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  • 黄慨,周欢,顾传君,黄绍权,黄华林,冼学权,李冬冬,黄志民.电化学法原位碳化制备纳米碳酸钙的探索[J].广西科学学院学报,2020,36(2):184-192.    [点击复制]
  • HUANG Kai,ZHOU Huan,GU Chuanjun,HUANG Shaoquan,HUANG Hualin,XIAN Xuequan,LI Dongdong,HUANG Zhimin.Exploration on the Preparation of Nano Calcium Carbonate by Electrochemical Assisted In-situ Carbonization Method[J].Journal of Guangxi Academy of Sciences,2020,36(2):184-192.   [点击复制]
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电化学法原位碳化制备纳米碳酸钙的探索
黄慨1,2, 周欢1,3, 顾传君1,2, 黄绍权2, 黄华林1, 冼学权1,2, 李冬冬4, 黄志民1,2
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(1.国家非粮生物质能源工程技术研究中心, 广西生物炼制重点实验室, 广西南宁 530007;2.广西科学院高性能新材料产业研究院, 广西南宁 530007;3.广西大学, 广西南宁 530004;4.广西北投环保水务集团有限公司, 广西南宁 530029)
摘要:
本文聚焦大理石加工行业废浆的资源化利用问题,以湿法冶金萃取工艺纯化得到的氯化钙溶液为主要原料,重点探索利用电化学原位碳化的方法从氯化钙制备纳米碳酸钙,实现从固废转变成高端钙基材料的目标。研究采用电化学法+原位碳化反应的制备方法,创造适合环境,使得氯化钙与二氧化碳直接发生碳化反应。通过调控直流电压、反应温度、反应时间、晶型控制剂添加量(柠檬酸)和CO2通气速率等影响因素,研究其对生成碳酸钙形貌和粒径的影响。采用X衍射光谱(XRD)、场发射扫描电镜(FESEM)、透射电镜(TEM)分别对碳酸钙形貌、粒径及比表面积进行表征。实验结果表明,电化学原位碳化反应的较佳工艺条件为直流电压12 V、反应温度20℃、反应时间3 h、柠檬酸添加量5 mmol/L、CO2通气速率30 mL/min。该条件下可得到链状纳米碳酸钙,直径30 nm,长径比(L/D)约8。利用电化学法原位碳化氯化钙可制备获得链状纳米碳酸钙,不需要外加碱,其碳化过程可表述为电化学复分解反应。
关键词:  电化学辅助法  原位碳化  纳米碳酸钙  氯化钙  二氧化碳
DOI:10.13657/j.cnki.gxkxyxb.20200603.004
基金项目:广西创新驱动发展专项资金项目(桂科AA17202030-2、桂科AA18242006-3),广西技术创新引导项目(桂科AC17292008),贺州市创新驱动重大项目(贺科创ZX1807002)和广西科技攻关项目(桂科攻1598007-7)资助。
Exploration on the Preparation of Nano Calcium Carbonate by Electrochemical Assisted In-situ Carbonization Method
HUANG Kai1,2, ZHOU Huan1,3, GU Chuanjun1,2, HUANG Shaoquan2, HUANG Hualin1, XIAN Xuequan1,2, LI Dongdong4, HUANG Zhimin1,2
(1.National Engineering Research Center for Non-food Biorefinery, Guangxi Key Laboratory of Biorefinery, Nanning, Guangxi, 530007, China;2.Advanced Materials Industry Institute of Guangxi Academy of Sciences, Guangxi Academy of Sciences, Nanning, Guangxi, 530007, China;3.Guangxi University, Nanning, Guangxi, 530004, China;4.Guangxi Beitou Environment&Water Group Co., Ltd., Nanning, Guangxi, 530029)
Abstract:
This article focuses on the resource utilization of waste slurry in marble processing industry,and tries to take the calcium chloride solution purified by hydrometallurgy extraction process as the main raw material.The electrochemical in-situ carbonization method is mainly explored to prepare nano calcium carbonate from calcium chloride,so as to realize the goal of transforming solid waste into high-end calcium based materials.The preparation method of electrochemical assistance + in-situ carbonization was used to create a suitable environment for the direct carbonization of calcium chloride and carbon dioxide.By adjusting the DC voltage,reaction temperature,reaction time,the amount of crystalline control agent added (citric acid) and CO2 aeration rate and other influencing factors,the influence on the morphology and particle size of calcium carbonate were studied.The morphology,particle size and specific surface area of calcium carbonate were characterized by X-ray Diffraction (XRD),Field Emission Scanning Electron Microscopy (FESEM) and Transmission Electron Microscopy (TEM),respectively.The experimental results show that the preferred process conditions for electrochemical assisted in-situ carbonization are DC voltage 12 V,reaction temperature 20℃,reaction time 3 h,citric acid addition 5 mmol/L,and CO2 ventilation rate 30 mL/min.Under this condition,a chain-shaped nano calcium carbonate with a diameter of 30 nm and L/D ratio of about 8 can be obtained.The chain like nano calcium carbonate was prepared by in-situ carbonation of calcium chloride with electrochemical assistant method,without adding alkali.The carbonization process can be expressed as electrochemical metathesis reaction.
Key words:  electrochemical assisted method  in-situ carbonization  nano calcium carbonate  calcium chloride  carbon dioxide

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