在国家“双碳”目标背景下，减少煤炭行业的碳排放、实现碳封存已成为亟待解决的难题。煤炭行业作为高碳化石能源生产者和主体碳排放源提供者，在生产和消费过程中引发的大宗固废堆存、大型采空区形成和大量CO₂排放是制约煤炭可持续开发利用与绿色健康发展的瓶颈所在。为协同解决二氧化碳封存与固废消纳问题，基于功能性充填技术在煤矿采空区中构筑CO₂封存空间，利用碱性固废矿化封存CO₂，既可以实现CO₂安全封存，又可以有效处理采空区与规模化处置固废，对煤炭行业高质量发展具有重要意义。

本研究以改性镁渣为研究对象，提出了两级矿化方法（即先搅拌矿化后矿化养护），围绕改性镁渣矿化反应过程与矿物相转化特性，分析了改性镁渣两级矿化反应机制与反应动力学。为进一步提高固碳效率，以添加外加剂的方法提高固碳效率，探明了外加剂对改性镁渣的固碳增效机制。深入分析了改性镁渣矿化材料的性能演化规律，基于以上理论研究结果开展了采空区改性镁渣矿化封存CO₂的工业示范试验，进一步验证了改性镁渣矿化材料的固碳性能。主要研究工作及重新成果如下：

      （1）提出了碱性固废两级矿化方法，设计了搅拌固碳反应装置，探明了反应参数（液固比、搅拌速率、通气速率、通气时间）对固碳特性的影响机制，确定了最佳矿化反应参数。对比分析了一级搅拌固碳、矿化养护与两级矿化改性镁渣的矿化反应特性，改性镁渣中的主要矿物成分β-C₂S的矿化产物主要为方解石与硅胶。两级矿化的固碳量相较于一级搅拌固碳，提高了205.02%；相较于矿化养护，两级矿化的固碳量提高了92.68%。明确了改性镁渣的两级矿化机制，主要为CO₂在基体孔隙内的扩散与溶解、Ca²⁺从内部基质扩散到表面、碳酸盐沉淀三个过程。

      （2）设计研发了矿化热测量设备，基于反应热力学计算与矿化反应热，分析了改性镁渣矿化反应过程，并通过分子动力学模拟了改性镁渣中的主要矿物β-C₂S的矿化反应过程；基于改性镁渣矿化材料中钙镁离子浸出浓度与pH变化规律，探明了钙镁离子浸出-CO₂溶解-碳酸盐生成的传质过程。明确了改性镁渣矿物颗粒由表面向内分别为碳酸钙产物层，中间位无定形硅胶层，与内部的未反应的矿物颗粒，基于缩核模型建立了改性镁渣矿化反应动力学模型。

     （3）改性镁渣颗粒表面的碳酸钙与硅胶层阻碍了碱性钙镁离子的浸出以及CO₂的溶解扩散，是限制矿化反应程度的主要原因之一。系统探究了NH₄Cl、NaCl与EDTA-2Na对改性镁渣矿化材料的固碳量、强度以及矿化产物等影响规律，揭示了不同外加剂对改性镁渣矿化反应的增效机制。NH₄Cl主要通过对改性镁渣颗粒表面产生侵蚀溶解作用与调节pH的作用，加快了碱性离子的浸出。改性镁渣中NH₄Cl掺量为1%时，固碳量提升18.79%。EDTA-2Na主要通过螯合作用，促进Ca²⁺的溶解。0.1%的EDTA-2Na的加入可将固碳量提升18.82%，强度提高59.52%。氯化钠主要通过氯离子侵蚀破坏产物层与增强反应体系离子强度来提高矿化反应程度。添加1%的氯化钠可将固碳量提高15.82%，强度提高19.05%。

     （4）通过对矿化材料的性能研究，得到了矿化材料的孔结构分布、渗透特性以及矿化深度演化规律，明确了矿化材料由于矿化程度不同导致的非协调破坏模式，探明了矿化材料的强度强化机制。掌握了两级矿化后的改性镁渣中重金属元素：Cd、Cu、Cr、Zn、Pb与Ni浸出浓度随龄期不断降低的浸出规律，揭示了矿化材料矿化固化重金属的主要机理为物理包裹、吸附共沉淀与化学沉淀。

     （5）建立了CO₂充注方法与工艺技术、CO₂矿化材料制备与输送工艺、CO₂封存与监测方案，构筑了CO₂封存储库，开展了采空区CO₂矿化封存工程示范试验研究，形成了采空碱性固废矿化封存CO₂的新方法。示范试验7d时的固碳量为22.51%，矿化效率为39.80%，矿化7d时的单轴抗压强度最高为3.92MPa。根据自主研发的温度-湿度-pH-电导率实时监测系统，可间接获知矿化材料的反应程度。对采空区碱性固废矿化封存CO₂进行了碳减排核算，得到了采空区1t碱性固废矿化封存CO₂可减少碳排放195.55 kg。

Under the background of the national " double carbon " target, reducing carbon emissions and achieving carbon sequestration in the coal industry has become an urgent problem to be solved. As a producer of high-carbon fossil energy and a provider of main carbon emission sources, the coal industry's large-scale solid waste storage, large-scale goaf formation and large-scale CO₂ emissions caused in the process of production and consumption are the bottlenecks restricting the sustainable development and utilization of coal and green and healthy development. To collaboratively solve the problems of carbon dioxide storage and solid waste disposal, a CO₂ storage space is constructed in the goaf of coal mines based on functional filling technology. Alkaline solid waste mineralization is used to store CO₂, which can not only achieve safe CO₂ storage, but also effectively treat goaf and dispose of solid waste on a large scale. This is of great significance for the high-quality development of the coal industry.

