CN116984026B - 一种除醛除臭催化剂及其制备方法和应用 - Google Patents
一种除醛除臭催化剂及其制备方法和应用 Download PDFInfo
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Abstract
本发明涉及一种除醛除臭催化剂及其制备方法和应用，所述除醛除臭催化剂为表面修饰有含氨基的三甲氧基硅烷的改性介孔金属氧化物。用于介孔金属氧化物表面改性的含氨基三甲氧基硅烷可在催化剂表面形成热稳定性层，能够有效延长所述催化剂的使用寿命；表面氨基基团的引入，能够有效去除甲醛、甲硫醇等有毒有害气体；氨基与甲醛反应产生的席夫碱能使所述催化剂表面呈碱性，吸附于所述催化剂表面的甲硫醇在碱性环境下，又可发生缩合产生二硫键，在除醛的同时实现更高的除臭效率；所述介孔金属氧化物具有的还原性可将席夫碱还原为胺，实现催化剂的再生。
Description
技术领域
本发明涉及空气净化催化剂领域，特别涉及一种除醛除臭催化剂及其制备方法和应用。
背景技术
醛类物质是一种有强烈刺激性气味的气体，不仅气味刺鼻，而且会对人体危害大，潜伏期长，被称为“室内污染第一杀手”；醛类物质还是导致新生儿畸形、儿童白血病、青少年记忆力和智力下降的主要原因，被世界卫生组织确定为“致癌和致畸性物质”。因此，市面上用于去除醛类物质的方法也是五花八门，总体而言，可以分为以下几类：
第一类：多孔材料物理吸附，比如活性炭、竹炭和硅藻土等，但这种方法不能分解醛类物质，只能暂时捕捉。当室温升高、吸附饱和时，会再次释放醛类物质，形成二次污染。第二类：在室内种养绿色植物，利用植物的光合作用来消除醛类物质。事实上，植物的呼吸能力相当有限，通常是微克级别。如房间内醛类物质超标，需要摆放数千盆植物，加上持续光照才能起一定效果。第三类：喷涂醛类物质溶解酶，醛类物质溶解酶可以将醛类物质氧化成酸或还原为醇，但是产物的毒性依然存在，而且高浓度的清除剂喷在空气中，会对人产生新的污染危害。第四类：应用空气净化器，在室内空气已经出现污染的情况下，使用空气净化器可以在一定程度上减轻污染程度，但是空气净化器只能起到辅助和补救的作用，并不意味着能从根本上消除空气污染。第五类：光触媒（光催化剂）分解醛类物质，其核心成分一般是纳米二氧化钛（TiO2）。然而，一般的光触媒只能在紫外光激发下才能发生反应。显而易见，对于室内除醛，光触媒几乎不会有任何作用，因为大多数的节能灯、日光灯和LED灯都几乎不含有紫外波段的光。对于不能在可见光波段（400至800nm）发生光催化反应的光触媒来说，即使它别的指标再好，对醛类物质等有害气体的防护效果也是极其有限的。众所周知，太阳光中约4％左右是紫外光，约49％左右是可见光，剩下的是红外光和远红外光。在室内如果利用光触媒除醛，除非安装紫外灯对光触媒进行照射，否则不会起任何催化作用。
再者，醛类物质有其特殊的释放曲线，与温度和湿度相关，现有的化学方法除醛类物质，只能暂时除去表面的醛类物质，无法实现有效的去除。而且，在醛类气体存在的场所，一般都会同时存在硫化物等具有恶臭气味的气体。而那些活性炭或在活性炭上附着酸性或碱性物质的吸附剂，由于寿命短，必须频繁更换。另外，在蜂窝陶瓷上附着金属氧化物的催化剂，氧化分解活性低，而且存在生成大量有害反应副产物的问题。
