电石渣浸取液制备超细CaCO_3的碳化工艺研究
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摘要
以NH_4Cl溶液浸取电石渣得到的Ca~(2+)溶液为钙源,以Na_2CO_3为碳化剂,制备超细CaCO_3。研究了Ca~(2+)浓度、碳化剂的滴加速度、反应温度、反应时间、pH、[CO32-]/[Ca~(2+)]摩尔比对CaCO_3产率的影响。结果表明,在Ca~(2+)浓度0.3 mol/L,Na_2CO_3滴速30 mL/min,温度40℃,反应时间30 min,Ca~(2+)溶液的pH为9,[CO32-]/[Ca~(2+)]摩尔比1.1的条件下,CaCO_3产率92.07%,纯度97.35%。经X射线衍射和扫描电镜分析,合成的CaCO_3以方解石型为主,并含有部分球霰石型。方解石型含量为62.85%,颗粒为表面光滑致密的立方体结构,粒径为4～9μm,平均晶粒尺寸60 nm;球霰石型含量为37.15%,颗粒为表面不圆滑的球形结构,粒径3～8μm,平均晶粒尺寸28 nm。
Preparation of CaCO_3 with carbide slag leached by NH_4Cl as Ca~(2+)resources and Na_2CO_3 as carbonation agent was studied.Effect of the concentration of Ca~(2+)aqueous,the dropping speed of Na_2CO_3,the reaction temperature and reaction time,the pH of the solution and the mol ratio of[CO32-]/[Ca~(2+)]on the yield of CaCO_3 were investigated.The results show that the yield of CaCO_3 was 92.07%with a purity of 97.35% under the optimized conditions in which the concentration of Ca~(2+)aqueous was 0.3 mol/L;the dropping speed of Na_2CO_3 was 30 mL/min;the reaction temperature was 40 ℃ and the reaction time was 30 min;the pH of the solution was 9 and the mol ratio of[CO23-]/[Ca~(2+)] was1.1.XRD pattern and SEM images revealed that both calcite and vaterite CaCO_3 were obtained simultaneously.Calcite was the major phase with a content of 62.85%.The calcite particle was cubic with smooth and density surface.The particle size of calcite was 4～9 μm,and the crystal size was 60 nm.Vaterite was the minor phase with a content of 37.15%.The vaterite particle was ball-shaped with unsmooth surface.The particle size of vaterite was 3～8 μm,and the crystal size was 28 nm.
Preparation of CaCO_3 with carbide slag leached by NH_4Cl as Ca~(2+)resources and Na_2CO_3 as carbonation agent was studied.Effect of the concentration of Ca~(2+)aqueous,the dropping speed of Na_2CO_3,the reaction temperature and reaction time,the pH of the solution and the mol ratio of[CO32-]/[Ca~(2+)]on the yield of CaCO_3 were investigated.The results show that the yield of CaCO_3 was 92.07%with a purity of 97.35% under the optimized conditions in which the concentration of Ca~(2+)aqueous was 0.3 mol/L;the dropping speed of Na_2CO_3 was 30 mL/min;the reaction temperature was 40 ℃ and the reaction time was 30 min;the pH of the solution was 9 and the mol ratio of[CO23-]/[Ca~(2+)] was1.1.XRD pattern and SEM images revealed that both calcite and vaterite CaCO_3 were obtained simultaneously.Calcite was the major phase with a content of 62.85%.The calcite particle was cubic with smooth and density surface.The particle size of calcite was 4～9 μm,and the crystal size was 60 nm.Vaterite was the minor phase with a content of 37.15%.The vaterite particle was ball-shaped with unsmooth surface.The particle size of vaterite was 3～8 μm,and the crystal size was 28 nm.
引文
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[2]蒋明,黄小凤,刘红盼,等.电石渣资源化应用研究进展[J].硅酸盐通报,2016,35(12):4025-4031.
[3]Sun J,Liu W Q,Hu Y C,et al.Enhanced performance of extruded-spheronized carbide slag pellets for high temperature CO2capture[J].Chemical Engineering Journal,2016,285:293-303.
[4]蒋明,刘红盼,黄小凤.电石渣在环境污染控制中的应用[J].无机盐工业,2017,49(3):6-8.
[5]郭琳琳,范小振,张文育,等.电石渣制备高附加值碳酸钙的研究进展[J].化工进展,2017,36(1):364-371.
[6]郭琳琳,徐美,刘博静,等.氯化铵浸取电石渣制备碳酸钙研究[J].应用化工,2017,46(9):1757-1760.
[7]Weimarn P P V.The precipitation laws[J].Chemical Reviews,2002,2(2):217-242.
[8]李永新,方宾.作图法求算碳酸钙水溶液的溶解度及p H值[J].安徽师范大学学报:自然科学版,1999,22(1):84-85.
[9]Kontoyannis C G,Vagenas N V.Calcium carbonate phase analysis using XRD and FT-Raman spectroscopy[J].Analyst,2000,125(2):251-255.
[10]王芬,余军霞,肖春桥,等.CO2碳化法制备微米级球霰石型食品碳酸钙的研究[J].硅酸盐通报,2017,36(1):43-50.