并继续搅拌保温0.5h;再进行过滤、干燥,再转移到马弗炉中,在700℃下煅烧3h,然后将产物研磨细碎,命名为P1;
(2)TiO2的制备:将3份碳酸钠和45份去离子水混合均匀,然后在磁力搅拌下,逐滴加入5份异丙醇钛,搅拌10min,转移至反应釜中,在200℃下进行24h的水热反应;反应结束后,将其洗涤、离心、干燥;
(3)TiO2-C3N4分散液的制备:将7份尿素、5份柠檬酸以及37份去离子水混合均匀,然后加入1份步骤(2)所制备的二氧化钛,超声20min,然后转移至反应釜中,在150℃下进行12h的水热反应;反应结束后,将固体产物超声、离心、洗涤、干燥;然后将其置于管式炉中,通入氮气并以2℃/min的速率升温至200℃,保温30min,然后再以5℃/min的速率升温至550℃,煅烧4h。
(4)蛭石TiO2-C3N4光触媒剂的制备:将P1和P2混合均匀,加入5份聚乙二醇-8,反复进行超声震荡,搅拌1h,再在500W下进行20min微波加热;最后进行冷却、除菌,即得一种含有蛭石的TiO2-C3N4光触媒剂。
实施例3
一种含有蛭石的TiO2-C3N4光触媒剂及其制备方法,其具体步骤如下:
(1)蛭石的处理:清洗10份蛭石,用搅碎机将蛭石破碎,然后采用球磨机将蛭石块研磨粉碎,加入1份1-3mol/L的稀盐酸,持续搅拌过程中升温至70℃,并继续搅拌保温0.5h;再进行过滤、干燥,再转移到马弗炉中,在700℃下煅烧3h,然后将产物研磨细碎,命名为P1;
(2)TiO2的制备:将3份碳酸钠和45份去离子水混合均匀,然后在磁力搅拌下,逐滴加入3份异丙醇钛,搅拌10min,转移至反应釜中,在200℃下进行24h的水热反应;反应结束后,将其洗涤、离心、干燥;
(3)TiO2-C3N4分散液的制备:将5份尿素、3份柠檬酸以及41份去离子水混合均匀,然后加入1份步骤(2)所制备的二氧化钛,超声20min,然后转移至反应釜中,在180℃下进行12h的水热反应;反应结束后,将固体产物超声、离心、洗涤、干燥;然后将其置于管式炉中,通入氮气并以2℃/min的速率升温至200℃,保温30min,然后再以5℃/min的速率升温至550℃,煅烧4h。
(4)蛭石TiO2-C3N4光触媒剂的制备:将P1和P2混合均匀,加入5份聚乙二醇-8,反复进行超声震荡,搅拌1h,再在500W下进行20min微波加热;最后进行冷却、除菌,即得一种含有蛭石的TiO2-C3N4光触媒剂。
对比例1
本发明对比例1与实施例3的区别在于没有添加蛭石。
对比例2
本发明对比例2与实施例3的区别在于没有掺杂蛭石和二氧化钛(TiO2)。
本次实验的降解对象选自甲醛、甲苯、丙酮以及罗丹明B染液和甲基橙染液;对本发明实施例1-3所制备的一种蛭石-TiO2-C3N4光触媒剂和对比例1-2制备的光触媒剂进行有机物降解测试,实验分为暗反应吸附以及光反应催化测试两部分,其作用效果具体如表1以及表2所示。
(1)气相降解有机污染物实验:将上述5种光触媒剂倒入不同反应皿中,做好标记,再分别置于密闭的气相光催化反应器中,然后将氙灯固定到距装置顶端2cm的位置,开始注射0.01mL有机污染物(甲醛、甲苯和丙酮),首先进行30分钟的暗反应过程,并在暗反应结束后抽取0.002mL气体,进行第一次取样,将抽取的气体及时打入气相色谱中,记录峰面积;然后打开光源进行光反应测试,每10min取一次样品,每次抽取0.002mL气体,将抽取的气体及时打入气相色谱中,记录峰面积;总计1.5h后结束实验,观察有机污染物的降解情况。
(2)液相降解染液实验:分别配置10-4mol/L浓度的罗丹明B溶液与甲基橙溶液作为降解染液,采用氙灯作为模拟光源;将100mg光触媒剂加入100mL染液中,将烧杯置于恒温磁力搅拌器上,并将氙灯固定到距反应液面10cm的距离,首先进行30分钟的暗反应过程。待暗反应结束后,打开光源开始光反应测试,每5min取一次样品,总计1.5h后结束实验,最后将这些样品进行紫外分析,根据吸光度的差别,换算成降解率。
表1:实施例1-3和对比例1-2所制备的光触媒剂在暗反应测试中对有机污染物的降解情况
由表1数据可以观察到,对比例1和对比例2所制备的光触媒剂吸附能力较低,而本发明实施例1-3所制备的一种含有蛭石的TiO2-C3N4光触媒剂在暗反应测试过程中,具有优异的吸附效果,可以提高对有机污染物的降解能力。
表2:实施例1-3和对比例1-2所制备的光触媒剂在光反应催化测试中对有机污染物的降解情况
由表2数据可以观察到,本发明实施例1-3所制备的一种含有蛭石的TiO2-C3N4光触媒剂具有优异的降解效果,其在暗反应吸附以及光降解测试后,对有机污染物的降解率可保持在90%以上。
