CN106378132A - 一种有机废气净化催化剂及其制备方法 - Google Patents
一种有机废气净化催化剂及其制备方法 Download PDFInfo
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Abstract
本发明提供一种有机废气净化催化剂及其制备方法。该催化剂以Al2O3作为载体,以贵金属Pd、Pt作为主要催化活性组分,以Ni、Mn、Ce、Rh、Ru、Zr、La、Nb、Ti中的一种或几种以及碱金属和碱土金属中的一种或几种作为催化助剂。上述催化剂可以以颗粒、条状以及环状催化剂的形式应用,也可以将Al2O3和全部催化活性组分以及助剂担载在蜂窝陶瓷上制成整体催化剂。本发明的催化剂具有活性高、水热稳定性高、长寿命等优点;该催化剂可用于有机废气中烷烃、芳烃等挥发性有机物的高效脱除,起燃温度低,能够广泛应用于工业有机废气的净化处理,实现能源的充分利用、节能与环保的目的。
Description
技术领域
本发明涉及一种有机废气净化催化剂及其制备方法。
背景技术
石油化工、精细化工、涂料、制药、皮革、纺织印染等行业的生产过程中,都会释放出碳烃化合物、甲苯、二甲苯、苯乙烯、乙酸乙酯、丙酮、甲醛等挥发性有机化合物。挥发性有机废气是造成大气污染的主要有害物之一,它们如果不经处理直接排入大气会造成严重的环境污染。
催化燃烧是净化挥发性有机废气最有效的方法之一,它利用有机废气净化催化剂的作用下,可在较低温度发生氧化反应,生成CO2 和H2O 而除去,其核心技术是催化剂。近年来,随着人们对环境问题的重视,这一技术在国内外得到了大量研究和快速的发展。
现有的有机废气净化催化剂普遍存在催化剂活性和稳定性不高、水热稳定性不好、寿命较短以及生产成本高等缺陷。因此,研制出高活性、高稳定性、高寿命、低成本的有机废气净化催化剂是十分具有实用价值的。
发明内容
本发明的目的是克服现有技术存在的上述不足,提供一中净化有机废气的催化剂及其制备方法。
本发明可以通过以下技术方案予以实现:
一种有机废气净化催化剂,其特征在于:该催化剂包含主要活性组分、助剂、载体;其中:主要活性组分选自贵金属Pd、Pt,其含量以单质金属计,Pd的含量为催化剂总重量的0.05wt%~0.2wt%;Pt的含量为整个催化剂总重量的0.1wt%~0.4wt%;
助剂包括助剂一和助剂二;助剂一选自Ni、Mn、Ce、Rh、Ru、Zr、La、Nb、Ti中的一种或几种,其含量以单质金属计,为催化剂总重量的0.02wt%~5wt%;
助剂二选自碱金属和碱土金属中的一种或几种,其含量以单质金属计,为催化剂总重量的0.05wt%~3wt%;
所述催化剂为颗粒、条状以及环状催化剂,载体为Al2O3;或为负载主要活性组分、助剂的整体催化剂;
上述的有机废气净化催化剂,Pd的含量优选为催化剂总重量的0.09wt%~0.16wt%;Pt的含量优选为整个催化剂总重量的0.12wt%~0.27wt%;
上述的有机废气净化催化剂,其助剂一选自Ni、Mn、Ce、Rh、Ru、Zr、La、Nb、Ti中的一种或几种,其含量优选为催化剂总重量的0.1wt%~ 3.3wt%;
上述的有机废气净化催化剂,其助剂二选自碱金属和碱土金属中的一种或几种,其含量优选为催化剂总重量的0.09wt%~1.6wt%;
所述催化剂可用于有机废气中烷烃、芳烃的高效脱除,起燃温度低,能够广泛应用于工业有机废气的净化处理,具有较好的催化活性及水热稳定性。
