煤气化作为煤炭高效、清洁利用的核心技术之一，将煤转化为合成气的同时也产生了巨量的煤气化渣。目前，煤气化渣处理主要以堆积和填埋为主，不仅处理成本大，还造成了严重的环境污染。核能是现阶段大力发展的新能源之一，核能中铀-235核裂变过程中会产生碘的放射性同位素，¹³¹I和¹²⁹I，对人类健康和生存环境造成了巨大的长期风险。煤气化渣一般可分粗渣和细渣。煤气化细渣具有粒度细、残炭量大等特点，具有转化为多孔材料的优势和潜力。为此，本文选择水煤浆气化细渣为研究对象，开展煤气化细渣制备多孔材料及其在放射性碘废水处理中的应用研究。首先，重点开展了超声强化酸浸法对气化细渣高炭组分的碘吸附性能和结构性质的研究，揭示了多孔材料结构特征和超声强化作用机理；其次，以超声酸浸法制备的多孔材料为原料，分别制备了多孔炭材料、ZSM-5分子筛和多孔炭/ZSM-5复合材料，探究了上述材料的碘吸附性能。研究工作对于煤气化细渣材料化利用，以及含放射性碘废水的处理具有一定理论和实际意义。主要研究结果如下：

(1)在煤气化细渣的粒度组成特性研究基础上，通过湿法筛分的方法分选出煤气化细渣高炭组分。采用BET、SEM等分析方法，研究了气化细渣高炭组分的组成结构。结果表明，残炭具有明显的粒度依存性，125~250 μm和250~500 μm粒度级的固定碳含量高达60%以上，为典型的高炭组分；该高炭组分拥有丰富的孔结构，且以介孔为主。

(2)以高炭组分为原料，探究了超声酸浸条件对煤气化细渣高炭组分碘吸附性能和结构性质的影响。结果表明：在酸浓度为4 mol/L、超声时间为1.5 h、超声功率为210 W、和酸浸温度为50 ℃时，所制备的多孔材料具有最佳碘吸附性能，碘吸附值达到468.53 mg/g，其比表面积达到474.97 m²/g，且具有以介孔为主的丰富孔隙结构。超声时间、酸浓度和超声功率是影响多孔材料孔结构与碘吸附性能主要因素。在酸浸过程中引入超声场，能够有效促进灰组分中金属元素的溶出，强化酸浸的传质效果，还能使SiO₂和残炭得到富集。超声酸浸对残炭的作用不仅有利于碳灰粘结体的解离，还会使堵塞在孔道内的灰颗粒脱附，从而使残炭孔隙结构连通性增加；此外，超声空化作用和机械作用能够促进碳颗粒表面裂纹的产生，促进微孔结构的发展，增强碳颗粒内部无机组分的可及性。

(3)以超声酸浸后的多孔材料为原料，分别采用化学活化法和水热活化法制备了多孔炭和ZSM-5分子筛，并进行了条件优化，并在此基础上成功制备了多孔炭/ZSM-5复合材料。结果表明，在活化温度为850 ℃、活化时间为1.5 h和活化剂KOH用量质量比为3的条件下，制备的多孔炭材料的碘吸附值为1057.55 mg/g，比表面积高达905.70 m²/g，且具有丰富微孔-中孔结构。ZSM-5分子筛最佳的合成条件是晶化时间3天，晶化温度160 ℃，导向剂（25%四丙基氢氧化铵溶液）的用量摩尔比为0.35。水热时间对ZSM-5分子结晶度和形貌有重要影响。采用化学活化-水热晶化两步法制备了多孔炭/ZSM-5复合材料。在上述最优条件下制备的多孔炭/ZSM-5复合材料具有丰富的比表面积和孔隙结构，其碘吸附值高达1126.74 mg/g，比表面积高达917.70 m²/g。碘吸附容量取决于多孔炭/ZSM-5复合材料的孔隙结构及活性位点等多因素，大孔和中孔结构有利于水中碘的传质，微孔结构能够进行优良的碘吸附，较大的比表面积能提供较多的活性位点。