发明内容
为了在除醛的同时能够实现长效除臭的技术效果，本发明提供了一种除醛除臭催化剂及其制备方法和应用。
一种除醛除臭催化剂，由如式I所示的三甲氧基硅烷对介孔金属氧化物进行表面改性制得；
；
其中，a+c=2-5，b为0-1之间的整数，且a、b、c不同时为0。
发明人在试验中发现，若氨基所连碳链越长，在所述介孔金属氧化物表面接枝的氨基分子与金属氧化物表面越远，氨基与吸附于所述介孔金属氧化物的甲醛、甲硫醇等气体之间的接触反应就越难进行，导致除醛除臭效率的减弱。
在本发明的一些实施方式中，所述介孔金属氧化物包含Mn、Ti、Zn、Cu、Co中的至少一种金属。
在本发明的一些实施方式中，所述介孔金属氧化物至少包含Mn和Cu，且Mn：Cu的摩尔比为4:1-2。发明人在试验中发现，在制备所述介孔金属氧化物时，若Mn与Cu的含量比过大，所述介孔金属氧化物表面酸性较大，不利于对甲硫醇的吸附降解，Mn与Cu的含量比过小，则不利于甲醛的去除。
在本发明的一些实施方式中，所述介孔金属氧化物的制备方法包含如下步骤：
S1：将金属化合物加入醇类溶剂中后，调节溶液pH至酸性，于40-50℃水浴中使其充分溶解，获得溶液A；将介孔模板剂于40-50℃水浴中溶于醇类溶剂，获得溶液B；将溶液A、B混合，搅拌至均匀；
S2：将S1所得溶胶转移至反应容器并密封，50-60℃水浴中老化，老化后将溶胶烘干至干凝胶，焙烧即得所述介孔金属氧化物。
在本发明的一些实施方式中，S1中所述金属化合物为金属的异丙醇盐、硝酸盐、氯化盐中的至少一种；调节溶液pH所用试剂为硝酸、盐酸中的至少一种，使用体积浓度为35-40%，溶液pH调至3-4。
在本发明的一些实施方式中，S2中的老化时间为3-5d。
在本发明的一些实施方式中，所述表面改性介孔金属氧化物的制备方法包含如下步骤：在充入惰性气体的反应容器中加入有机溶剂，然后将所述介孔金属氧化物浸入有机溶剂，加热搅拌，待体系温度升至100-120℃，缓慢加入具有如式I结构的三甲氧基硅烷并回流，待反应结束，抽滤洗涤干燥即得所述表面改性介孔金属氧化物。
在本发明的一些实施方式中，所述介孔金属氧化物与具有式I结构的三甲氧基硅烷的投加质量比为1:1-1.5；回流时间为10-12h。
对于所述除醛除臭催化剂的应用，将所述表面改性介孔金属氧化物制成粉状，均匀地分散于纤维滤芯中，应用到空气净化场景。
有益效果：与现有技术相比，本发明通过在介孔金属氧化物表面接枝含氨基的三甲氧基硅烷，不仅提高了所述介孔金属氧化物的除醛效率，同时，还使其具有优秀的除臭性：氨基与甲醛反应产生的席夫碱使所述催化剂表面呈碱性，而吸附于表面的甲硫醇在碱性环境下即可发生缩合形成稳定的二硫键，稳定并提升了催化剂对甲硫醇的吸附去除率；更为重要的是，所述介孔金属氧化物中含有的锰氧化物具有还原性，可将席夫碱中的碳氮双键还原为胺，使得所述催化剂再生。另外，所用含氨基的三甲氧基硅烷可在所述表面改性介孔催化剂表面形成热稳定层，能够有效延长所述催化剂的使用寿命。
具体实施方式
下面结合实施例对本发明作进一步详细描述。需要说明的是，下面的实施例及对比例为本发明的示例，仅用来说明本发明，而不用来限制本发明。在不偏离本发明主旨或范围的情况下，可进行本发明构思内的其他组合和各种改良。
以下示例性地说明实施例及对比例中所用介孔金属氧化物的制备：
介孔金属氧化物-1