本发明还提供一种净化有机废气催化剂的制备方法,根据应用工况的不同,可分为颗粒、条状以及环状催化剂的制备和蜂窝陶瓷整体催化剂的制备,具体步骤如下:
1、颗粒、条状以及环状催化剂制备过程依次如下:
(1) 颗粒、条状以及环状催化剂载体的制备:将拟薄水铝石、硝酸铝和氯化铝的混合物分别进行滚球、挤条或压片成型,100~150℃干燥2~6h,400~900℃焙烧3~6h,得到Al2O3催化剂载体;
(2) 助剂二的负载:将助剂二的前驱体溶液采用等体积浸渍的方式浸渍到颗粒、条状以或环状催化剂Al2O3载体上,100~150℃干燥2~6h,300~500℃焙烧3~6h;
(3) 助剂一及主要活性组分的负载:调节助剂一和主要活性组分的前驱体混合溶液的PH值,浸渍到已经负载助剂二的催化剂上,浸渍时间为10~60min,100~150℃干燥2~6小时,300~500℃焙烧3~6h,得到非均匀型蛋壳型催化剂。
2、整体催化剂制备过程依次如下:
涂层浆料制备:按照权利要求1 所述比例称取主要活性组分及助剂的前驱体、拟薄水铝石粉,加入适量硝酸调节PH值,用球磨机球磨5-24h,得到有机废气净化催化剂作为蜂窝陶瓷载体涂层的涂层浆料;
将上述浆料一次均匀涂覆到蜂窝陶瓷载体上,并用高压气体吹出蜂窝陶瓷载体孔隙内多余的浆液;100~150℃干燥2~6h,300~600℃焙烧3~6h,得到有机废气净化催化剂。
本发明为了满足不同工况,提供了颗粒、条状以及环状有机废气净化催化剂和蜂窝陶瓷整体有机废气净化催化剂。本发明的制备方法工艺简单,无需昂贵的制造设备,制造成本较低,催化性能好。总的来说,本发明与现有技术相比较具有以下优点和效果:
通过贵金属Pd、Pt的协同作用,并加入助剂,大大提高了催化剂的活性。可以根据不同工况,调整非均匀蛋壳型颗粒、条状以及环状有机废气净化催化剂的制备条件,满足工艺要求。
在整体型有机废气净化催化剂的制备上,本发明采用一次性均匀涂覆,简化了催化剂制备工艺。
对于分子量较大的有机废气,具有良好的脱除效果,精度高。
催化剂具有非常好的稳定性,可以满足含水体系的有机废气催化脱除。
具体实施方式
下面结合实例和比较例对本发明做进一步的说明,但本发明的保护范围并不局限于实施例表述的范围。
实施例1
称取20g本公司生产的γ- Al2O3球形载体(Ф1~1.2mm,比表面积为220.3m2•g-1,平均孔径为14.5nm),400℃焙烧5h后备用。称取一定量的Mg(NO3)2溶液对载体进行等体积浸渍,然后再110℃烘箱中干燥4h,最后在350℃空气气氛中焙烧5h;分别称取一定量的Pd(NO3)2、Pt(NO3)2、Mn(NO3)2及La(NO3)3溶液混合,调节PH值至5,采用过量浸渍法对上面处理过的氧化铝球形载体进行负载,浸渍时间为30min,然后在100℃烘箱中干燥6h,最后在400℃空气气氛中焙烧5h,制得含量为0.05wt%Pd-0.4%Pt-2.1%Mn-0.53%La-0.12%Mg/ Al2O3的有机废气净化球形颗粒催化剂。
实施例2
称取20g本公司生产的γ- Al2O3条状载体(Ф2×(3~8)mm,比表面积为243.5m2•g-1,平均孔径为13.5nm),600℃焙烧6h后备用。称取一定量的Ca(NO3)2溶液对载体进行等体积浸渍,然后再100℃烘箱中干燥6h,最后在500℃空气气氛中焙烧3h;分别称取一定量的Pd(NO3)2、Pt(NO3)2及Ce(NO3)3溶液混合,调节PH值至4.5,采用过量浸渍法对以上处理过的氧化铝条状载体进行负载,浸渍时间为10min,然后在150℃烘箱中干燥2h,最后在300℃空气气氛中焙烧6h,制得含量为0.2wt%Pd-0.1%Pt-5.0%Ce-3.0%Ca/ Al2O3的有机废气净化条状催化剂。
