CN1039203C - 高强度高活性氨合成催化剂的制造方法及熔制设备 - Google Patents

高强度高活性氨合成催化剂的制造方法及熔制设备 Download PDF

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CN1039203C
CN1039203C CN93100955A CN93100955A CN1039203C CN 1039203 C CN1039203 C CN 1039203C CN 93100955 A CN93100955 A CN 93100955A CN 93100955 A CN93100955 A CN 93100955A CN 1039203 C CN1039203 C CN 1039203C
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仰华胄
王逸恩
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    • C01C1/00Ammonia; Compounds thereof
    • C01C1/02Preparation, purification or separation of ammonia
    • C01C1/04Preparation of ammonia by synthesis in the gas phase
    • C01C1/0405Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst
    • C01C1/0411Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst characterised by the catalyst
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

本发明涉及一种氨合成催化剂的制造方法及设备,属催化剂生产领域。该工艺采用专用设备三电极电阻炉取代多年来一直沿用的单相电阻熔炉熔制催化剂,提高了催化剂熔炼温度并降低了能耗;采用多喷头流体喷射成球法以及简便的固液分离技术,提高了催化剂的活性和强度,保证了催化剂的外观色泽。本发明使合成氨球形催化剂制造吨耗电率下降20%-30%,成品率为80%,催化剂单粒抗碎强度4.0mm以上>35kg,催化剂活性提高0.5%以上。

Description

高强度高活性氨合成催化剂的制造方法及熔制设备
本发明涉及一种氨合成催化剂的制造方法及熔制设备,属催化剂生产领域。
中国发明专利85101606公开了一种液体分散法高强度氨合成球形催化剂制造方法,此方法采用磁铁矿、氧化铝、碳酸钙等为原料,经电炉熔炼,流体分散水冷成球,制造高强度氨合成催化剂。此方法的主要缺点是,采用两个电极单相电阻炉熔制原料熔炼温度低,成球率也不高,且成球后冷却液与催化剂分离慢,降低了球形催化剂的强度。传统的制造熔铁催化剂,一般采用双电极单相电阻炉,电弧炉、感应电炉等。双电极单相电阻炉,造价低廉,使用方便,但最大的缺点是熔炼温度偏低(~1500℃),变压器功率利用率低,影响催化剂质量;电弧炉温度较高(~2000℃),但由于碳素电极还原性强,很容易导致催化齐产品铁比(Fe2+/Fe3+)过高,也影响催化剂质量;感应电炉温度适当,并可缩短熔炼时间,但造价昂贵,且炉衬容易受碱性物质侵蚀,更换频繁不适于大规模工业化生产。
本发明的目的是提供一种高强度、高活性氨合成催化剂的制造方法及熔制设备,采用本制造方法可准确掌握熔炼温度,并能提高成球率及催化剂强度,同时又可降低成本。
本发明是这样实现的:将制造氨合成催化剂原料精选磁佚矿和氧化铝、硝酸钾、碳酸钙等,按一定比例混合均匀后,装入本发明专用熔制设备三电极电阻炉中熔炼,熔炼时用纯铁调整熔浆中的二价铁和三价铁的比例,熔炼电压保持在15v-50v的范围内变化,熔炼4-8小时,当铁比(即Fe2+/Fe3+)达到适当值时,慢慢倒出熔装,催化剂熔浆落在由多喷头喷枪喷射的液体上,喷枪喷头可以是两个,也可以是三个,这样催化剂熔浆可得到比较均匀的冲击而破裂分散并自行收缩成球,然后落入园锥形冷却池内,催化剂在冷却池内凝结成粒度不同的球状或近似球状的颗粒,冷却池上口直径>1600mm,高>800mm,锥形池下口直径为80-120mm,锥形池内冷却液液面高度由一个循环泵来稳定,液面距出料口的垂直距离为500-1000mm,冷却液温度大于70℃。从园锥形冷却池下口流出的含有催化剂颗粒的液体注入倾斜的弧形筛网上,弧形筛网网孔直径1-2mm,筛网长度1400-2000mm,弧形筛网倾斜度大于30度,催化齐颗粒和冷却液在筛网上分离,冷却液可循环使用,分离使用,分离后的催化剂颗粒用干燥的氮气或空气进行热处理,再进行筛选除去未成形的不规则颗粒,分粒度装箱,即可得到催化剂成品。
附图说明:
图1.是本发明工艺流程示意图;
图2.是三电极电阻炉俯视图。
以下结合附图对本发明进行详细说明:
图1中1是三电极电阻炉;2是三喷头喷枪;3是冷却池;4是弧形筛网;5是集液池。将原料精选磁铁矿氧化铝、硝酸钾、碳酸钙等按一定比例混合均匀后,装入三电极电阻炉1中进行熔炼,熔炼电压控制在15v-50v的范围内,熔炼4-8小时,当铁比达到适当值时,慢慢将熔浆倒在三喷头喷枪2的喷液口上,使催化剂熔浆充分分散并自行收缩成球,然后自行落入园锥形冷却池3内,催化剂在冷却池3内的冷却液中凝结成大小不同的形状颗粒,冷却池内冷却液液面距出料口的垂直距离为500-1000mm,冷却液温度大于70℃,从次冷却池3下口流出的含有催化剂颗粒的液体注入倾斜的弧形筛网4上进行固液分诹,液体流入集液池5中,可循环使用,分离后的催化剂颗粒用干燥的氮气进行处理,再进行筛选,即可得催化剂成品。
结合图2,三电极电阻炉由高温耐火材料6将熔炉炉腔隔成丫形,三个电极7分置于丫形炉腔的三个项点,三电极到丫形炉腔中心的距离相等,通过调整电炉变压器的输出电压可控制熔炼温度,三电极电阻炉熔炼温度比单相电阻炉提高100℃以上。
本发明的突出优点是:采用三电极电阻炉提高了熔炼温度,并减少了电耗,生产吨催化剂耗电率下降20%-30%,采用多喷头喷枪喷射液体冲击高温熔浆,提高分散度,使熔浆分散均匀,提高了成球率,使成品率>80%,冷却时催化剂颗粒与冷却液接触时间很短就被迅速分离,这样就提高了催化剂的强度,催化剂单粒抗碎强度4.0mm以上>35Kg,同时催化剂活性提高0.5%以上。
下面介绍一个本发明的应用实例,采用180EVA电炉变压器,使用三电极电阻炉熔炼混合原料300公斤,加纯铁19公斤,熔炉电压为20-45V,熔炼六小时,当铁比达到0.55时出炉,经喷射成球,冷却、分离得到催化剂280公斤,3.0-4.0mm球单粒抗碎强度≥30公斤,大于4mm球其抗碎强度≥35公斤。此种催化剂活性比原工艺生产的催化剂活性提高0.5%以上。

