CN114849723A - 一种纳米级含钼脱硫催化剂及其制备方法 - Google Patents
一种纳米级含钼脱硫催化剂及其制备方法 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 49
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 13
- 239000011733 molybdenum Substances 0.000 title claims abstract description 13
- 238000006477 desulfuration reaction Methods 0.000 title claims abstract description 10
- 230000023556 desulfurization Effects 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title abstract description 7
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims abstract description 36
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 26
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000005751 Copper oxide Substances 0.000 claims abstract description 15
- 229910000431 copper oxide Inorganic materials 0.000 claims abstract description 15
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims abstract description 13
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims abstract description 12
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 10
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 8
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 7
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052742 iron Inorganic materials 0.000 claims abstract description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 4
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- 238000003786 synthesis reaction Methods 0.000 claims abstract description 4
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 claims description 24
- 239000002002 slurry Substances 0.000 claims description 13
- 239000002243 precursor Substances 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000007790 solid phase Substances 0.000 claims description 5
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 4
- 238000001308 synthesis method Methods 0.000 claims description 3
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical group Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 2
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 2
- 230000005389 magnetism Effects 0.000 claims description 2
- 239000012702 metal oxide precursor Substances 0.000 claims description 2
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- 238000000354 decomposition reaction Methods 0.000 description 10
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
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- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
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- 239000010419 fine particle Substances 0.000 description 1
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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Abstract
本发明提供了一种纳米级含钼脱硫催化剂及其制备方法,催化剂由纳米级氧化钼,纳米级四氧化三铁或纳米级氧化铜组成,主催化剂为铁或铜氧化物,催化剂中铁或铜和钼的摩尔比为4:1‑8:1,催化剂可在200‑250℃催化分解硫化氢为氢气和硫蒸汽,催化剂的平均粒径为10‑30nm,比表面积为40‑100m2/g,可以通过超声波合成的方式获得纳米级金属氧化物。
Description
技术领域
本发明涉及一种纳米级含钼脱硫催化剂及其制备方法,属于沼气中硫化氢气体处理技术领域。
背景技术
随着社会经济和人民生活水平的不断提高,人们产生的有机垃圾数量逐年递增,沼气产生源从早期的分散式的农村化粪池扩展到大型垃圾填埋场,大型有机垃圾处理厂厌氧消化罐,集中式高浓度有机废水厌氧消化罐等人为的大型有机物处理设施,其产生量巨大,可以作为一种清洁可再生能源进行利用。
沼气的主要成分为甲烷和二氧化碳,但其中含有大量杂质,如硫化氢气体,如不有效去除,沼气中硫化氢的腐蚀性缩短沼气利用系统的设备及管道,并且硫化氢气体的燃烧产物:二氧化硫和硫酸会加剧系统设备的腐蚀,如释放到空气还将造成酸雨。因此,在利用沼气作为能源利用前,须将沼气中的硫化氢进行去除。
硫化氢的去除方法主要分为三类:湿法、干法和生物法。其中湿法吸收硫化氢后,须进行进一步处理;生物法占地较大,稳定性较差;干法操作简单,但吸附容量有限,吸附材料需要进行更换或再生,吸附材料中或解析的硫化氢仍需进行治理。
工业领域中,在400-800℃高温下,利用硫化钼等作为催化剂实现硫化氢的分解,产生氢气和单质硫,在去除硫化氢的同时产生可燃气体,提高沼气的热值,并收集纯度较高单质硫。但其反应温度过高,导致处理硫化氢气体成本高。因此,需要一种低温分解硫化氢气体的催化剂,降低硫化氢气体分解成本。
发明内容
本发明针对现有的硫化氢分解过程,反应温度高导致的硫化氢分解成本高的问题,提供一种较低温度分解硫化氢气体的催化剂及其制备方法,降低沼气中硫化氢的分解成本。
为实现以上技术目的,本发明的催化剂及其制备方法如下:
含钼催化剂由纳米级氧化钼,纳米级四氧化三铁或纳米级氧化铜组成,主催化剂为铁或铜氧化物,催化剂中铁或铜和钼的摩尔比为4:1-8:1,催化剂可在200-250℃催化分解硫化氢为氢气和硫蒸汽,钼氧化物的加入提高脱硫精度,即分解效率升高,较单一铁或铜氧化物的催化剂提高沼气中硫化氢高效分解持续时间。
纳米级催化剂的平均粒径为10-30nm,比表面积为40-100m2/g,催化剂中的纳米级金属氧化物可以通过超声合成的方法配制,催化剂使用铁或铜氧化物前驱物质和钼氧化物前驱物质添加到正癸烷中,通过超声波反应分别合成纳米级四氧化三铁(含磁性)或纳米级氧化铜和纳米级三氧化钼,而后按比例进行充分混合。细小的颗粒和大的比表面积保证了更高的催化剂活性点位。纳米级金属氧化物也可以采用商用材料。
超声反应合成中使用的四氧化三铁前驱物质为五羰基铁,氧化铜前驱物质为氯化铜或醋酸铜,氧化钼前驱物质为六羰基钼。具体的超声波合成方法如下:
1)将金属氧化物前驱物质投加到正癸烷中,形成0.3-0.4mol/L的浆液;
2)浆液通过氮气进行充分脱气;
3)脱气的浆液通过超声波破碎仪设置工作频率20kHz,脉冲占空比70-80%的情况下,破碎3-6h,浆液迅速形成金属氧化物浆液;
4)超声波破碎完的通过离心分离获得固相,经正癸烷清洗3遍以上后,在185℃(比正癸烷的沸点174.2℃高10℃)下干燥8h以上,充分去除残留正癸烷;
5)获得纳米级金属氧化物。
从以上描述可以看出,本发明具备以下优点:
1、本发明中纳米级的催化剂增加了催化效率,提供了稳定高效的分解过程;
2、本发明中添加的氧化钼可以提高脱硫精度。