实施例3
称取20g本公司生产的γ- Al2O3环状载体(外径Φ6×内径Φ5×高4(mm),比表面积为251.2m2•g-1,平均孔径为12.3nm),900℃焙烧3h后备用。称取一定量的NaNO3溶液对载体进行等体积浸渍,然后再150℃烘箱中干燥2h,最后在300℃空气气氛中焙烧6h;分别称取一定量的Pd(NO3)2、Pt(NO3)2及Ni(NO3)2溶液混合,调节PH值至6.0,采用过量浸渍法对以上处理过的氧化铝环状载体进行负载,浸渍时间为60min,然后在120℃烘箱中干燥4h,最后在300℃空气气氛中焙烧6h,制得含量为0.12wt%Pd-0.2%Pt-3.3%Ni-0.09%Na/ Al2O3的有机废气净化环状催化剂。
实施例4
分别称取一定量的Pd(NO3)2、Pt(NO3)2、Zr(NO3)4及KNO3溶液混合,加入一定量的拟薄水铝石粉,并加入适量硝酸调节PH至4.0,用球磨机球磨12h,得到涂层浆料;将上述浆料一次均匀涂覆到40×40×25mm的蜂窝陶瓷载体上,并用高压气体吹出蜂窝陶瓷载体孔隙内多余的浆液;100℃干燥6h,600℃焙烧3h,得到含量为0.13wt%Pd-0.27%Pt-3.01%Zr-1.19%K/Al2O3 /堇青石蜂窝陶瓷有机废气净化整体催化剂。
实施例5
分别称取一定量的Pd(NO3)2、Pt(NO3)2、Rh(NO3)3、Ca(NO3)2及Mg(NO3)2溶液混合,加入一定量的拟薄水铝石粉,并加入适量硝酸调节PH至3.0,用球磨机球磨24h,得到涂层浆料;将上述浆料一次均匀涂覆到40×40×25mm的蜂窝陶瓷载体上,并用高压气体吹出蜂窝陶瓷载体孔隙内多余的浆液;150℃干燥2h,450℃焙烧4h,得到含量为0.16wt%Pd-0.25%Pt-0.11%Rh-1.44%Ca-0.16%Mg/ Al2O3/堇青石蜂窝陶瓷有机废气净化整体催化剂。
实施例6
分别称取一定量的Pd(NO3)2、Pt(NO3)2、Ru(NO3)3及NaNO3溶液混合,加入一定量的拟薄水铝石粉,并加入适量硝酸调节PH至3.5,用球磨机球磨5h,得到涂层浆料;将上述浆料一次均匀涂覆到40×40×25mm的蜂窝陶瓷载体上,并用高压气体吹出蜂窝陶瓷载体孔隙内多余的浆液;110℃干燥3.5h,300℃焙烧6h,得到含量为0.18wt%Pd-0.12%Pt-0.02%Ru-0.05%Na/ Al2O3/堇青石蜂窝陶瓷有机废气净化整体催化剂。
实施例7
分别称取一定量的Pd(NO3)2、Pt(NO3)2、Nb(NO3)3、Ti(NO3)4及Mg(NO3)2溶液混合,加入一定量的拟薄水铝石粉,并加入适量硝酸调节PH至5.5,用球磨机球磨16h,得到涂层浆料;将上述浆料一次均匀涂覆到40×40×25mm的蜂窝陶瓷载体上,并用高压气体吹出蜂窝陶瓷载体孔隙内多余的浆液;130℃干燥3h,500℃焙烧2h,得到含量为0.09wt%Pd-0.22%Pt-0.09%Nb-2.67%Ti-1.56%Mg/ Al2O3/堇青石蜂窝陶瓷有机废气净化整体催化剂。
以上所制备的催化剂进行甲苯催化燃烧实验,通过对甲苯的去除率来测试催化剂的活性。在甲苯进口浓度 4000mg/ m3,空速 10000h-1 ,反应器入口温度为250℃的条件下进行催化燃烧性能评价。结果见表一:
