CN1004401B - 低温无焰燃烧催化剂及其制法 - Google Patents
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Abstract
本发明提出一种以硅酸铝纤维为第一担体，活性氧化物为第二担体，含有贵金属及稀土金属和碱土金属氧化物为助催化剂的新型的低温无焰燃烧催化剂及其制备方法。本发明的催化剂可用于做软便安全的热源以及某些工业有害气体的污染消除。
Description
本发明属于一种包含贵金属的催化剂及其制备方法。
目前国外对低温无焰燃烧催化剂有一定研究。如英国专利894，612;1，336，617;2，019，240A;美国专利3，697，447;3，802，856;3，835，066;3，867，311;4，048，092;法国专利2，395，067;2，539，327等。这些专利所报导的催化剂，其担体为石棉、玻璃纤维、氧化铝纤维、硅酸铝纤维等或它们的混合体。以Pt、Pd、Rh或者它们的组合为活性金属，有的还添加Co、Ni或稀土氧化物，用喷涂或浸渍的方法使其沉积在担体上。这些催化剂各有其特点，制法及用途也不尽相同。
本发明的目的在于提出一种以活化金属氧化物作为第二担体、贵金属用量低、含有稀土和碱土金属的低成本、高性能的新型低温无焰燃烧催化剂。
本发明的内容为：
1.选用一种耐火纤维作为担体，在这种担体上沉积或涂布一种活性氧化铝作为第二担体，使担体比表面积扩大。第二担体重量占催化剂总重量的3～10%。
2.选用贵金属Pt或Pd或二者的组合作为活性金属组分，Pt与Pd的重量比为0.25～1∶1。贵金属在催化剂中的含量（wt%）为0.07～0.15。
3.选用稀土氧化物CeO2或La2O3以及一种碱土金属的氧化物，最好为MgO作为助催化剂。稀土氧化物在催化剂中含量（wt%）为0.8～1.8，碱土金属氧化物为0.5～2。
4.制作工艺包括以下步骤：
（1）先将耐火纤维洗净制成滤饼作为第一担体，再吸入可溶性铝盐溶液，干后用稀氨水处理，然后在110℃下陈化干燥，再升温400℃，活性氧化铝沉积在滤饼上成为第二担体。
（2）用浸渍或均匀滴入的方法在滤饼上加铈或镧的硝酸盐或醋酸盐溶液，晾干后用氨水浸泡，取出用清水洗涤、110℃烘干，升温500℃分解为CeO2或La2O3。
（3）加入碱土金属的硝酸盐，最好是Mg（NO3）2溶液，晾干后烘干。
（4）加入Pt或Pd的可溶性化合物或二者组合的溶液，110℃烘干，升温500℃，使其分解而得到最终产物。
本发明中的耐火纤维是山东耐火材料厂生产的工业品硅酸铝纤维，其化学成份为：Al2O346～56%，SiO248～53%，Fe2O3≤1.2%，纤维直径1～4微米。
本发明中所说的Pt、Pd的可溶性化合物是指Pt、Pd的氯络合酸、氨络合物、氯化物;Pd的硝酸盐。
本发明的催化剂可用于丙烷、丁烷、甲烷/天然气，液化石油汽、汽油、苯、甲苯、二甲苯的无焰催化燃烧，除了用作轻便、安全的热源的催化剂如家庭取暖，野外取暖，小型运输车船，小型生产车间取暖，孵鸡，油漆烘干等，还可用于工业有害蒸汽苯、甲苯、二甲苯的污染消除。
实施例：
1.硅酸铝纤维15g，洗净，搅成浆状，倒入方形布氏漏斗中，真空抽滤，制成片状滤饼，干后厚度约为1.5mm，长宽各为21.8cm，重14.5g。将滤饼吸入150ml 5%Al（NO3）3·9H2O溶液，晾干后在110℃干燥3小时，干燥纤维片放入1∶1NH4OH中热至90℃并保持5分钟，取出用热水浸洗三次，晾干后在110℃烘2小时，放在马弗炉中在160℃下保温30分钟，然后升温至400℃保温3小时。经此处理的纤维担体85-IA比表面积为16m2/g，比未经处理的担体（比表面积为0.32M2/g）提高约50倍。
