Research progress on the transformation and utilization of nitrogen element based on chemical looping
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摘要: “双碳”背景下，氮或将成为取代碳的重要元素，可完成无碳燃料氨以及其他化合物的生产。其中，氨不仅是重要的化工原料，更是良好的能源载体。化学链技术通过重新设计反应路径，将过程分解为不同空间或时间内进行的两个或多个子反应，通过载体介质的反应和再生在耦合系统中实现物质和能量传递。作为一种新兴的清洁、有效能源转化手段，化学链技术近年来得到了广泛的关注。基于此，本文对化学链技术在含氮化合物合成与转化领域中的研究进行综述，概述了以Haber-Bosch工艺为基础的多相催化和光、电等外场力驱动的化学链合成氨工艺的新发展，并对其进行总结和讨论。在含氮化合物合成方面，介绍了化学链技术用于氨氧化制一氧化氮以及烷基硝酸酯为关键中间体的烷烃化学链制醇类物质的过程。最后对基于化学链的氮转化与利用面临的挑战进行了分析和讨论，以期为今后化学链制含氮化学品提供参考。Abstract: Under the background of “Carbon Peak and Carbon Neutrality”, nitrogen may become an important element to replace carbon, completing the production of carbon-free fuel ammonia and other compounds. Among them, ammonia, not only an important chemical raw material, but also a good energy carrier, has been widely studied by scholars. However, the existing Haber-Bosch ammonia process is a fossil energy-dependent, energy-intensive and carbon-emitting process. Hence, the development of a new “green” ammonia process driven by renewable energy is an important project for the sustainable development of human society. Chemical looping technology breaks down the process into two or more sub-reactions carried out in different space or time by redesigning the reaction path, and realizes material and energy transfer in a coupled system through the reaction and regeneration of the carrier medium, characterized by easy coupling to renewable energy sources, atmospheric pressure operation, and avoidance of reactants competing for adsorption. In addition to the advantages of intensifying the reaction process, chemical looping technology has a lower carbon emission compared with the traditional technology, which is an effective way in response to “carbon control” strategy and has gained widespread attention in recent years. However, research on chemical looping synthesis and conversion is mostly dominated by carbon-based materials, and for nitrogen-based materials, the only more in-depth chemical looping ammonia synthesis technology still faces the problems of low nitrogen fixation efficiency and low ammonia production rate of nitrogen carriers. Based on this, this paper reviews the research of chemical looping technology in the field of synthesis and conversion of nitrogen-containing compounds, outlines the new development of multiphase catalysis based on the Haber-Bosch process and the chemical looping ammonia synthesis process driven by external field forces, such as light and electricity, and divide the chemical looping ammonia synthesis process into the chemical looping ammonia synthesis process with hydrogen as the hydrogen source and the chemical looping ammonia synthesis process with water as the hydrogen source, according to the hydrogen source are summarized and discussed in this paper. In the synthesis of nitrogen-containing compounds, the chemical looping technology for the oxidation of ammonia to nitric oxide as well as the chemical looping process for the production of alcohols from alkanes with alkyl nitrates as the key intermediates are detailed presented. Among them, the chemical looping ammonia oxidation process has good NO selectivity and avoids N2O production, which is an efficient and clean advanced technology. Under mild reaction conditions, the light-driven chemical looping synthesizes alcohols to form the key intermediate R-ONO2. Such a light-assisted pathway can achieve high activity and selectivity at low temperatures, providing a new idea for the preparation of value-added chemicals at low temperatures. Finally, the challenges of nitrogen conversion and utilization are analyzed and discussed, with the expectation to provide a reference for the promotion of non-carbon fuel production and the low-carbon transition of chemicals. The development of superior nitrogen carriers, efficient reactors, novel chemical looping processes, and full life cycle and economic evaluation of scale-up production will help to explore the possibilities of industrialization and commercialization of chemical looping technology in the future.