表一 催化燃烧评价结果
实施例 | 甲苯转化率 |
1 | 99.2% |
2 | 99.3% |
3 | 99.8% |
4 | 99.8% |
5 | 99.6% |
6 | 99.1% |
7 | 99.5% |
由此可见,本发明的催化剂对有机废气有较好的净化效果。
Claims (7)
1.一种有机废气净化催化剂,其特征在于:该催化剂包含主要活性组分、助剂、载体;
所述的主要活性组分选自贵金属Pd、Pt,其含量以单质金属计,Pd的含量为催化剂总重量的0.05wt%~0.2wt%;Pt的含量为整个催化剂总重量的0.1wt%~0.4wt%;
所述的助剂包括助剂一和助剂二;助剂一选自Ni、Mn、Ce、Rh、Ru、Zr、La、Nb、Ti中的一种或几种,其含量以单质金属计,为催化剂总重量的0.02wt%~5wt%;
所述的助剂二选自碱金属和碱土金属中的一种或几种,其含量以单质金属计,为催化剂总重量的0.05wt%~3wt%;
所述催化剂为颗粒、条状以及环状催化剂,载体为Al2O3;或为负载主要活性组分、助剂的整体催化剂。
2.按照权利要求1 所述的有机废气净化催化剂,其特征在于:Pd的含量优选为催化剂总重量的0.09wt%~0.16wt%;Pt的含量优选为整个催化剂总重量的0.12wt%~0.27wt%。
3.按照权利要求1 所述的有机废气净化催化剂,其特征在于:所述助剂一选自Ni、Mn、Ce、Rh、Ru、Zr、La、Nb、Ti中的一种或几种,其含量优选为催化剂总重量的0.1wt%~3.3wt%。
4.按照权利要求1 所述的有机废气净化催化剂,其特征在于:所述助剂二选自碱金属和碱土金属中的一种或几种,其含量优选为催化剂总重量的0.09wt%~1.6wt%。
5.按照权利要求1 所述的有机废气净化催化剂,其特征在于:所述催化剂载体和整体催化剂的涂层选自Al2O3。
6.权利要求1 所述催化剂的制备方法,其特征在于:
所述颗粒、条状以及环状催化剂制备过程依次如下:
(1) 颗粒、条状以及环状催化剂载体的制备:将拟薄水铝石、硝酸铝和氯化铝的混合物分别进行滚球、挤条或压片成型,100~150℃干燥2~6h,400~900℃焙烧3~6h,得到Al2O3催化剂载体;
(2) 助剂二的负载:将助剂二的前驱体溶液采用等体积浸渍的方式浸渍到颗粒、条状以或环状催化剂Al2O3载体上,100~150℃干燥2~6h,300~500℃焙烧3~6h;
(3) 助剂一及主要活性组分的负载:调节助剂一和主要活性组分的前驱体混合溶液的PH值,浸渍到已经负载助剂二的催化剂上,浸渍时间为10~60min,100~150℃干燥2~6小时,300~500℃焙烧3~6h,得到非均匀型蛋壳型催化剂。
7.权利要求1 所述催化剂的制备方法,其特征在于:
所述整体催化剂制备过程依次如下:
涂层浆料制备:按照权利要求1 所述比例称取主要活性组分及助剂的前驱体、拟薄水铝石粉,加入适量硝酸调节PH值,用球磨机球磨5~24h,得到有机废气净化催化剂作为蜂窝陶瓷载体涂层的涂层浆料;
将上述浆料一次性均匀涂覆到蜂窝陶瓷载体上,并用高压气体吹出蜂窝陶瓷载体孔隙内多余的浆液;100~150℃干燥2~6h,300~600℃焙烧3~6h,得到有机废气净化催化剂。
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