均匀滴加116Ml浓度为0.4725g Ce（NO3）·6H2O/100ml的溶液于85-IA纤维担体中，晾干后在110℃烘干3小时，冷后在1∶1NH4OH中热至90℃并浸3～5分钟，取出用清水洗涤，晾干后在110℃烘干3小时，升温至250℃并保持/小时，再升温至500℃锻烧3小时，得到含CeO2的样品85-IAC。
再均匀滴加116ml浓度为1.65g Mg（NO3）2·6H2O/100ml的溶液，晾干后在110℃烘干3小时，得到85-IACM，继续均匀滴加浓度为12.5mgPd/100ml的Pd（NO3）2溶液116ml，晾干后在110℃烘干2小时，然后升温至250℃并保持1小时，升温至500℃燃烧2小时，得到最终催化剂产品85-IACMP。
2.将一片加入Mg（NO3）2的纤维均匀滴加Pt和Pd的混合溶液197ml（浓度为12.5mg Pd/100ml的Pd（NO3）2溶液81ml加上浓度为3.75mg Pt/100ml的H2PtCl6溶液116ml）。晾干后在110℃烘干2小时，然后升温250℃保持/小时，再升温500℃煅烧2小时，得到催化剂产品85-IACMPP。
3.在一片经过如实施例/中加Al（NO3）2溶液处理后的纤维担体85-IA上均匀滴加浓度为0.375g La（NO3）3·6H2O/100ml的溶液116ml，晾干后在110℃烘干3小时，冷后用1∶1NH4OH中热至90℃并保持3～5分钟，取出用清水洗涤三次，晾干后在110℃烘干3小时，升温至250℃并保持/小时，再升温至500℃煅烧3小时，再用实施例/中的方法在上面载上MgO及Pd，得到催化剂产品85-IALMP。
4.在按实施例3处理的滴加了La（NO3）3溶液的85-IAL纤维片上滴加浓度为1.65g Mg（NO3）2·6H2O/100ml的溶液116ml，晾干后烘干3小时，得到85-IALM，再滴加Pd和Pt的混合溶液197ml（与实施例2相同），晾干后烘干，升温至250℃保持1小时，升温至500℃煅烧2小时，得到催化剂产品85-IALMPP。
四个实施例中的催化剂成份如表Ⅰ。
表Ⅰ，催化剂成分
用一种简便的低温无焰燃烧器如附图所示的手炉来检验本发明的催化剂的实用效果。将表Ⅰ中的催化剂以及85-IACM，85-IALM分别冲成φ＝30mm的小园片。用85-IACMP或85-IACMPP放在上面，用85-IACM放在下面（如附图所示），或用85-IALMP或85-IALMPP放在上面，85-IALM放在下面。用汽油作燃料，滴数滴乙醇在燃烧床上，用火柴点燃（85-IACMP，85-IACMPP不用滴酒精，用火柴点数秒至30秒即可燃着），酒精燃完后，催化剂即达一定温度，汽油蒸汽在界面处与空气接触发生反应而燃烧。检测结果如下：
（1）催化剂起燃温度低，易点燃。
（2）燃烧时床面红亮均匀，无明火焰，未嗅到酸味或其它刺激气味。
（3）经测量，使用中催化床床中温度为320～395℃，平均350℃;床边温度370～400℃，平均390℃;排气口温度97～104℃，平均102℃;炉壳温度为60～63℃，平均62℃。
（4）催化剂寿命列于表Ⅱ。
表Ⅱ，催化剂寿命
为了定量说明催化剂的活性，将0.4g 85-IACMP催化剂填充于内径0.4cm硬质玻管制成的反应器内，保持催化床长度为17cm，将其放入可控温的管式炉内，将炉温升至203℃，并保温使催化剂温度达到平衡。以丁烷为燃料，按C4H10∶O2＝1∶9（V/V）的比例注入10μl的混合气。用色谱仪监测经催化床氧化后排出的丁烷，由记录的数据计算得转化率为62%。再升温至283℃，303℃，323℃，分别计算得丁烷的转化率为77.8%，97.0%，100%。说明在323℃实验条件下，丁烷可全部燃烧生成CO2和H2O。在色谱仪上也未检出CO或其他部分氧化的化合物。
附图说明
1.金属上壳
2.金属下壳
3.可卸燃烧头
4.85-IACMP催化剂（燃烧床）
5.85-IACM
6.铜丝网
7.棉花（汽油浸透）
8.热气出口
9.空气入口
Claims (19)
1、一种担体为硅酸铝纤维，包含有贵金属及稀土金属氧化物的低温无焰燃烧催化剂，其特征在于其组分及含量为：