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Key words:
- chemical looping /
- nitrogen-containing compounds /
- ammonia synthesis /
- ammonia oxidation
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图 6 各种元素氮化物在化学链合成氨过程中的研究程度
Figure 6 The degree to which nitrides of various elements are studied in the process of ammonia synthesis in the chemical looping
表 1 载氮体的常见制备方法
Table 1 Common preparation methods for nitrogen carriers
Method Advantages Disadvantages Ref. co-precipitation
methodthe operation is simple, the cost is low, the prepared nitrogen carrier material has high hardness, uniform components, and dense powder the addition of precipitant may lead to high local concentrations and agglomeration [29] one-step
pyrolysis methodeasy to operate, low preparation temperature and short time-consuming the surface of the hydrogenated nitrogen carrier is rough and cracks appear [30−33] mechanical
mixing methodsimple to operate and easy to control poor uniformity and easy agglomeration [34,35] immersion
methodthe operation is simple, easy to control, and the active component has a high atomic utilization the preparation time is long, the uniformity is poor, and it is not suitable for industrial production [34,36,37] sol-gel method the prepared sample has a high specific surface area, controllable microstructure and good uniformity the cost of raw materials is high and the preparation time is long [38] molten salt
synthesis methodthe operation is simple, the preparation temperature is low, the uniformity is good, and the product purity is high the scope of application is small, the molten salt is toxic, and special equipment is required (PTFE lined steel reactor with nitrogen-filled glove box, etc.) [39] 
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表 2 典型载氮体介导的化学链合成氨过程总结
Table 2 Summary of ammonia synthesis processes with typical nitrogen-loaded mediated chemical looping
Nitrogen Carrier Nitrogen Carrier Type Hydrogen Source Drive Type Reaction Conditions Reaction Rate
(Efficiency)Ref. Ca3N2 Ionic
NitrideH2 Thermally
DrivenN Fixation：700 ℃
Hydrogenation：550 ℃，1×105 Pa98 μmol/(g∙h) [52] CrN Transition Metal Nitride H2 Thermally
DrivenN Fixation：750 ℃
Hydrogenation：700 ℃，1×105 Pa83.55 μmol/(g∙h) [36] Co-CrN Transition Metal Nitride H2 Thermally
DrivenAs Above 818.2 μmol/(g∙h) [36] Mo2N Transition Metal Nitride H2 Thermally
DrivenN Fixation：600 ℃
Hydrogenation：450 ℃，1×105 Pa4576 μmol/(g∙h) [32] BaNH Ionic
NitrideH2 Thermally
DrivenN Fixation & Hydrogenation：
300 ℃，1×105 Pa198 μmol/(g∙h) [66] Ni-BaNH Ionic
NitrideH2 Thermally
DrivenAs Above 3125 μmol/(g∙h) [66] Li2NH Ionic
NitrideH2 Thermoelectric
CouplingMolten Salt Electrolytic Cell：
2V，400 ℃，1×105 Pa64 μmol/(g∙h) [71] Li3N Ionic
NitrideH2O Thermoelectric
CouplingElectrolysis：
3V，450 ℃，1×105 Pa
N Fixation & Hydrolysis：
100 ℃，1×105 Pa88.5%
（initial current efficiency）[48] Mg3N2 Ionic
NitrideH2O Photothermal
CouplingN Fixation：1×105 Pa
Reduction & Hydrolysis：
＜100 mTorr
Light Source Heating1.67 μmol/(g∙h) [73] Mn5N2 Transition Metal Nitride H2O Thermally
DrivenHydrolysis：
500 ℃，1×105 Pa
N Fixation：
1150 ℃，1×105 Pa54%，2 h
(the percentage of lattice nitrogen converted to ammonia)[77] CrN Transition Metal Nitride H2O Thermally
DrivenReduction：
1200~1500 ℃，1×105 Pa
N Fixation & Hydrolysis：
1000 ℃，1×105 Pa108 μmol/(g∙h) [78] AlN Covalent Metal Nitride H2O Thermally
DrivenN Fixation：
1500~1700 ℃，1×105 Pa
Hydrolysis：
1000 ℃，1×105 Pa88%，1 h
(the percentage of lattice nitrogen converted to ammonia)[81]
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