Claims (5)

1.一种制备氨合成催化剂的方法,是将原料精选磁铁矿、氧化铝、硝酸钾和碳酸钙  经配制混合均匀后,装入三电极电阻炉(1)熔炼,熔炼电压保持15-50v,熔炼时间为4-8小时,出炉催化剂熔浆落在由多喷头喷枪(2)喷射的液体上,冲击破裂进行收缩成球后,落入圆锥形冷却池(3)内,凝结成球状或近似球形的颗粒,从冷却池(3)下口注在倾斜的弧形筛网(4)上,进行固液分离后干燥筛选制成。
2.根据权利要求1所述的一种制备氨合成催化剂的方法,其特征在于多喷头喷枪(2)的喷头为三个。
3.根据权利要求1所述的一种制备氨合成催化剂的方法,其特征在于锥形冷却池(3)中冷却液面距电阻炉出料口的垂直距离为500-1000mm,冷却液温度大于70℃。
4.根据权利要求1所述的一种制备氨合成催化剂的方法,其特征在于弧形筛网(4)倾斜度大于30度。
5.一种用于制备氨合成催化剂的三电极电阻炉,其特征在于电阻炉(1)由高温耐火材料(6)将熔炉炉腔分隔成Y形,三个电极(7)分别置于Y形炉腔的三个顶点。
CN93100955A 1993-01-09 1993-01-09 高强度高活性氨合成催化剂的制造方法及熔制设备 Expired - Fee Related CN1039203C (zh)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8414788B2 (en) 2005-04-01 2013-04-09 Fike Corporation Reverse acting rupture disc with laser-defined electropolished line of weakness and method of forming the line of weakness

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0174080A1 (en) * 1984-08-03 1986-03-12 Imperial Chemical Industries Plc Catalystsfor the synthesis of ammonia
EP0174716A1 (en) * 1984-06-19 1986-03-19 Agrimont S.p.A. Process for preparing iron-based catalysts for the synthesis of ammonia and catalysts so obtained

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0174716A1 (en) * 1984-06-19 1986-03-19 Agrimont S.p.A. Process for preparing iron-based catalysts for the synthesis of ammonia and catalysts so obtained
US4789657A (en) * 1984-06-19 1988-12-06 Fertimont S.P.A. Process for preparing iron-based catalysts for the synthesis of ammonia and catalysts so obtained
EP0174080A1 (en) * 1984-08-03 1986-03-12 Imperial Chemical Industries Plc Catalystsfor the synthesis of ammonia

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8414788B2 (en) 2005-04-01 2013-04-09 Fike Corporation Reverse acting rupture disc with laser-defined electropolished line of weakness and method of forming the line of weakness

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