剧毒气体PH3的干法净化技术研究进展

doi:10.11949/0438-1157.20230604

摘要/Abstract

摘要：

磷化氢（PH₃）是一种来源广泛的剧毒气体，未经处理排放到大气中会对人体和环境造成严重危害。近年来，国家对PH₃的排放进行了严格的规定，因此，尾气中PH₃的深度净化受到了广泛的关注。干法是主流的PH₃净化技术，主要包括吸附法和催化法。相较于湿法，干法具有性能好、稳定性强、耗水量小以及不产生二次污染等优点。本文首先从吸附法入手，分别探讨了复合金属氧化物吸附剂、活性炭基吸附剂及其他材料（分子筛、二氧化硅等）的研究现状，深入分析了各类脱磷吸附剂的结构性质及优缺点。其次对催化分解PH₃的机理进行了总结归纳，重点讨论了各类催化剂的构-效关系。最后，介绍了其他干法（燃烧法、等离子体降解法、生物法）在PH₃净化领域的应用。在此基础上，讨论了干法脱磷技术的主要优势以及面临的挑战，并对干法脱除PH₃技术的发展方向进行了展望。本工作可以为脱磷吸附剂/催化剂的构建和设计提供参考和指导。

关键词: PH₃, 吸附剂, 催化剂, 氧化, 载体, 干法净化技术

Abstract:

Phosphine (PH₃) is a highly toxic gas that comes from a wide range of sources. If it is discharged into the atmosphere without treatment, it will cause serious harm to the human body and the environment. In recent years, the state has imposed strict regulations on the emission of PH₃, so the deep purification of PH₃ from exhaust gas has received widespread attention. The dry methods are the mainstream PH₃ purification technology, which mainly include adsorption and catalytic methods. Compared with the wet method, the dry method has the advantages of good performance, high stability, low water consumption, and no secondary pollution. In this paper, starting from the adsorption method, the research status of composite metal oxide adsorbent, activated carbon adsorbent, and other materials (molecular sieve, silica, etc) were discussed, and the structural properties and advantages and disadvantages of various types of dephosphorylated adsorbents were analyzed in depth. Secondly, the mechanism of catalytic decomposition of PH₃ was summarized, focusing on the structure-activity relationship of various types of catalysts. Finally, the application of other dry methods (combustion, plasma degradation, and biological methods) in the field of PH₃ purification were introduced. On this basis, the main advantages of dry dephosphorization technologies as well as the challenges are discussed, and the direction of development of dry PH₃ removal technologies is envisioned. This work is expected to provide reference and guidance for the construction and design of adsorbents/catalysts for phosphorus removal.

Key words: PH₃, adsorbents, catalysts, oxidation, support, dry purification technology

中图分类号:

TQ 09

杨学金, 杨金涛, 宁平, 王访, 宋晓双, 贾丽娟, 冯嘉予. 剧毒气体PH₃的干法净化技术研究进展[J]. 化工学报, 2023, 74(9): 3742-3755.

Xuejin YANG, Jintao YANG, Ping NING, Fang WANG, Xiaoshuang SONG, Lijuan JIA, Jiayu FENG. Research progress in dry purification technology of highly toxic gas PH₃[J]. CIESC Journal, 2023, 74(9): 3742-3755.

图/表 7

图1 PH3的干法净化技术

Fig.1 Dry purification technology for PH3

表1 铜基材料PH3净化条件对比

Table 1 Comparison of PH3 purification conditions for copper-based materials

材料种类	活性组分	吸附剂比表面积/(m²/g)	吸附剂总孔容/(cm³/g)	吸附剂平均孔径/nm	气体组成	反应温度/℃	气体总流速/(ml/min)	质量空速/(ml/(h·g))	穿透标准	磷容/(mg/g)	文献
Ce-Cu-Al	CuO	45.8	0.10	4.5	N₂ + H₂S + PH₃ + 1% O₂	70	500	10000	—	201.9	[42]
Cu-Fe-Ce	CuO	110.27	0.16	5.64	N₂ + 456 mg/m³ H₂S + 911 mg/m³ PH₃ + 1% O₂	70	—	30000	—	151.7	[43]
30Cu@TiO₂	CuO	63.77	0.31	—	N₂ + 1518 mg/m³ PH₃	120	100	30000	90%	135.73	[32]
Cu _x /TiO₂	CuO	110.3	0.31	5.7	N₂ + 1518 mg/m³ PH₃+ 1% O₂	90	100	60000	97%	136.2	[30]
Cu/TiO₂	CuO	—	—	—	N₂ + 759 mg/m³ PH₃	25	100	—	99%	108.48	[27]
Cu/γ-Al₂O₃	CuO	232	0.43	—	N₂ + 76 mg/m³ PH₃	20	60	—	90%	32.09	[28]
Flower-shaped CuO/AC	CuO	—	—	—	N₂ + PH₃ + 1.6% O₂	110	—	750	—	96.08	[44]
Cu _x /ACF	CuO	1768.9	0.57	0.96	N₂ + H₂S + PH₃ + 0.5% O₂	90	—	36000	—	132.1	[45]
Modified walnut-shell ACs	CuO	1419	0.70	—	N₂ + 1518 mg/m³ PH₃+ 1% O₂	120	250	—	90%	284.12	[46]
Cu/HZSM-5-[S1]	CuO	192.2	0.11	2.1	N₂ + 684 mg/m³ H₂S + 911 mg/m³ PH₃ + 1 % O₂	90	100	20000	60%	150.90	[47]
Ce₁Cu₃₀O _x /HZSM-5	CuO	282	0.16	2.26	N₂ + 1214 mg/m³ PH₃ + 1 % O₂	90	100	15000	60%	114.36	[29]
Cu/SBA-15	CuO	177.6	0.252	5.31	N₂ + 304 mg/m³ H₂S + 1214 mg/m³ PH₃ + 0.5 % O₂	80	100	10000	60%	104. 84	[48]
Cu-Fe / SBA-15	CuO	206.3	—	5.49	N₂ + 304 mg/m³ H₂S + 1214 mg/m³ PH₃ + 0.5 % O₂	80	100	10000	60%	120. 05	[49]
Cu-Fe /硅藻土	CuO	45.33	0.415	9.74	N₂ + 304 mg/m³ H₂S + 1214 mg/m³ PH₃ + 0.5 % O₂	80	100	10000	60%	29.61	[50]