S1：将0.5mol氯化锰加入无水乙醇中后，使用37%浓盐酸调节溶液pH至3-4，于45℃水浴中使其充分溶解，获得溶液A；将介孔模板剂P123于40℃水浴中溶于无水乙醇，获得溶液B；将溶液A、B混合，搅拌至均匀；
S2：将S1所得溶胶转移至反应容器并密封，50℃水浴中老化3d，老化后将溶胶于105℃烘干，然后于350℃焙烧3.5h即得所述介孔金属氧化物-1。
介孔金属氧化物-2
S1：将氯化锰、氯化铜按照摩尔比4:1加入无水乙醇中后，使用37%浓盐酸调节溶液pH至3-4，于45℃水浴中使其充分溶解，获得溶液A；将介孔模板剂P123于40℃水浴中溶于无水乙醇，获得溶液B；将溶液A、B混合，搅拌至均匀；
S2：将S1所得溶胶转移至反应容器并密封，50℃水浴中老化3d，老化后将溶胶于105℃烘干，然后于350℃焙烧3.5h即得所述介孔金属氧化物-2。
介孔金属氧化物-3
S1：将氯化锰、氯化铜、氯化钛按照摩尔比4:1:2加入无水乙醇中后，使用37%浓盐酸调节溶液pH至3-4，于45℃水浴中使其充分溶解，获得溶液A；将介孔模板剂P123于40℃水浴中溶于无水乙醇，获得溶液B；将溶液A、B混合，搅拌至均匀；
S2：将S1所得溶胶转移至反应容器并密封，50℃水浴中老化3d，老化后将溶胶于105℃烘干，然后于350℃焙烧3.5h即得所述介孔金属氧化物-3。
介孔金属氧化物-4
S1：将氯化锰、氯化铜、氯化锌按照摩尔比2:1:2加入无水乙醇中后，使用37%浓盐酸调节溶液pH至3-4，于45℃水浴中使其充分溶解，获得溶液A；将介孔模板剂P123于40℃水浴中溶于无水乙醇，获得溶液B；将溶液A、B混合，搅拌至均匀；
S2：将S1所得溶胶转移至反应容器并密封，50℃水浴中老化3d，老化后将溶胶于105℃烘干，然后于350℃焙烧3.5h即得所述介孔金属氧化物-4。
介孔金属氧化物-5
与介孔金属氧化物-4的制备方法类似，不同在于所用氯化锰、氯化铜、氯化锌的摩尔比为5:1:2。
介孔金属氧化物-6
与介孔金属氧化物-4的制备方法类似，不同在于所用氯化锰、氯化铜、氯化锌的摩尔比为1.5:1:2。
实施例1
在充入氮气的反应容器中加入200ml无水甲苯，然后将5g介孔金属氧化物-1进入无水甲苯中，加热搅拌，待体系温度升至120℃，缓慢滴加5g的3-氨乙基三甲氧基硅烷，回流反应12h，反应结束后抽滤，用甲苯和乙醇冲洗，然后于100℃干燥3-4h，即可得到所述除醛除臭催化剂。
实施例2
在充入氮气的反应容器中加入200ml无水甲苯，然后将5g介孔金属氧化物-2进入无水甲苯中，加热搅拌，待体系温度升至120℃，缓慢滴加6g的3-氨戊基三甲氧基硅烷，回流反应12h，反应结束后抽滤，用甲苯和乙醇冲洗，然后于100℃干燥3-4h，即可得到所述除醛除臭催化剂。
实施例3
在充入氮气的反应容器中加入200ml无水甲苯，然后将5g介孔金属氧化物-3进入无水甲苯中，加热搅拌，待体系温度升至120℃，缓慢滴加7.5g的3-氨苯基三甲氧基硅烷，回流反应12h，反应结束后抽滤，用甲苯和乙醇冲洗，然后于100℃干燥3-4h，即可得到所述除醛除臭催化剂。
实施例4
制备过程同实施例2，不同之处在于所用原料为介孔金属氧化物-4和具有式I-1结构的三甲氧基硅烷。
实施例5
制备过程同实施例1，不同之处在于所用原料为介孔金属氧化物-5。
