采空区CO₂储存作为解决煤炭行业碳排放难题的重要负碳技术储备，能够实现CO₂储存与固废资源充填利用等多种目标，在废弃资源二次利用、碳减排等方面具有广泛应用前景。化学储碳作为安全性、稳定性较高的储碳方式之一，存在自然状态下储碳强度低、周期长等问题，为了探究解决以上难题的途径通过采空区充填碱性固废协同储碳的技术理念得到广泛关注。因此，本文依托自主研发的CO₂地质储存综合实验平台，探讨了采空区储碳条件下CO₂-水界面特性及溶解传质规律，明晰了采空区煤岩体-CO₂反应的矿物溶解-矿化特征，揭示了碱性固废充填采空区协同CO₂矿化储碳效应，并提出了关闭矿井采空区“碱性固废+碎胀煤岩体”联合储碳技术思路、关键技术和风险监测手段，旨在为煤矿采空区CO₂安全高效封存提供理论支撑。主要成果如下：

自主研发了CO₂地质储存综合实验平台，包含CO₂-水原位界面张力测定系统、地球化学反应实验系统以及辅助检测设备。从气液界面张力、CO₂溶解性以及煤岩体溶解-矿化特性参数等方面开展相关研究，并可以开展碱性固废矿化转变及安全储碳机理探究实验，为后续章节提供可靠实验手段。

掌握了采空区储碳条件下CO₂-水界面特性及溶解传质规律，环境温度一定时，界面张力与环境压力呈线性负相关关系；环境温度升高，界面张力相应增加；界面张力与矿化度存在正相关性；CO₂-盐溶液之间界面张力呈现出随着阳离子价态升高而增大的现象；采空区环境压力与CO₂溶解度呈正相关关系，当温度为25℃、纯水条件下，压力由0.5 MPa增至2.5 MPa，对应CO₂溶解度由0.162 7 mol/kg升至0.714 1 mol/kg；CO₂溶解度随着温度与矿化度升高而降低；相同质量分数下，一价阳离子溶液比二价阳离子溶液可溶解更多CO₂。

明晰了采空区煤岩体-CO₂反应的矿物溶解-矿化特征，采空区煤岩体与CO₂反应主要包含3个过程：矿物溶解→元素释放-迁移→矿物转化-沉淀；采空区煤岩体主要的溶解性矿物为碳酸盐矿物与硅酸盐矿物，SiO₂溶解性较低，FeS₂仅在煤体中存在；主要的沉淀性矿物以方解石、铁白云石、菱铁矿、钠蒙脱石为主；方解石、白云石、菱铁矿一般会经历溶解再沉淀过程，钠/钙蒙脱石主要是由于长石等矿物溶解后经过迁移转化形成。

阐明了不同碱性固废矿化储碳能力特性，温度和压力均会促进溶解-矿化作用，碱性固废矿化反应动力学与其比表面积（即反应接触面）以及活性含钙物质的量之间存在显著关系，反应后期表面覆盖（有效反应面积降低）和活性点位减少成为矿化反应限制主要因素；温压参数与矿化储碳量、矿化效率变化趋势均存在正相关性，升高压力对加速矿化的影响主要是由于压力促使反应液中HCO₃^-/CO₃^2-离子加速溶解；碱性固废钙含量越高，对应矿化储碳量与矿化效率也会随之增大。

得出了CO₂扩散-溶解作用对采空区储碳安全性的影响特征，温度越高，水环境矿化度越高，相应盖层储碳安全阈值也随之增大，进一步计算了目标采空区相应理论盖层储碳安全阈值为4.28~4.29 MPa；对于采空区储碳而言，当注入的CO₂和密闭采空区流体之间压力差超过盖层储碳阈值时，毛细管就会发生破裂，注入的CO₂就会泄漏到大气中，因此合理评价采空区环境储碳安全性及注入参数是该技术实现的基础。

揭示了矿物溶解-矿化效应对采空区储碳安全性影响机制。对于采空区而言，短期内CO₂-H₂O-煤岩以溶解作用为主，孔裂隙扩张会增加其储碳能力，钙镁铁含量越高，会增强采空区煤岩体溶解-矿化效应，有利于储碳稳定性提升以及安全性增加；对于盖层（稳定的上覆岩层）而言，应当选择钙镁铁含量较低的泥岩（黏土矿物为主），减少溶解作用，并通过黏土矿物水化膨胀强化孔裂隙封堵能力，以此提升盖层密闭性和采空区储碳长时安全性。最后提出了关闭矿井采空区“碱性固废+碎胀煤岩体”联合储碳技术思路，对关键技术和风险监测手段进行了应用展望。

本研究立足于关闭矿井采空区安全高效储碳基础，通过完善CO₂充注采空区条件下煤岩-碱性固废溶解矿化规律及安全储碳理论体系，探究加快采空区CO₂安全高效稳定储碳的有效途径，为采空区CO₂储存的推广提供理论支撑、数据基础和实践指导。