图2 (a) 不同酸的使用对Ce-Cu-Al吸附剂性能的影响[42]；(b) 三种Ce-Cu-Al吸附剂的H2-TPR谱图[42]；(c) 30Cu@TiO2和TiO2的CO2-TPD谱图[32]；(d) 不同负载量时XCu@TiO2的BET分析[32]；(e) Cu x /TiO2净化PH3机理图[30]；(f) XCu@TiO2脱除PH3反应机理[32]；(g) Cu x /TiO2的H2-TPR谱图[30]；(h) Cu x /TiO2的CO2-TPD谱图[30]；(i) Cu/TiO2吸附剂在不同气氛下的PH3失活曲线[27]；(j) CuCl2改性γ-Al2O3吸附剂四次再生循环后的磷容[28]

Fig.2 (a) Effect of different acids on the performance of Ce-Cu-Al adsorbents[42]; (b) H2-TPR profiles of three kinds of Ce-Cu-Al adsorbents[42]; (c) CO2-TPD profiles of 30Cu@TiO2 and TiO2[32]; (d) BET analysis of XCu@TiO2 at different loading levels[32]; (e) Cu x /TiO2 purification mechanism of PH3[30]; (f) XCu@TiO2 reaction mechanism for PH3 removal[32]; (g) H2-TPR profiles of Cu x /TiO2[30]; (h) CO2-TPD profiles of Cu x /TiO2[30]; (i) PH3 deactivation curves of Cu/TiO2 adsorbents under different atmospheres[27]; (j) Phosphorus capacity of CuCl2-modified γ-Al2O3 adsorbent after four regeneration cycles[28]

图3 (a) 反应前后吸附剂的SEM图像[52]；(b) 不同活性炭吸附剂的PH3穿透曲线[52]；(c) PH3在浸渍活性炭上吸附的班厄姆吸附动力学曲线[53]；(d) 花型和不规则型CuO/AC吸附剂磷容[44]；(e) 花型CuO/AC吸附剂的SEM图像[44]；(f) 不同浓度CuAc2浸渍AC的PH3穿透曲线[55]；(g) 不同焙烧温度下Cu x /ACF吸附剂的XRD谱图[45]；(h) Cu0.15/ACF的原位红外光谱图[45]；(i) 3DCuO/C吸附剂的SEM图像[31]；(j) 3DCuO/C吸附剂的EPR谱图[31]；(k) 三种改性吸附剂的磷容对比[46]；(l) Cu/ACF-X的CO2-TPD谱图[60] (1 G=10-4 T)

Fig.3 (a) SEM images of the adsorbent before and after the reaction[52]; (b) PH3 breakthrough curves of different activated carbon adsorbents[52]; (c) Banham adsorption kinetic curve of PH3 adsorption on impregnated activated carbon[53]; (d) Phosphorus capacity of flower-shaped and irregular CuO/AC adsorbents[44]; (e) SEM image of flower type CuO/AC adsorbent[44]; (f) PH3 breakthrough curves of AC impregnated with different concentrations of CuAc2[55]; (g) XRD patterns of Cu x /ACF adsorbents at different calcination temperatures[45]; (h) In situ infrared spectrogram of Cu0.15/ACF[45]; (i) SEM images of 3DCuO/C adsorbent[31]; (j) EPR spectrum of 3DCuO/C adsorbent[31]; (k) Comparison of phosphorus capacity of three modified adsorbents[46]; (l) CO2-TPD profiles of Cu/ACF-X[60]

