煤炭是我国的化石能源和主体能源，在国民经济发展中占据非常重要的地位。在开采同时产生采空区等矿井地下空间，随着煤化工行业的迅速发展，在生产和消费过程中又产生了大量固体废弃物——煤气化粗渣（Coal Gasification Coarse Slag，CGCS）及CO₂等副产物。在“双碳”战略目标引领下，将CO₂封存于煤矿地下空间有望实现矿区内碳资源的高效闭环管理，推动“就地生产、就地利用、就地封存”的绿色低碳开发路径。然而，由于井下环境普遍潮湿，CGCS基沸石分子筛存在较强亲水性，水分子的竞争吸附效应会显著抑制其对CO₂的吸附能力。因此，提升分子筛的疏水性是增强其在潮湿矿井环境中CO₂吸附性能的关键。本文以CGCS为原料合成沸石分子筛，并通过多种方法对其疏水性能进行优化，旨在提升其在矿井采空区对CO₂的吸附效果。具体研究内容如下：

（1）以CGCS为原料，通过对CGCS预处理后采用碱熔融-水热合成法制备结构完整、结晶度高的沸石分子筛，并进行了系统表征。结果表明，该材料具有显著亲水特性：静态水吸附量为17.61%，静态水接触角为14.1°，硅铝比(SiO₂/Al₂O₃摩尔比)较低为1.39，同时含有大量亲水的-OH，比表面积为47.61 m²/g。

（2）采用气相沉积法（CVD），以C₁₆TMS为改性剂对CGCS基沸石分子筛进行疏水改性。结果表明，在CGCS基沸石分子筛与C₁₆TMS量比为1:2，反应温度为180℃，反应时间为12 h时样品综合性能较优，与未改性CGCS基沸石分子筛相比，吸水量下降至12.66%，静态水接触角提高至55.3º，比表面积下降了4.301 m²/g，外表面积下降了27.955 m²/g，孔容下降了0.115 cm³/g，改性后分子筛的骨架结构未被破坏，且疏水性有所提高。

（3）采用盐酸和柠檬酸对CGCS基沸石分子筛进行脱铝处理以提高其硅铝比。对比分析表明，柠檬酸改性效果更佳。在柠檬酸溶液浓度为3 mol/L，反应温度为90℃，反应时间为9 h时样品综合性能较优，静态水吸附量降低至12.64%，静态水接触角提高至50º，比表面积由47.615 m²/g提高为239.171 m²/g大幅度提升。改性后样品的硅铝比与疏水性提高。

（4）采用单组份气体吸附实验台测定柠檬酸改性最佳样品（A-CA-B）在不同湿度下的CO₂吸附性能，并通过饱和盐溶液调控RH=33%、58%、75%。结果表明，A-CA-B在RH<1%时吸附量为268.4 g/cm³，随湿度升高吸附量下降，RH=75%时降幅达21.3%，与未改性样品相比疏水性增强。Langmuir模型能较好拟合不同湿度下的吸附行为（R²=0.94718~0.99527），Freundlich和Temkin模型在高湿环境下适用性较差。动力学分析显示，A-CA-B吸附速率提高，平衡时间缩短约30 min。循环实验表明，A-CA-B在RH=75%条件下五次循环后吸附下降率仅10.9%，表现出良好的再生性能。

Coal is China's fossil energy and the main energy, and occupies a very important position in the development of the national economy. With the rapid development of coal chemical industry, a large number of greenhouse gases such as coal gasification coarse slag (CGCS) and CO₂ are produced in the production and consumption process. Under the strategic background of "double carbon" goal, CO₂ storage in underground space of coal mine is expected to realize the efficient closed-loop management of carbon resources in the mining area, and build a green recycling development mode of "on-site production, on-site utilization and on-site storage". However, the downhole environment usually has high humidity characteristics, and CGCS based zeolite molecular sieve has strong hydrophilicity, which is easy to compete to adsorb water molecules and reduce the adsorption capacity of CO₂. Therefore, improving the hydrophobicity of zeolite molecular sieve is very important to improve its CO₂ adsorption performance in underground wet environment. In this paper, zeolite molecular sieve was prepared from coal gasification coarse slag (CGCS) and its hydrophobicity was optimized to improve its CO₂ adsorption performance in mine goaf. The specific research contents are as follows:

(1) Using CGCS as raw material, zeolite molecular sieves were prepared by alkali fusion hydrothermal synthesis after CGCS pretreatment, and a series of characterization tests were carried out. The results show that the structure is complete, the crystallinity is high, the static water adsorption capacity is 17.61%, the static water contact angle is 14.1 °, the silicon aluminum ratio is 1.39, and contains a large amount of hydrophilic -oh, with a specific surface area of 47.61 m²/g.

(2) Using cetyltrimethoxysilane (C₁₆TMS) as modifying agent, CGCS based zeolite molecular sieve was modified by silane under different conditions by vapor deposition (CVD) to reduce its surface hydrophilic functional groups. It was found that the skeleton structure of the modified molecular sieve was not destroyed, and the hydrophobicity was improved. When the molar ratio of CGCS based zeolite to c16tms was 1:2, the reaction temperature was 180 ℃, and the reaction time was 12 h, the comprehensive performance of the sample was better. Compared with the unmodified CGCS based zeolite, the water absorption was 12.66%, which decreased by 4.96%, the static water contact angle was 55.3 ℃, which increased by 41.2 ℃, the specific surface area decreased by 4.301 m²/g, the surface area decreased by 27.955 m²/g, and the pore volume decreased by 0.115 cm³/g.

(3) Using hydrochloric acid and citric acid as modifying agents, the CGCS based zeolite molecular sieve was dealuminated under the same conditions to improve the silicon aluminum ratio. Considering the results of XRD and water absorption of the modified samples, citric acid was selected as the optimal modifier. The CGCS based zeolite molecular sieve was dealuminated by citric acid under different conditions. It was found that the silicon aluminum ratio and hydrophobicity of the modified sample were improved. When the concentration of citric acid solution was 3 mol/L, the reaction temperature was 90 ℃, and the reaction time was 9 h, the comprehensive performance of the sample was better. Compared with the unmodified CGCs based zeolite molecular sieve, the static water adsorption capacity was 12.64%, which was reduced by 4.97%, the static water contact angle was 50 º, which was increased by 35.9 º, and the specific surface area was significantly increased from 47.615 m²/g to 239.171 m²/g.

(4) The adsorption performance of citric acid modified best sample (A-CA-B) at different humidity was measured by a single component gas adsorption test-bed, and the RH=33%, 58%, 75% were adjusted by saturated salt solution. The results showed that the adsorption capacity of A-CA-B was 268.4 g/cm³ at RH<1%, which decreased with the increase of humidity, and decreased by 21.3% at RH=75%. Compared with the unmodified sample, the hydrophobicity of A-CA-B was enhanced. Langmuir model can better fit the adsorption behavior under different humidity (R²=0.94718~0.99527), while Freundlich and Temkin models are not suitable for high humidity environment. Kinetic analysis showed that the adsorption rate of a-ca-b was increased and the equilibrium time was shortened by about 30min. The cycle experiment showed that the adsorption rate of a-ca-b was only 10.9% after five cycles at RH=75%, showing good regeneration performance.

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