CN106622281B - 一种有机配体改性甲醛净化催化剂的制备方法 - Google Patents
一种有机配体改性甲醛净化催化剂的制备方法 Download PDFInfo
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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Abstract
本发明公开了一种有机配体改性甲醛净化催化剂的制备方法，将总含量为氧化钛重量1‑10%的La与Cu、Fe、Ni三种中至少一种与Sn、Mn两种中至少一种进行混合预混，再加水混合制成水溶性盐，再加入氧化钛粉料，经干燥高温焙烧制成改性催化剂载体，再加入到金属Pt有机溶液中，经干燥高温焙烧制成改性催化剂载体粉末，再加入拟薄水铝石和甲基纤维素、水制成改性浆料，将蜂窝孔陶瓷片浸渍在改性浆料中，干燥焙烧冷却还原，得到有机配体改性甲醛净化催化剂。本发明不仅能过滤粉尘、消除异味、杀菌消毒和吸附有害气体，还能完全催化分解甲醛有害气体，使吸附的有害气体不会形成二次污染，再是催化剂层不易脱落和开裂，使用寿命长。
Description
技术领域
本发明涉及室内空气净化技术，尤其是涉及一种有机配体改性净化空气分解甲醛的催化剂及其用催化剂制成的空气净化器。
背景技术
随着工业化进程的不断加快，室内空气污染日趋严重，使得室内空气净化也尤为关注。因此人们对居家环境的质量也有了更高的要求。目前对于室内空气净化大都采用滤网+活性炭滤网紫外线杀菌消毒+静电吸附滤网等方法来吸附粉尘、消除异味、杀菌消毒来净化空气。
随着人们生活水平的提高，居家装修已成为普遍性的时尚，但大量建筑材料和装潢材料又造成了室内空气的污染，这些材料中各种化学添加剂使用量也在不断增加，使得新装修房间内空气中挥发性气体浓度高于室外，甚至高于工业区。因此室内空气除有粉尘颗粒、微生物污染物外，还有化学添加剂产生的甲醛、甲苯、氨等挥发性气体等。其中挥发性气体主要甲醛。而甲醛是一种无色易溶的刺激性气体，当室内含量为 0.1 毫克/立方米时就有异味和不适感；0.5 毫克/立方米可刺激眼睛引起流泪；0.6 毫克/立方米时引起咽喉不适或疼痛；浓度再高可引起恶心、呕吐、咳嗽、胸闷、气喘甚至肺气肿；30 毫克/立方米时可当即导致死亡。长期接触低剂量甲醛还可引起慢性呼吸道疾病和致癌。
目前市场上的空气净化器的种类繁多、功能不尽相同，使用方法也不相同，空气净化器一般设置在室内地面上，也有将净化材料装入框内挂在墙壁上或用袋装式设置有分散设置在室内或移动的空气内。但仅工作原理来分，主要有以下两种：一种是被动吸附过滤式的空气净化器。被动式的空气净化，是用风机将空气抽入机器，通过内置的滤网、活性炭滤网、紫外线杀菌消毒+静电吸附滤网过滤空气，主要能够起到过滤粉尘、消除异味、杀菌消毒和吸附有害气体等作用，但它不能分解有害气体，容易使吸附的有害气体再次脱开形成二次污染；二种是主动式的空气净化器，它常采用银离子、负离子、低温等离子技术，虽然它摆脱了风机与滤网的限制，不是被动的等待室内空气被抽入净化器内进行过滤净化，之后再通过风机排出，而是有效、主动的向空气中释放净化灭菌因子，通过空气弥漫性的特点，到达室内的各个角落对空气进行无死角净化，但该类空气净化器最大的缺陷就是臭氧释放量超标。光触媒技术净化空气是一种以纳米级二氧化钛为代表的具有光催化功能的光半导体材料的新技术，它涂布于基材表面，在光线的作用下，产生催化降解功能，能降解空气中甲醛等有毒有害气体，但净化效率较低。
发明内容
