CN106362719B - 一种改性活性炭和制备方法及其应用 - Google Patents
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- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 70
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 36
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 35
- 239000003054 catalyst Substances 0.000 claims abstract description 35
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims abstract description 20
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- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 4
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明提供了一种改性活性炭和制备方法及其应用,属于催化剂载体的制备领域。其制备方法如下:一种石墨化活性炭经HNO3处理后,在氨气气氛下进行高温热处理,得到介孔率高的活性炭载体。该载体具有较大的孔隙容积,较高的介孔率(≥97%),导电性好等特点。用于氨合成催化剂载体时,能显著提高贵金属钌的分散度,提高催化剂的抗甲烷化能力、热稳定性和活性。在催化领域中具有广阔的应用前景。
Description
技术领域
本发明属于催化剂载体的制备领域,具体涉及一种改性活性炭和制备方法及其应用。
背景技术
对于各种农产品来说,肥料对其生长和提高产量都是极其重要的,要合成各种适合农作物使用的肥料,合成氨工业的发展发挥了巨大的作用。其中,合成氨铁催化剂的发明,开创了催化合成氨工业,并且铁催化剂价格低廉、稳定性较好,现已成为世界上研究得最透彻、最成功的催化剂之一。但是使用铁催化剂时,氨合成反应必须在高温高压的条件下才能进行,能耗较大,对设备要求较为苛刻。
钌催化剂的出现,使得氨合成反应在低温低压下进行成为了可能,大大降低了能耗,节约了能源,并且具有较高的氨合成活性,成为了继熔铁催化剂以来的第二代氨合成催化剂。目前,活性炭负载的钌催化剂已实现了工业化生产,但是活性炭自身的机械强度不够高,在高温、含氢的气氛中很不稳定,易发生甲烷化反应,这是制约钌催化剂大规模使用的因素之一。因此制备出具有高活性、高稳定性的钌基氨合成催化剂是人们研究的热点。中国专利CN1270081A描述的催化剂制备路线为含钌化合物溶液浸渍炭载体,用氢气把含钌化合物前躯体还原为金属钌,再浸渍助催化剂。但是用氢气还原的方法制备的催化剂中通常会残留氯离子,对催化剂的性能和使用寿命存在一定的影响。中国专利CN101053834A将活性炭在氢气中200-3000℃下处理,再用HNO3水浴回流处理,最后分别将碱金属助剂和活性组分钌负载到活性炭中,制备得到的催化剂改善了活性组分的分散,提高了催化剂的活性。这些方法制备出的钌基氨合成催化剂,其活性、稳定性有待进一步提高。
发明内容
本发明的目的在于针对现有技术的不足,提供一种改性活性炭和制备方法及其应用。该改性活性炭比表面、孔结构适宜,介孔率≥97%,介孔孔容为0.73-1.03;以其为载体的钌基氨合成催化剂具有抗甲烷化、活性高、稳定性好等优点。
为实现上述发明目的,本发明采用如下技术方案:
一种改性活性炭的制备方法:商用活性炭经石墨化、扩孔预处理后,采用2wt%-10wt%的硝酸溶液60~75℃浸泡1~3h,洗涤至中性,干燥;再于900-1100 ℃下、氨气气氛中热处理1-4h后,在氨气气氛中降至室温后,取出,即得活性炭载体。
所述的浸泡为采用水浴回流的方式浸泡,硝酸溶液与预处理后的活性炭的质量比为5-10:1。
热处理时氨气的气体流速为50-500 ml/min。
一种如上所述的制备方法制得的活性炭,其介孔率≥97%,介孔孔容为0.73-1.03。
一种利用如上所述的活性炭为载体的钌基氨合成催化剂,是以金属钌为活性组分,以碱金属和碱土金属金属作为助剂;钌含量为载体质量的2-10%,碱金属和碱土金属的含量为载体质量的的2-10%。
所述的活性组分的前驱体为RuNO(NO3)3,所述的碱土金属助剂的前驱体为Ba(NO3)2,碱金属助剂前驱体为KNO3。
一种利用如上所述的活性炭为载体制备钌基氨合成催化剂的方法,具体步骤为:
(1)活性炭的预处理:将商用活性炭在氩气惰性气氛中进行高温石墨化处理,1800-2000 ℃处理2-10小时,再在400-460℃下进行空气氧化扩孔处理20-30小时,将预处理好的活性炭洗涤,干燥;
(2)石墨化活性炭的改性处理:步骤(1)的石墨化炭采用2wt%-10wt%的硝酸溶液在60-75℃浸泡1-3h,洗涤至中性,干燥;再于900-1100 ℃下、氨气气氛中热处理1-4h后,在氨气气氛中降至室温后,取出,即得活性炭载体;
(3)催化剂的制备:首先将RuNO(NO3)3、Ba(NO3)2、KNO3混合配成溶液,然后采用等体积共浸渍的方法负载到改性后的活性炭载体上,最后将浸渍后的产物在红外灯下烘干20-40 min,制得催化剂。
本发明的有益效果在于:
本发明首先采用硝酸对石墨化活性炭进行氧化处理,提高了石墨化活性炭微孔中表面含氧官能团的数量,然后在氨气气氛下进行热处理,使氨气与石墨化活性炭微孔表面的含氧官能团反应,以去除含氧集团,从而使微孔孔径扩大,从微孔变为介孔;具有烧失率低,介孔率高,孔径分布集中,稳定性好等特点;用于氨合成催化剂载体时,能显著提高贵金属钌的分散度,提高催化剂的抗甲烷化能力、热稳定性和活性。在催化领域中具有广阔的应用前景。
具体实施方式
以下结合具体实施例对本发明进行进一步描述,但本发明的包括范围不仅限于此:
实施例1
一种改性活性炭的制备方法,具体步骤为:
(1)活性炭的预处理:取5 g商用活性炭在氩气惰性气氛中1900 ℃高温石墨化10小时,再在450 ℃氧气气氛下进行扩孔处理30小时,得到预处理后的活性炭,洗涤、干燥后备用;
(2)石墨化活性炭的改性处理:将步骤(1)预处理后的活性炭经破碎筛分出12-16目的活性炭颗粒,浸泡于70 ℃、浓度为5 wt%的硝酸溶液中,恒温2 h,取出后用蒸馏水洗涤至中性,于烘箱中110 ℃干燥12 h;之后将干燥后的样品放置于氨气气氛下1100 ℃热处理2 h,气体流速75ml/min,在该气氛下降至室温取出,即得改性后的活性炭载体,介孔率≥97%,介孔孔容为0.73-1.03。
实施例2
一种改性活性炭的制备方法,具体步骤为:
(1)活性炭的预处理:取5 g商用活性炭在氩气惰性气氛中2000℃高温石墨化2小时,再在450 ℃氧气气氛下进行扩孔处理30小时,得到预处理后的活性炭,洗涤、干燥后备用;
(2)石墨化活性炭的改性处理:将步骤(1)预处理后的活性炭经破碎筛分出12-16目的活性炭颗粒,浸泡于60 ℃、浓度为10 wt%的硝酸溶液中,恒温3 h,取出后用蒸馏水洗涤至中性,于烘箱中90 ℃干燥16 h;之后将干燥后的样品放置于氨气气氛下1100 ℃热处理2 h,气体流速100ml/min,在该气氛下降至室温取出,即得改性后的活性炭载体,介孔率≥97%,介孔孔容为0.73-1.03。
实施例3
一种改性活性炭的制备方法,具体步骤为:
(1)取5 g商用活性炭在氩气惰性气氛中1800 ℃高温石墨化5小时,再在460 ℃氧气气氛下进行扩孔处理20小时,得到预处理后的活性炭,洗涤、干燥后备用;
(2)石墨化活性炭的改性处理:将步骤(1)预处理后的活性炭经破碎筛分出12-16目的活性炭颗粒,浸泡于75 ℃、浓度为7 wt%的硝酸溶液中,恒温1 h,取出后用蒸馏水洗涤至中性,于烘箱中100 ℃干燥14 h;之后将干燥后的样品放置于氨气气氛下900 ℃热处理2h,气体流速50ml/min,在该气氛下降至室温取出,即得改性后的活性炭载体,介孔率≥97%,介孔孔容为0.73-1.03。
对比例1是指已扩孔的石墨化活性炭样品,未经硝酸和氨气处理;对比例1的样品,实施例1-实施例3所制得的改性活性炭的性能参数如下表1所示:
表1
应用实施例1
分别以实施例1的改性活性炭(样品1)、实施例2的改性活性炭(样品2)、实施例3的改性活性炭(样品3)、仅经高温石墨化和扩孔处理后的商用活性炭(样品4)为载体,采用等体积浸渍的方法将6%的活性组分钌、10%的金属助剂钡负载到改性后的活性炭载体上,最后将浸渍后的产物在红外灯下烘干30 min,制得催化剂。
催化剂活性评价在高压活性测试装置中进行,催化剂装填在内径12 mm的固定床反应器的等温区,堆积体积2 ml,反应器为氨高温催化裂解得到的氢、氮混合气,H2:N2=3:1,在400 ℃,10 MP,10000 h-1的条件下,各催化剂的氨合成活性测试结果如下表2所示:
表2
从表中可以看出,经本发明改性的活性炭负载的钌基氨合成催化剂的催化活性好于未经改性处理的普通活性炭,且稳定性也有很大的提高,也说明了其抗甲烷化能力的提高。
以上所述仅为本发明的较佳实施例,凡以本发明申请专利所做的均等变化与修饰,皆应属于本发明的涵盖范围。
Claims (7)
1.一种改性活性炭的制备方法,其特征在于:商用活性炭经石墨化、扩孔预处理后,采用2wt%-10wt%的硝酸溶液在60~75℃浸泡1~3h,洗涤至中性,干燥;再于900-1100 ℃下、氨气气氛中热处理1-4h后,在氨气气氛中降至室温后,取出,即得活性炭载体。
2.根据权利要求1所述的改性活性炭的制备方法,其特征在于:所述的浸泡为采用水浴回流的方式浸泡,硝酸溶液与预处理后的活性炭的质量比为5-10:1。
3.根据权利要求1所述的改性活性炭的制备方法,其特征在于:热处理时氨气的气体流速为50-500 ml/min。
4.一种如权利要求1-3任一项所述的制备方法制得的活性炭,其特征在于:所述的活性炭的介孔率≥97%,介孔孔容为0.73-1.03cm3/g。
5.一种利用权利要求4所述的活性炭为载体的钌基氨合成催化剂,其特征在于:
以金属钌为活性组分,以碱金属和碱土金属作为助剂;钌含量为载体质量的2-10%,碱金属和碱土金属的含量为载体质量的的2-10%。
6.根据权利要求5所述的钌基氨合成催化剂,其特征在于:所述的活性组分的前驱体为RuNO(NO3)3,所述的碱土金属助剂的前驱体为Ba(NO3)2,碱金属助剂前驱体为KNO3。
7.一种制备如权利要求5所述的钌基氨合成催化剂的方法,其特征在于:首先将RuNO(NO3)3、Ba(NO3)2、KNO3混合配成溶液,然后采用等体积共浸渍的方法负载到活性炭载体上,最后将浸渍后的产物在红外灯下烘干20-40 min,制得钌基氨合成催化剂。
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