Coal gasification, as one of the core technologies for efficient and clean utilization of coal, produces a large amount of coal gasification slag while converting coal into syngas. At present, coal gasification slag treatment is mainly accumulated and landfilled, which not only costs a lot, but also causes serious environmental pollution. Nuclear energy is one of the new energy sources vigorously developed at the present stage. The radioactive isotopes of iodine, ¹³¹I and ¹²⁹I, will be produced during the nuclear fission of uranium-235 in nuclear energy, which poses a huge long-term risk to human health and living environment. Coal gasification slag can be divided into coarse slag and fine slag. Coal gasification fine slag has the characteristics of fine particle size and large amount of carbon residue, which has the advantage and potential of transforming into porous materials. Therefore, in this paper, coal water slurry gasification fine slag is selected as the research object to prepare porous materials and its application in the treatment of radioactive iodine wastewater. Firstly, the study on the iodine adsorption and structural properties of high-carbon components of gasification fine slag by ultrasonic enhanced acid leaching was focused on, and the structural characteristics of porous materials and the mechanism of ultrasonic enhanced action were revealed. Secondly, porous carbon, ZSM-5 molecular sieve and porous carbon /ZSM-5 composite materials were prepared by ultrasonic acid leaching, and the iodine adsorption properties of these materials were investigated. The research work has certain theoretical and practical significance for the material utilization of coal gasification fine slag and the treatment of radioactive iodine wastewater. The main findings are as follows:

(1) Based on the study of particle size composition characteristics of fine coal gasification slag, the high-carbon components of fine coal gasification slag were separated by wet screening method. The composition and structure of high-carbon components of fine gasification slag were studied by BET and SEM. The results show that the carbon residue has obvious grain size dependence, and the fixed carbon content of 125~250μm and 250~500μm particle size is more than 60%, which is a typical high carbon component. The high-carbon component has abundant pore structure and is mainly mesoporous.

(2) The effect of ultrasonic acid leaching on the iodine adsorption and structural properties of high-carbon components of coal gasification fine slag was studied. The results show that: When the acid concentration is 4 mol/L, ultrasonic time is 1.5 h, ultrasonic power is 210 W, and the acid leaching temperature is 50 ℃, the prepared porous material has the best iodine adsorption performance, the iodine adsorption value is 468.53 mg/g, the specific surface area is 474.97 m²/g, and the pore structure is mainly mesoporous. Ultrasonic time, acid concentration and ultrasonic power are the main factors affecting the pore structure and iodine adsorption performance of porous materials. The introduction of ultrasonic field in the acid leaching process can effectively promote the dissolution of metal elements in the ash component, strengthen the mass transfer effect of acid leaching, and enrich SiO₂ and carbon residue. The effect of ultrasonic acid leaching on carbon residue is not only conducive to the dissociation of carbon ash binder, but also to the desorption of ash particles blocked in pores, thus increasing the connectivity of carbon residue pore structure. In addition, ultrasonic cavitation and mechanical action can promote the formation of surface cracks of carbon particles, promote the development of microporous structures, and enhance the accessibility of inorganic components inside carbon particles.

(3) Porous carbon and ZSM-5 molecular sieves were prepared by chemical activation method and hydrothermal activation method respectively from the porous material after ultrasonic acid leaching, and the conditions were optimized. On this basis, porous carbon /ZSM-5 composites were successfully prepared. The results show that under the conditions of activation temperature 850 ℃, activation time 1.5 h and KOH dosage/mass ratio 3, the iodine adsorption value of the prepared porous carbon material is 1057.55 mg/g, the specific surface area is up to 905.70 m²/g, and the structure of micropore and mesopore is abundant. The optimum synthesis conditions of ZSM-5 molecular sieve were crystallization time of 3 days, crystallization temperature of 160 ℃, and molar ratio of guide agent (25% tetrapropyl ammonium hydroxide solution) of 0.35. The hydrothermal time has an important effect on the crystallinity and morphology of ZSM-5 molecules. Porous carbon /ZSM-5 composites were prepared by a two-step process of chemical activation and hydrothermal crystallization. The porous carbon /ZSM-5 composite prepared under the above optimal conditions has rich specific surface area and pore structure, with iodine adsorption value up to 1126.74 mg/g and specific surface area up to 917.70 m²/g. The adsorption capacity of iodine depends on the pore structure and active sites of porous carbon /ZSM-5 composites. The large and medium pore structures are conducive to the mass transfer of iodine in water, the micropore structures can perform excellent iodine adsorption, and the large specific surface area can provide more active sites.

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