针对上述现有技术中空气净化器所存的问题，本发明提供了一种既可过滤和吸附空气中粉尘颗粒、消除异味、杀菌消毒和吸附有害气体，又可有效分解有害气体，提高净化效率的有机配体改性甲醛净化催化剂的制备方法。
本发明所述有机配体改性甲醛净化催化剂的制备方法步骤是：
1、先用陶瓷原料及辅料经球磨、练泥、成型、烘干定型和高温焙烧制成蜂窝孔陶瓷片，
2、将氧化钛原料球磨粉碎成200目以上的粉料，
3、将总含量为氧化钛粉料重量1-10%的La与Cu、Fe、Ni三种中至少一种与Sn、Mn两种中至少一种进行混合预混，再加两倍氧化钛粉料重量的水混合制成相应的水溶性盐，
4、在搅拌条件下，在水溶性盐中加入步骤b的氧化钛粉料，再水浴蒸干，经100-120oC干燥后，再高温焙烧制成改性催化剂载体，
5、称取硝酸铂溶液，硝酸铂溶液中Pt含量为改性催化剂载体重量0.1-2%，将硝酸铂溶液加入到由甲醇、乙醇两种至少一种与甲醛、乙醛两种中至少一种与乙二醇丁醚组成的有机混合溶剂中，加水配成0.01mol/L金属Pt离子有机溶液，
6、在搅拌条件下，将改性催化剂载体加入金属Pt离子有机溶液中，用碳酸钠调节pH值为碱性，再水浴蒸干，经100-120oC干燥后，再高温焙烧制成改性催化剂载体粉末，
7、在改性催化剂载体粉末中加入其重量5-20%的拟薄水铝石和其重量0.5-2%的甲基纤维素及适量的水，充分球磨搅拌并调节成固含量为20-30%、pH值为酸性的改性浆料，
8、将上述蜂窝孔陶瓷片浸渍在改性浆料中，取出后吹扫孔道残余液，经100-120oC干燥后，再在200-600℃高温焙烧，冷却后将其置于还原炉中，通入体积比为10%氢气和90%氮气形成的混合气体，并加热至200℃保温还原，冷却后得到有机配体改性甲醛净化催化剂。
本发明在制备净化分解甲醛整体式催化剂时，一是以氧化钛催化剂层为载体，再在氧化钛中加入具有分散作用的La与Cu、Fe、Ni三种中至少一种与Sn、Mn两种中至少一种进行预混，使混合物能在氧化钛上形成单层分散，形成强的相互作用，从而提高氧化钛稳定性；二是通过加入La，提高了活性组分Pt的分散度，从而提高催化层的活性、选择性；三是制备过程中，引入有机溶剂为改性催化剂，利用有机溶剂与Pt的络合或者分散作用，改变浸渍液的表面张力，降低催化剂Pt纳米粒子的颗粒大小，提高活性中心的分散度，进而提高催化剂的活性，获得一种室温高效稳定处理甲烷的催化剂；五是在甲醛氧化分解过程中，单质Pt是活性中心，Cu、Fe、Ni能与活性组分Pt形成合金，减缓活性组分的氧化过程，SnO2和Mn2O3具有活泼的低温氧化物种，能促进甲醛的分解，提高催化剂层的活性；四是通过加入拟薄水铝石和甲基纤维素，拟薄水铝石与硝酸作用形成的铝溶胶，可以作为浆料的胶黏剂，加强催化剂与陶瓷载体之间的相互作用，提高催化剂浆料的上载量，降低涂层的脱落率，甲基纤维素作为表面活性剂，可以调高浆料的分散性，提高浆料的流动性，便于涂覆上载，同时亦能降低涂层的脱落率。
本发明通过在以氧化钛为基础的催化剂层中加入Pt活性组分与起分散和稳定作用的金属，使蜂窝孔陶瓷片的表面吸附、催化性能大大增强，在充分过滤粉尘、消除异味、杀菌消毒和吸附有害气体等作用的同时，能完全催化分解甲醛有害气体，使吸附的有害气体不会形成二次污染。再是催化剂层不易脱落和开裂，其使用寿命长。
本发明利用甲醇、乙醇、甲醛、乙醛、乙二醇丁醚能降低浸渍溶液的表面张力，从而改变毛细管作用力，使得进入氧化钛载体孔道结构中的Pt颗粒更细小，根据纳米粒子效应，Pt颗粒越小，暴露的活性中心越多，从而使得催化剂活性更高。同时甲醇、乙醇、甲醛、乙醛、乙二醇丁醚本身具有还原性，使得一部分PtO颗粒在的在焙烧过程中，直接还原成更为高效的Pt单质，而这一部分还原出来的Pt，能更为稳定的存在氧化钛的孔道结构中。碳酸钠溶液调节pH为碱性为了使进入载体孔道结构的Pt沉淀，防止在干燥过程中，部分Pt随溶剂挥发溢出。