①活性氧化铝为第二担体，占催化剂重量3～10%。
②活性金属，至少包含Pt、Pd中一种贵金属，占催化剂重量0.07～0.15%。
③稀土金属Ce或La的氧化物，占催化剂重量0.8～1.8%。
④碱土金属氧化物，占催化剂重量0.5～2%。
⑤余量为硅酸铝耐火纤维担体。
2、按照权利要求1所说的催化剂，其特征在于所说的硅酸铝纤维担体为山东耐火材料厂生产的工业品，其成分为：Al2O346～56%，SiO248～53%，Fe2O3≤1.2%。
3、按照权利要求1所说的催化剂，其特征在于所说的活性金属为Pt或Pd或二者的组合。Pt、Pd组合活性金属的重量比为Pt∶Pd＝0.25～1∶1。
4、按照权利要求1所说的催化剂，其特征在于所说的碱土金属氧化物最为好MgO。
5、一种制备权利要求1～4中催化剂的方法，其特征在于方法包括以下步骤：
（1）洗净硅酸铝纤维，制成滤饼。
（2）将可溶性铝盐溶液均匀滴加或浸到滤饼上，干燥后用氨水处理，110℃烘干并陈化后，在400℃煅烧。
（3）将Ce或La的可溶盐溶液滴加或浸到担体中，干后，用氨水处理，110℃干燥后，升温至500℃煅烧。
（4）加入碱土金属可溶盐溶液，再加入含Pt或Pd或二者组合的可溶性化合物的溶液，110℃下干燥，500℃下煅烧。
6、按照权利要求5所说的催化剂的制备方法，其特征在于：
（1）所说的可溶性铝盐为Al（NO3）3·9H2O。
（2）所说的Ce、La的可溶性盐为醋酸盐或硝酸盐。
（3）所说的碱土金属可溶性盐最好为Mg（NO3）2·6H2O。
7、按照权利要求5所说的催化剂的制备方法，其特征在于所说的含Pt、Pd的可溶性化合物为Pt、Pd的氯络合酸、氨络合物、氯化物，Pd的硝酸盐。
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| CN87105167.2A CN1004401B (zh) | 1987-07-23 | 1987-07-23 | 低温无焰燃烧催化剂及其制法 |
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| CN87105167.2A CN1004401B (zh) | 1987-07-23 | 1987-07-23 | 低温无焰燃烧催化剂及其制法 |
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| CN1004401B true CN1004401B (zh) | 1989-06-07 |
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| WO2011009283A1 (zh) * | 2009-07-23 | 2011-01-27 | 中国科学院大连化学物理研究所 | 煤层气脱氧催化剂机器制备方法和应用 |
| CN101632928B (zh) * | 2009-08-14 | 2014-10-01 | 昆明理工大学 | 火焰燃烧合成法一步制备nsr催化剂 |
| TWI576892B (zh) * | 2015-01-27 | 2017-04-01 | 國立中山大學 | 以燃燒反應生成物游離樣品並藉以進行質譜分析的方法及裝置 |
| CN107469832B (zh) * | 2017-07-24 | 2019-02-05 | 广东本立环保技术有限公司 | 一种用于含氯有机物废气催化燃烧催化剂及其制备方法 |
| CN115845845B (zh) * | 2022-11-21 | 2024-07-23 | 北京沐秀新能源科技有限公司 | 一种用于低品质油田伴生气无焰燃烧的催化剂及其制备方法与应用 |
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