图4 (a) 不同吸附剂的PH3突破曲线[47]；(b) Cu/HZSM-5-[S0]和Cu/HZSM-5-[S1]的CO2-TPD谱图[47]；(c) 不同Ce掺杂时吸附剂的突破曲线[29]；(d) 不同硝酸浓度改性Cu/SBA-15时吸附剂的PH3吸附/氧化性能[48]；(e) Cu/SBA-15的原位IR光谱[48]；(f) 不同样品的NH3-TPD曲线[49]；(g) 不同含量的Fe掺杂时Cu-Fe/SBA-15吸附剂的BET分析[50]；(h) 不同含量的Fe掺杂时Cu-Fe/硅藻土吸附剂的穿透曲线[50]；(i)、(j) 不同含量的Ce掺杂时吸附剂的EDS映射(Cu和Ce)图像[29]；(k) NaCl溶液改性5A分子筛前后的SEM图像[61]；(l) Cu-Fe/硅藻土吸附剂的SEM图像[50]

Fig.4 (a) PH3 breakthrough curves for different adsorbents[47]; (b) CO2-TPD profiles of Cu/HZSM-5-[S0] and Cu/HZSM-5-[S1][47]; (c) Breakthrough curves of adsorbents at different Ce doping[29]; (d) PH3 adsorption/oxidation performance of adsorbents at different nitric acid concentrations modified with Cu/SBA-15[48]; (e) In situ IR spectra of Cu/SBA-15[48]; (f) NH3-TPD curves of different samples[49]; (g) BET analysis of Cu-Fe/SBA-15 adsorbent at different levels of Fe doping[50]; (h) Breakthrough curves of Cu-Fe/diatomite adsorbents at different levels of Fe doping[50]; (i), (j) EDS mapping (Cu and Ce) images of the adsorbent at different levels of Ce doping[29]; (k) SEM images before and after modification of 5A molecular sieve by NaCl solution[61]; (l) SEM images of Cu-Fe/diatomite adsorbent[50]

图5 (a) 不同温度下各催化剂的PH3分解性能[67]；(b) 催化剂反应后的XRD谱图[67]；(c) 额外煅烧还原后和正常煅烧还原后的催化剂在425℃时的PH3分解率和催化剂f在不同温度时的PH3分解率[35]；(d) 不同Ni∶Fe摩尔比合成的催化剂m在425℃下的PH3分解率[35]；(e) FeNiO/HNTs和BFeNiO/HNTs的H2-TPR谱图[9]；(f) 不同纳米材料催化剂的PH3等温分解实验[36]；(g) P层表面PH3的不同状态示意图[36]；(h) CuFeP催化剂PH3分解产物XRD谱图[34]；(i) Ni/Fe3O4/TiO2催化剂催化分解PH3机理[35]；(j) FeNi/HNTs催化剂催化分解PH3机理[9]

Fig.5 (a) PH3 decomposition performance of each catalyst at different temperatures[67]; (b) XRD pattern of the catalyst after reaction[67]; (c) PH3 decomposition rates of catalysts after additional calcination reduction and normal calcination reduction at 425℃ and PH3 decomposition rates of catalyst f at different temperatures[35]; (d) PH3 decomposition rates at 425℃ for catalysts m synthesized with different Ni∶Fe molar ratios[35]; (e) H2-TPR profiles of FeNiO/HNTs and BFeNiO/HNTs[9]; (f) PH3 isothermal decomposition test of different nanomaterial catalysts[36]; (g) Schematic diagram of the different states of PH3 on the surface of P-layer[36]; (h) XRD pattern of CuFeP catalyst PH3 decomposition products[34]; (i) Mechanism of catalytic decomposition of PH3 by Ni/Fe3O4/TiO2 catalyst[35]; (j) Mechanism of catalytic decomposition of PH3 by FeNi/HNTs catalysts[9]

表2 几种不同纳米材料催化剂催化分解PH3条件对比

Table 2 Comparison of conditions for catalytic decomposition of PH3 by several different nanomaterial catalysts

纳米材料种类	活性组分	气体组成	气体总流速/(ml/min)	催化剂用量/g	质量空速/(ml/(h·g))	催化分解温度/℃	分解效率/%	分解产物	文献
Co/CNTs、Ni/CNTs、 Fe₂O₃/CNTs	Co₃O₄、NiO、Fe₂O₃	N₂+5% PH₃	60	0.3	2520	400	100	P、H₂、CoP、NiP₂、FeP	[66-67]
Ni/Fe₃O₄/TiO₂	Fe₃O₄、Ni	N₂+1% PH₃	—	0.2	3000	425	100	P₄	[35]
FeNi/HNTs	Fe₃O₄、Ni	N₂+5% PH₃	—	—	2520	420	100	P+H₂	[9]
Ni⁰@Fe₃O₄/HNTs	Fe₃O₄、Ni⁰	N₂+1% PH₃	—	0.1	1200	300~450	100	P+H₂	[36]
CuFeP	Fe、Cu	N₂+PH₃	88	—	—	400~500或>800	100	Fe₂P+Fe₃P	[34]
Co-P非晶合金	CoP	N₂+PH₃	70	—	—	470	99.8	高纯P	[33]

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剧毒气体PH₃的干法净化技术研究进展

Research progress in dry purification technology of highly toxic gas PH₃

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