本发明所述的有机配体改性甲醛净化催化剂包括蜂窝孔陶瓷片和浸渍涂覆在蜂窝孔表面上并由氧化钛、活性金属和起分散、稳定作用的金属或金氧化物组成的催化层通过高温焙烧制成。它可以用来制成箱式的空气净化器，也可以填充在框体中制成悬挂式净化器，还可以制成各种袋装空气净化器放置办公桌上、茶几上、沙发上以及汽车内的某个位置。
用本发明所述催化剂制成的空气净化器进行室内空气净化，经专业部门多次检测室内空气中甲醛含量均在0.08mg/m3以下。
具体实施方式
实施例1
本发明所述有机配体改性甲醛净化催化剂的制备方法步骤是：
1、先用40-50wt%的氧化铝（粉）、30-40wt%二氧化硅（粉）及10-30wt%的粘接剂、润滑剂和熔剂组成的辅料，加适量水经球磨、练泥、成型、烘干定型和高温焙烧制成蜂窝孔陶瓷片，蜂窝孔陶瓷片呈圆柱形，直径为25毫米，高度为12.5毫米，蜂窝孔目数为300目；
2、用氧化钛原料球磨粉碎成250目的氧化钛粉料；
3、将总含量为氧化钛粉料重量5%的La、Cu与Mn的粉末先预混，再加两倍氧化钛粉料重量的水混合制成相应的水溶性盐，La（镧）、Cu与Mn的重量比为4∶3∶3，
4、在搅拌条件下，在水溶性盐中加入步骤b的氧化钛粉料，再用80oC水浴蒸干，经120oC干燥12小时后，再在600oC高温焙烧4小时制成改性催化剂载体，
5、称取硝酸铂溶液，其中硝酸铂溶液中Pt含量为改性催化剂载体重量0.4%，将硝酸铂溶液加入到由重量比为4∶4∶2的甲醇、乙醛与乙二醇丁醚组成的有机溶混合剂中，加水配成0.01mol/L金属Pt离子有机溶液，
6、在搅拌条件下，将改性催化剂载体加入金属Pt离子有机溶液中，用0.1mol/L的碳酸钠溶液调节pH值为8，再用80oC水浴蒸干，经120oC干燥12小时后，再在200-600oC高温焙烧4小时制成改性催化剂载体粉末，
7、在改性催化剂载体粉末中加入其重量10%的拟薄水铝石和其重量1%的甲基纤维素和适量的水，充分球磨搅拌并调节成固含量为20-30%、pH值为4的酸性改性浆料，
8、将上述蜂窝孔陶瓷片浸渍在改性浆料中，浸渍5min后取出，吹扫孔道残余液，经100-120oC干燥后，再在200-600℃高温焙烧4小时，冷却后将其置于还原炉中，通入体积比为10%氢气和90%氮气形成的混合气体，并加热至200℃保温还原，冷却后得到有机配体改性甲醛净化催化剂。
所述金属Pt也可用Pd（钯）、Rh（铑）或金（Au）代用。所述适量的水表示将其调节为固含量为20-30%、pH值为4.5的酸性改性浆料时所用的水。
实施例2，
所述有机配体改性甲醛净化催化剂的制备方法步骤是：
1、先用40-50wt%的氧化铝（粉）、30-40wt%二氧化硅（粉）及10-30wt%的粘接剂、润滑剂和熔剂组成的辅料，加适量水经球磨、练泥、成型、烘干定型和高温焙烧制成蜂窝孔陶瓷片，蜂窝孔陶瓷片呈圆柱形，直径为25毫米，高度为12.5毫米，蜂窝孔目数为300目；
2、用氧化钛原料球磨粉碎成250目的氧化钛粉料；
3、将总含量为氧化钛粉料重量3-5%的La、Fe与Sn的粉末先预混，再加两倍氧化钛粉料重量的水混合制成相应的水溶性盐，La（镧）、Fe与Sn的重量比为4∶3∶3，
4、在搅拌条件下，在水溶性盐中加入步骤b的氧化钛粉料，再用80oC水浴蒸干，经120oC干燥12小时后，再在600oC高温焙烧4小时制成改性催化剂载体，