(3)抗紫外线实验:采用紫外灯作为光源,将本发明实施例1-3所制备的一种含有蛭TiO2-C3N4光触媒剂以及和对比例2所制备的光触媒剂作为测试样品,将皮制品布料作为被照射物体,将光触媒剂与其保持100-400cm的距离,进行为期一周的照射实验,观察被涂物体表面的特征变化,其测试结果如表3所示。
表3:实施例1和对比例2所制备的光触媒剂的抗紫外测试
由表3可以观察到,本发明实施例1所制备的一种含有蛭石TiO2-C3N4的光触媒剂还具有良好的的抗紫外线性能,持续的紫外照射不会影响到被涂物体,如果将其应用于衣物或者家具除味时,也可以防止阳光暴晒对其产生的影响。
本发明所列举的各种原料,以及本发明各原料的上下区间取值,以及工艺参数(如温度、时间等)的上下区间取值都能实现本发明,在此不一一列举实施例。以上所述是本发明的优选实施方式而已,当然不能以此来限定本发明之权利范围,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,还可以做出若干改进和变动,这些都属于本发明的保护范围。这些改进和变动也视为本发明的保护范围。
Claims (9)
1.一种含有蛭石的TiO2-C3N4光触媒剂,其特征在于,所述的光触媒剂具体包括如下以重量份数计的原料:蛭石10-20份、异丙醇钛3-7份、尿素5-10份、柠檬酸2-5份、稀盐酸0.5-3份、碳酸钠0.2-3份、聚乙二醇-82-5份以及适量去离子水。
2.根据权利要求1所述的一种含有蛭石的TiO2-C3N4光触媒剂,其特征在于,所述的光触媒剂的浓度为50-250mg/L。
3.如权利要求1所述的一种含有蛭石的TiO2-C3N4光触媒剂的制备方法,其特征在于,所述的制备方法具体包括如下步骤:
(1)蛭石的处理:清洗蛭石,用搅碎机将蛭石破碎,然后采用球磨机将蛭石块研磨粉碎,加入1-3mol/L的稀盐酸,持续搅拌过程中升温至55-85℃,并继续搅拌保温0.5h,再进行过滤、干燥,再转移到马弗炉中煅烧,然后将产物研磨细碎,命名为P1;
(2)TiO2的制备:将碳酸钠和去离子水混合均匀,然后在磁力搅拌下,逐滴加入异丙醇钛,搅拌10-20min,转移至反应釜中,进行水热反应;反应结束后,将其洗涤、离心、干燥;
(3)TiO2-C3N4分散液的制备:将尿素、柠檬酸以及去离子水混合均匀,然后加入步骤(2)所制备的二氧化钛,超声10-20min,然后转移至反应釜中,进行水热反应;反应结束后,将固体产物超声、离心、洗涤、干燥;然后将其置于管式炉中,通入氮气并进行煅烧;然后将煅烧所得产物加入到去离子水中,并反复超声处理,将所得混合液命名为P2;
(4)蛭石TiO2-C3N4光触媒剂的制备:将P1和P2混合均匀,加入聚乙二醇-8,反复进行超声震荡,搅拌0.5-1h,再进行微波处理;最后进行冷却、除菌,即得一种含有蛭石的TiO2-C3N4光触媒剂。
4.根据权利要求3所述的一种含有蛭石的TiO2-C3N4光触媒剂的制备方法,其特征在于,步骤(1)所述的球磨机的转速为32r/min,电机功率为45kw,出料粒度为0.074-0.4mm。
5.根据权利要求3所述的一种含有蛭石的TiO2-C3N4光触媒剂的制备方法,其特征在于,步骤(1)所述的煅烧为在500-800℃下,煅烧1-5h。
6.根据权利要求3所述的一种含有蛭石的TiO2-C3N4光触媒剂,其特征在于,步骤(2)所述的水热为在180-200℃温度区间加热12-24h。
7.根据权利要求3所述的一种含有蛭石的TiO2-C3N4光触媒剂,其特征在于,步骤(3)所述的水热为在150-200℃温度区间加热6-12h。
步骤(3)或(4)所述的超声条件为在0-10℃水浴中,采用20-50kHz频率的超声仪,超声20min/次。
8.根据权利要求3所述的一种含有蛭石的TiO2-C3N4光触媒剂,其特征在于,步骤(3)所述的煅烧为以2℃/min的速率升温至200℃,保温30min,然后再以5℃/min的速率升温至550℃,煅烧3-8h。
9.根据权利要求3所述的一种含有蛭石的TiO2-C3N4光触媒剂,其特征在于,步骤(4)所述的微波处理为在300-600W,加热5-30min。
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CN115715990A (zh) * | 2022-11-15 | 2023-02-28 | 塔里木大学 | 一种g-C3N4/蛭石/TiO2三元复合材料的制备方法及应用 |
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CN115715990A (zh) * | 2022-11-15 | 2023-02-28 | 塔里木大学 | 一种g-C3N4/蛭石/TiO2三元复合材料的制备方法及应用 |
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