In this study, the modified magnesium slag was taken as the research object, and a two-stage mineralization method was proposed. Based on the mineralization reaction process and mineral phase transformation characteristics of modified magnesium slag, the two-stage mineralization reaction mechanism and reaction kinetics of modified magnesium slag were analyzed. To further improve the carbon sequestration efficiency, the method of adding additives was used to enhance the carbon sequestration efficiency, and the mechanism of enhancing the carbon sequestration efficiency of modified magnesium slag by additives was explored. The performance evolution law of modified magnesium slag mineralized materials was deeply analyzed, and based on the above theoretical research results, carried out an industrial demonstration test of CO₂ sequestration by modified magnesium slag mineralization in goaf, further verifying the carbon fixation performance of modified magnesium slag mineralization materials. The main research conclusions are as follows:

(1) A two-stage mineralization method for alkaline solid waste was proposed, and a stirring carbon fixation reaction device was designed. The influence mechanism of reaction parameters (liquid-solid ratio, stirring rate, aeration rate, aeration time) on carbon fixation characteristics was explored, and the optimal mineralization reaction parameters were determined. The mineralization reaction characteristics of one-stage stirring carbon fixation, static mineralization and two-stage mineralization modified magnesium slag were compared and analyzed. The mineralization products of the main mineral component β-C₂S in the modified magnesium slag were mainly calcite and silica gel. The carbon sequestration capacity of two-stage mineralization increased by 205.02% compared to one-stage stirring carbon sequestration; Compared to static mineralization, the carbon sequestration of two-stage mineralization increased by 92.68%. The two-stage mineralization mechanism of modified magnesium slag has been clarified, mainly consisting of three processes: diffusion and dissolution of CO₂ in the matrix pores, diffusion of Ca²⁺from the internal matrix to the surface, and carbonate precipitation.

(2) The mineralization reaction process of modified magnesium slag was analyzed based on thermodynamic calculations and mineralization reaction heat using a modified mineralization heat measurement device. The mineralization reaction process of the main mineral β-C₂S in the modified magnesium slag was simulated by molecular dynamics; Based on the variation of calcium and magnesium ion leaching concentration and pH in modified magnesium slag mineralized materials, the mass transfer process of calcium and magnesium ion leaching CO₂ dissolution carbonate generation was investigated. A kinetic model for the mineralization reaction of modified magnesium slag was established based on the shrinking core model, which clarified that the modified magnesium slag mineral particles consist of a calcium carbonate product layer from the surface to the interior, an amorphous silica layer in the middle, and unreacted mineral particles inside.

(3) The calcium carbonate and silica gel layer on the surface of modified magnesium slag particles hinder the leaching of alkaline calcium and magnesium ions and the dissolution and diffusion of CO₂, which is one of the main reasons limiting the degree of mineralization reaction. The system investigated the effects of NH₄Cl, NaCl, and EDTA-2Na on the carbon fixation, strength, and mineralization products of modified magnesium slag mineralization materials, revealing the synergistic mechanism of different additives on the mineralization reaction of modified magnesium slag. NH₄Cl mainly accelerates the leaching of alkaline ions by causing erosion and dissolution on the surface of modified magnesium slag particles and adjusting pH. When the NH₄Cl content in modified magnesium slag is 1%, the carbon fixation capacity increases by 18.79%. EDTA-2Na mainly promotes the dissolution of Ca ions through chelation. The addition of 0.1% EDTA-2Na can increase carbon sequestration by 18.82% and strength by 59.52%. Sodium chloride mainly improves the degree of mineralization reaction by corroding and damaging the product layer with chloride ions and enhancing the ion strength of the reaction system. Adding 1% sodium chloride can increase carbon sequestration by 15.82% and strength by 19.05%.

(4) Through the study of the properties of mineralized materials, the pore structure distribution, permeability characteristics and the evolution law of mineralization depth of mineralized materials are obtained. The non-coordinated failure mode of mineralized materials due to different degrees of mineralization is clarified, and the strength strengthening mechanism of mineralized materials is proved. The leaching law of heavy metal elements such as Cd, Cu, Cr, Zn, Pb, and Ni in modified magnesium slag after two-stage mineralization was clarified, and the leaching concentration continuously decreased with age. The main mechanism of mineralization solidification of heavy metals in mineralized materials was identified as physical encapsulation, adsorption co precipitation, and chemical precipitation.

(5) The CO₂ injection methods and process technologies, CO₂ mineralization material preparation and transportation processes, CO₂ storage and monitoring plans were established, constructed CO₂ storage warehouses, and conducted demonstration experiments on CO₂ mineralization and storage projects in goaf areas. The carbon fixation amount at 7 days of demonstration experiment was 22.51%, the mineralization efficiency was 39.80%, and the highest uniaxial compressive strength at 7 days of mineralization was 3.92 MPa. Based on the self-developed real-time monitoring parameters of temperature humidity pH conductivity, the reaction degree of mineralized materials can be indirectly obtained. Carbon emission reduction accounting was conducted on the mineralized CO₂ storage of alkaline solid waste in goaf, and it was found that 1 ton of mineralized CO₂ storage of alkaline solid waste in goaf can reduce carbon emissions by 195.55 kg.

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