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基于一步相转移-碳化法的电石渣制备纳米碳酸钙工艺研究
Research on the process of preparing nano calcium carbonate from calcium carbide slag based on one-step phase transfer carbonization method
【摘要】 电石渣是电石法生产乙炔过程中产生的副产品,属于Ⅱ级工业固废,其主要成分是Ca(OH)2,实现电石渣的高值化、规模化、集约化利用,对于节约资源和保护环境具有重要意义。本文采用一步相转移-碳化法,以工业电石渣为原料制备纳米碳酸钙,以Ca2+相转移率为考察指标,开展了单因素条件试验和正交试验,采用X射线衍射仪(XRD)、场发射扫描电子显微镜(FE-SEM)、场发射透射电子显微镜(FE-TEM)等手段对样品形貌和结构进行表征分析。结果表明:适宜的相转移反应工艺条件为相转移剂摩尔比4∶3、反应温度3℃、反应时间20 min、搅拌速率200 r/min,此条件下Ca2+相转移率达91.97%;经筛选确定DG2为较适宜的晶型控制剂,较优的碳化工艺条件为碳化温度10℃、CO2流速0.3 L/min、晶型控制剂添加量3%,此条件下制备的样品为纯相方解石晶型纳米碳酸钙,粒径为30 nm,粒度分布均匀;相转移剂中Y3-通过络合形成的空间位阻及在CaCO3晶体表面的吸附,会影响CaCO3粒子的长大;晶型控制剂DG2可在高浓度Y3-影响下,与Ca2+螯合形成稳定的环状络合物,并通过在碳酸钙晶体表面的吸附作用,共同促进纳米碳酸钙的形成。研究成果可为工业电石渣综合利用研究提供新思路。
【Abstract】 Calcium carbide slag is a by-product generated during the production of acetylene by calcium carbide method, belonging to grade II industrial solid waste. Its main component is Ca(OH)2. The high-value, large-scale, and intensive utilization of calcium carbide slag is of great significance for resource conservation and environmental protection. This article adopts a one-step phase transfer carbonization method to prepare nano calcium carbonate from industrial carbide slag. The Ca2+ phase transfer rate is used as the evaluation index, and single factor condition experiments and orthogonal experiments are carried out. X-ray diffraction(XRD), field emission scanning electron microscopy(FE-SEM), field emission transmission electron microscopy(FE-TEM) and other methods are used to characte-rize and analyze the morphology and structure of the samples. The results show that the suitable phase transfer reaction conditions are a phase transfer agent molar ratio of 4∶3, a reaction temperature of 3 ℃, a reaction time of 20 min, and a stirring rate of 200 r/min. Under these conditions, the Ca2+phase transfer rate reach 91.97%; After screening, DG2 is determined to be a suitable crystal form control agent. The suitable carbonization process conditions are carbonization temperature of 10 ℃, CO2 flow rate of 0.3 L/min, and crystal form control agent addition of 3%. The sample prepared under these conditions is pure phase calcite crystal nano calcium carbonate with a particle size of 30 nm and uniform particle size distribution; The steric hindrance formed by the complexation of Y3- in the phase transfer agent and its adsorption on the surface of CaCO3 crystals can affect the growth of CaCO3 particles; The crystal form control agent DG2 can chelate with Ca2+to form stable cyclic complexes under the influence of high concentration Y3-, and jointly promote the formation of nano CaCO3 through adsorption on the surface of calcium carbonate crystals. The research results can provide new ideas for the comprehensive utilization of industrial carbide slag.
【Key words】 carbide slag; phase transfer agent; crystal control agent; carbonization method; nano-CaCO3; orthogonal test; conditional test; complexation reaction;
- 【文献出处】 化工矿物与加工 ,Industrial Minerals & Processing , 编辑部邮箱 ,2025年03期
- 【分类号】TQ132.32;TB383.1
- 【下载频次】53