具体实施方式
实施例中使用的超声波破碎仪器的功率为600W,脉冲操作时间可调。
下面结合实例对本发明的具体实施方式作进一步说明。在此需要说明的是,对于这些实施方式的说明用于帮助理解本发明,但并不构成对本发明的限定。此外,下面所描述的本发明各个实施方式中所涉及的技术特征只要彼此之间未构成冲突就可以相互组合。
实施例1
配制0.3mol/L的五羰基铁正癸烷浆液,以氮气充分脱气后,通过超声波破碎仪,在工作频率20kHz,脉冲占空比75%的设定下,破碎3h,经离心去掉上清液,以正癸烷清洗3次后,在185℃下干燥10h,获得黑色四氧化三铁粉末。其平均粒径为11nm,比表面积为54m2/g。
配制0.4mol/L的六羰基钼正癸烷浆液,以氮气充分脱气后,通过超声波破碎仪,在工作频率20kHz,脉冲占空比80%的设定下,破碎4h,经离心去掉上清液,以正癸烷清洗3次后,在185℃下干燥10h,获得银灰色氧化钼粉末。其平均粒径为16nm,比表面积为58m2/g。
将两种纳米级粉末按铁和钼比例6:1充分混匀获得催化剂。
实施例2
采用商用纳米氧化铜。其平均粒径为22nm,比表面积为43m2/g。
配制0.4mol/L的六羰基钼正癸烷浆液,以氮气充分脱气后,通过超声波破碎仪,在工作频率20kHz,脉冲占空比80%的设定下,破碎4h,经离心去掉上清液,以正癸烷清洗3次后,在185℃下干燥12h,获得银灰色氧化钼粉末。其平均粒径为16nm,比表面积为58m2/g。
将两种纳米级粉末按铜和钼比例5:1充分混匀获得催化剂。
对照例1
实施例1中不添加纳米级氧化钼的纳米级四氧化三铁粉末。
对照例2
实施例1中的纳米级四氧化三铁超声波合成时间减少至1h,生成粉末的平均粒径为28nm,比表面积为14m2/g的黑色四氧化三铁粉末。其他内容一致。
使用实施例和对照例的催化剂,以模拟的沼气进行了催化性能试验。模拟沼气成分为甲烷59%,二氧化碳40%,硫化氢1%,即10000ppm。在温度215℃,空速1800h-1下,使用石英管反应器,以2g催化剂量测试了不同催化剂的硫化氢分解性能。
实施例1中的催化剂在测试过程中前30h内在出口未检测出硫化氢气体,并在后续24h内继续保持硫化氢浓度在100ppm以下。而对比例1中的催化剂组试验过了32h后,在出口检测出硫化氢气体,但在不到9h出口硫化氢浓度突破了100ppm,说明纳米级氧化钼促进了硫化氢的分解,促进出口硫化氢浓度长期处于低位。而对比例2的催化剂组试验的催化剂反应仅20h,出口就检测出硫化氢气体,后续硫化氢浓度在100ppm以下的时间也缩减到6h,说明主催化剂的性能是硫化氢分解反应的主要因素。
实施例2中的催化剂在测试过程中前18h内在出口未检测出硫化氢气体,并在后续28h内继续保持硫化氢浓度在100ppm以下。
测试过程出口检测出硫化氢气体前,测算得出的脱硫量分别为实施例1,3.17g/g催化剂;实施例2,1.89g/g催化剂;对比例1,3.38g/g催化剂;对比例2,1.35g/g催化剂。测试中催化剂脱硫量高于常规脱硫吸附剂的量,因此,本发明催化剂具有催化分解硫化氢气体的能力。
所有试验过程中,均在反应器出口端生成黄色硫磺沉淀。
可以理解的是,以上关于本发明的具体描述,仅用于说明本发明而并非受限于本发明实施例所描述的技术方案。本领域的普通技术人员应当理解,仍然可以对本发明进行修改或等同替换,以达到相同的技术效果;只要满足使用需要,都在本发明的保护范围之内。
Claims (5)
1.一种纳米级含钼脱硫催化剂,其特征在于,催化剂由纳米级氧化钼,纳米级四氧化三铁或纳米级氧化铜组成,主催化剂为铁或铜氧化物,催化剂中铁或铜和钼的摩尔比为4:1-8:1,催化剂可在200-250℃催化分解硫化氢为氢气和硫蒸汽。
2.权利要求1所述的纳米级催化剂,其特征在于,所述催化剂的平均粒径为10-30nm,比表面积为40-100m2/g。
3.权利要求1所述的纳米级催化剂,其特征在于,所述催化剂中的纳米级氧化物可以通过超声波合成的方法配制,催化剂使用铁或铜氧化物前驱物质和钼氧化物前驱物质添加到正癸烷中,通过超声反应分别合成纳米级四氧化三铁(含磁性)或纳米级氧化铜和纳米级三氧化钼。
4.权利要求3所述的铁/铜氧化物前驱物质,其特征在于,所述四氧化三铁前驱物质为五羰基铁,氧化铜前驱物质为氯化铜或醋酸铜,氧化钼前驱物质为六羰基钼。
5.权利要求3所述的超声波合成纳米金属氧化物的方法,包括以下步骤:
1)将金属氧化物前驱物质投加到正癸烷中,形成0.3-0.4mol/L的浆液。
2)浆液通过氮气进行充分脱气。
3)脱气的浆液通过超声波破碎仪以工作频率为20kHz,脉冲占空比70-80%的条件下,进行3-6h超声波破碎,浆液迅速形成金属氧化物浆液。
4)超声波破碎完的通过离心分离获得固相,经正癸烷清洗3遍以上后,在185℃下干燥8h以上,充分去除残留正癸烷。
5)获得纳米级金属氧化物。
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