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

作　　者：蒋国华 王百年 汪晨 杨保俊 JIANG Guohua;WANG Bainian;WANG Chen;YANG Baojun(School of Chemistry and Chemical Engineering,Hefei University of Technology,Hefei Anhui 230009,China)

机构地区：[1]合肥工业大学化学与化工学院,安徽合肥230009

出　　处：《化工矿物与加工》2025年第3期48-56,共9页Industrial Minerals & Processing

基　　金：2022年度安徽省科技重大专项(112175456041)。

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Ca^(2+)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Ca^(2+)相转移率达91.97%;经筛选确定DG_(2)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℃、CO_(2)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Y^(3-)通过络合形成的空间位阻及在CaCO_(3)晶体表面的吸附,会影响CaCO_(3)粒子的长大;晶型控制剂DG_(2)可在高浓度Y^(3-)影响下,与Ca^(2+)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。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 Ca^(2+)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 Ca^(2+)phase transfer rate reach 91.97%;After screening,DG_(2) is determined to be a suitable crystal form control agent.The suitable carbonization process conditions are carbonization temperature of 10℃,CO_(2)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 Y^(3-)in the phase transfer agent and its adsorption on the surface of CaCO_(3)crystals can affect the growth of CaCO_(3)particles;The crystal form control agent DG_(2) can chelate with Ca^(2+)to form stable cyclic complexes under the influence of high concentration Y^(3-),and jointly promote the formation of nano CaCO_(3)through adsorption on the surface of calcium carbonate crystals.The research results can provide new ideas for the comprehensive utilization of

关 键 词：电石渣 相转移剂 晶型控制剂 碳化法 纳米碳酸钙 正交试验 条件试验 络合反应 

分 类 号：TQ127.1[化学工程—无机化工]