5、称取硝酸铂溶液，其中硝酸铂溶液中Pt含量为改性催化剂载体重量0.4%，将硝酸铂溶液加入到由重量比为5∶3∶3的乙醇、乙、甲醛与乙二醇丁醚组成的有机溶混合剂中，加水配成0.01mol/L金属Pt离子有机溶液，
6、在搅拌条件下，将改性催化剂载体加入金属Pt有机溶液中，用0.1mol/L的碳酸钠溶液调节pH值为8碱性，再用80oC水浴蒸干，经120oC干燥12小时后，再在200-600oC高温焙烧4小时制成改性催化剂载体粉末，
7、在改性催化剂载体粉末中加入其重量10%的拟薄水铝石和其重量1%的甲基纤维素和适量的水，充分球磨搅拌并调节成固含量为20-30%、pH值为4的酸性改性浆料，
8、将上述蜂窝孔陶瓷片浸渍在改性浆料中，浸渍5min后取出，吹扫孔道残余液，经100-120oC干燥后，再在200-600℃高温焙烧4小时，冷却后将其置于还原炉中，通入体积比为10%氢气和90%氮气形成的混合气体，并加热至200℃保温还原，冷却后得到有机配体改性甲醛净化催化剂。
所述金属Pt也可用Pd（钯）、Rh（铑）或金（Au）代用。所述适量的水表示将其调节为固含量为20-30%、pH值为4.5的酸性改性浆料时所用的水。
Claims (2)
1.一种有机配体改性甲醛净化催化剂的制备方法，其特征是：所述方法步骤是：
a、先用陶瓷原料及辅料经球磨、练泥、成型、烘干定型和高温焙烧制成蜂窝孔陶瓷片，
b、将氧化钛球磨粉碎成200目以上的粉料；
c、将总含量为氧化钛粉料重量1-10%的La与Cu、Fe、Ni三种中至少一种与Sn、Mn两种中至少一种进行混合预混，再加两倍氧化钛粉料重量的水混合制成相应的水溶性盐，
d、在搅拌条件下，在水溶性盐中加入步骤b的氧化钛粉料，再水浴蒸干，经100-120oC干燥后，再高温焙烧制成改性催化剂载体，
e、称取硝酸铂溶液，硝酸铂溶液中Pt含量为改性催化剂载体重量0.1-2%，将硝酸铂溶液加入到由甲醇、乙醇两种至少一种与甲醛、乙醛两种中至少一种与乙二醇丁醚组成的有机混合溶剂中，加水配成0.01mol/L金属Pt离子有机溶液，
f、在搅拌条件下，将改性催化剂载体加入金属Pt离子有机溶液中，用碳酸钠调节pH值为碱性，再水浴蒸干，经100-120oC干燥后，再高温焙烧制成改性催化剂载体粉末，
g、在改性催化剂载体粉末中加入其重量5-20%的拟薄水铝石和其重量0.5-2%的甲基纤维素及适量的水，充分球磨搅拌并调节成固含量为20-30%、pH值为酸性的改性浆料，
h、将上述蜂窝孔陶瓷片浸渍在改性浆料中，取出后吹扫孔道残余液，经100-120oC干燥后，再在200-600℃高温焙烧，冷却后将其置于还原炉中，通入体积比为10%氢气和90%氮气形成的混合气体，并加热至200℃保温还原，冷却后得到有机配体改性甲醛净化催化剂。
2.一种用权利要求1所述方法制成的催化剂制成的空气净化器，其特征是：所述空气净化器为箱式空气净化器，悬挂式净化器或空气净化袋。
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| CN104174395A (zh) * | 2014-08-04 | 2014-12-03 | 南昌大学 | 室温消除甲醛稀土改性负载型贵金属整体催化剂制备方法 |
| CN105561685A (zh) * | 2014-10-15 | 2016-05-11 | 康宁股份有限公司 | 蜂窝空气过滤器及其方法 |
| CN105289298A (zh) * | 2015-10-27 | 2016-02-03 | 展宗城 | 一种室温下消除甲醛的催化模块及其制备方法 |
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