实施例6
制备过程同实施例1，不同之处在于所用原料为介孔金属氧化物-6。
实施例7
制备过程同实施例4，不同之处在于所用原料为具有式I-2结构的三甲氧基硅烷。
实施例8
制备过程同实施例4，不同之处在于所用原料为具有式I-3结构的三甲氧基硅烷。
对比例1
制备过程同实施例1，不同之处在于所用原料为介孔金属氧化物-1，同时不加入3-氨乙基三甲氧基硅烷。
将上述实施例1-8及对比例1所得除醛除臭催化剂进行性能测试：
除醛除臭性：将所述催化剂压片过筛制成尺寸为40-60目的颗粒，将0.05g催化剂颗粒放入固定床反应器中，反应器中甲醛的浓度为40ppm，甲硫醇的浓度为40ppm，相对湿度为45％～50％，环境温度为22～25℃，气体总流量为3L/min；
热稳定性：将所述催化剂置于200℃下老化2d后，再进行上述除醛除臭操作，处理条件保持一致。
性能测试结果见表1：
由表1中的数据可知，本发明所提供的除醛除臭催化剂具有优秀的除醛除臭性能及一定的热稳定性：在测试中，甲醛去除率达到87%以上，甲硫醇去除率达到92%以上。在经过200℃的快速老化后，其除醛除臭效率虽有轻微降低，但依然能维持在85%以上。对比例1的数据从正面说明，所述催化剂表面接枝的含氨基甲氧基硅烷对于金属氧化物的除醛除臭性能及热稳定性有着较大的贡献。因此，本发明所述除醛除臭催化剂在空气净化领域有着广阔的应用前景。
Claims (7)
1.一种除醛除臭催化剂，其特征在于，由如式I所示的三甲氧基硅烷对介孔金属氧化物进行表面改性制得；
，其中，a+c=2-5，b为0或1，且a、b、c不同时为0；
所述介孔金属氧化物至少包含Mn和Cu，且Mn:Cu的摩尔比为4:1-2；
所述介孔金属氧化物的制备方法包含如下步骤：
S1：将金属化合物加入醇类溶剂中，调节溶液pH至酸性，于40-50℃水浴中使其充分溶解，获得溶液A；将介孔模板剂于40-50℃水浴中溶于醇类溶剂，获得溶液B；将溶液A、B混合，搅拌均匀；
S2：将S1所得溶胶转移至反应容器并密封，50-60℃水浴中老化，老化后将溶胶烘干，焙烧即得所述介孔金属氧化物。
2.根据权利要求1所述除醛除臭催化剂，其特征在于，S1中所述金属化合物为金属的异丙醇盐、硝酸盐、氯化盐中的至少一种。
3.根据权利要求1所述除醛除臭催化剂，其特征在于，S1中所述调节溶液pH所用试剂为硝酸、盐酸中的至少一种；溶液pH调至3-4。
4.根据权利要求1所述除醛除臭催化剂，其特征在于，S2中的老化时间为3-5d。
5.根据权利要求1所述除醛除臭催化剂，其特征在于，所述除醛除臭催化剂的制备方法包含如下步骤：在充入惰性气体的反应容器中加入有机溶剂，然后将所述介孔金属氧化物浸入有机溶剂，加热搅拌，待体系温度升至100-120℃，缓慢加入具有如式I结构的三甲氧基硅烷并回流，待反应结束，抽滤洗涤干燥即得所述除醛除臭催化剂。
6.根据权利要求5所述除醛除臭催化剂，其特征在于，所述介孔金属氧化物与具有式I结构的三甲氧基硅烷的投加质量比为1:1-1.5；回流时间为10-12h。
7.权利要求1-6任意一项所述除醛除臭催化剂的应用，其特征在于，将所述除醛除臭催化剂制成粉状，分散于纤维滤芯中，应用到空气净化场景。
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