As an important negative carbon technical reserve to solve the problem of carbon emission in coal industry, CO₂ storage in goaf can achieve various goals such as CO₂ storage and solid waste resource filling and utilization, and has a wide application prospect in the secondary utilization of waste resources and carbon emission reduction. Chemical carbon storage, as one of the safe and stable carbon storage methods, has some problems such as low carbon storage intensity and long period in natural state. In order to solve the above problems, the technical concept of collaborative carbon storage by filling industrial solid waste in goaf has been widely concerned. Therefore, based on the self-developed comprehensive experimental platform of CO₂ geological storage, this paper discusses the characteristics of CO₂-water interface and the law of dissolution and mass transfer under the condition of carbon storage in goaf, clarifies the mineral dissolution-precipitation characteristics of coal rock-CO₂ reaction in closed mine goaf, reveals the synergistic effect of CO₂ mineralization and carbon storage in goaf filled with alkaline solid waste, and puts forward the technical ideas, key technologies and risk monitoring methods of “alkaline solid waste + broken coal rock” combined carbon storage in closed mine goaf, aiming at providing theoretical support for safe and efficient storage of CO₂ in coal mine goaf. The main results are as follows:

We independently developed a comprehensive experimental platform for CO₂ geological storage. It includes CO₂-water in-situ interfacial tension measurement system, geochemical reaction experimental system and auxiliary detection equipment. Relevant experiments are carried out from the aspects of gas-liquid interfacial tension, CO₂ solubility and dissolution-mineralization characteristic parameters of coal and rock mass, and experiments on carbonation transformation of industrial solid waste and carbon storage mechanism can be carried out, providing reliable experimental means for subsequent chapters.

Grasp the characteristics of CO₂-water interface and the law of dissolution and mass transfer under the condition of carbon storage in goaf. When the ambient temperature is constant, there is a linear negative correlation between reservoir pressure and interfacial tension in goaf, and the interfacial tension increases with the increase of reservoir temperature. There is a positive correlation between salinity and interfacial tension; The interfacial tension between CO₂− salt solutions increases with the increase of cation valence. There is a positive correlation between the reservoir pressure in goaf and the solubility of CO₂. When the temperature is 25℃ and the water is pure, the pressure increases from 0.5 MPa to 2.5 MPa, and the solubility of CO₂ increases from 0.162 7 mol/kg to 0.7141 mol/kg. The solubility of CO₂ decreases with the increase of temperature and salinity. At the same mass fraction, monovalent cation solution can dissolve more CO₂ than divalent cation solution.

The mineral dissolution-precipitation characteristics of coal-rock mass -CO₂ reaction in goaf with water accumulation are clarified. The reaction between coal and rock mass and CO₂ in goaf with accumulated water mainly includes three processes: mineral dissolution → element release-migration → mineral transformation-precipitation; The main soluble minerals of coal and rock mass in goaf are carbonate minerals and silicate minerals, and the solubility of SiO₂ is low, and FeS₂ only exists in coal. The main sedimentary minerals are calcite, ankerite, siderite and sodium montmorillonite. Calcite, dolomite and siderite generally undergo the process of dissolution and re-precipitation, and sodium/calcium montmorillonite is mainly formed by mineral transformation after feldspar and other minerals are dissolved.

The characteristics of carbon storage capacity of different alkaline solid waste mineralization are clarified. Temperature and pressure will promote dissolution-mineralization. There is a significant relationship between the mineralization reaction kinetics of alkaline solid waste and its specific surface area (i.e. Reaction contacts surface) and the amount of active calcium-containing substances. In the later stage of the reaction, surface coverage (reduction of effective reaction area) and reduction of active sites become the main factors limiting the mineralization reaction. There is a positive correlation between temperature, pressure and mineralization carbon storage and mineralization efficiency. The effect of increasing pressure on accelerated carbonation is mainly due to the accelerated dissolution of HCO₃^-/ CO₃^2-ions in the reaction solution by pressure. The higher the calcium content of alkaline solid waste, the corresponding carbon storage and mineralization efficiency will also increase.

The influence characteristics of CO₂ diffusion-dissolution on the safety of carbon storage in goaf are obtained. The higher the temperature is, the higher the salinity of water environment is, and the corresponding safety threshold of carbon storage is also increased. Further, the safety threshold of sealing the corresponding cover is 4.28~4.29 MPa by using the water test in the goaf of the study area. For carbon storage in mined-out areas, when the pressure difference between injected CO₂ and reservoir fluid exceeds the sealing threshold of caprock, the capillary will break, and the injected CO₂ will leak into the atmosphere. Therefore, it is the basis for the realization of this technology to reasonably evaluate the environmental carbon storage safety and injection parameters in mined-out areas.

The influence mechanism of mineral dissolution-mineralization effect on the safety of carbon storage in goaf is revealed. For the reservoir, CO₂-H₂O- coal is mainly dissolved in a short period of time, and the expansion of pores and fractures will increase its carbon storage capacity. The higher the content of calcium, magnesium and iron, the better the dissolution-mineralization effect of the reservoir, which is conducive to the stable improvement of carbon storage and the increase of safety. For the caprock (stable overlying strata), mudstone (mainly clay minerals) with low calcium, magnesium and iron content should be selected to reduce dissolution, and the pore and fracture sealing effect should be increased through the hydration of clay minerals, so as to improve the sealing property of caprock and strengthen the long-term safety of carbon storage in goaf. Finally, the idea of “industrial solid waste+crushed coal and rock mass” combined carbon storage technology in goaf is put forward, and the application prospect of key technologies and industrial processes is carried out.

This study is based on the safe and efficient carbon storage in the closed mine goaf. By improving the dissolution and mineralization law of coal-rock-alkaline solid waste and the theoretical system of safe carbon storage under the condition of CO₂ filling in the goaf, it explores effective ways to accelerate the safe, efficient and stable carbon storage in the goaf, providing theoretical support, data foundation and practical guidance for the promotion of CO₂ storage in the goaf.

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