水热法合成超细斜发沸石试验研究  

Experimental study on hydrothermal synthesis of ultrafine clinoptilolite

作　　者：吴照洋[1,2,3,4] 郝小非 孙启亮[1,2,3,4] 张永兴 权藏玉 Wu Zhaoyang;Hao Xiaofei;Sun Qiliang;Zhang Yongxing;Quan Cangyu(Zhengzhou Institute of Multipurpose Utilization of Mineral Resources,CAGS,Zhengzhou Henan 450006,China;China National Engineering Research Center for Utilization of Industrial Minerals,Zhengzhou Henan 450006,China;Henan Provincial Engineering Technology Center for Molecular Sieve Adsorptionand Separation,Zhengzhou Henan 450006,China;Key Laboratory of Catalysis and Adsorption Materials of Zhengzhou City,Zhengzhou Henan 450006,China;Luoyang Xinling Micro Nano New Materials Co.,Ltd.,Luoyang Henan 471000,China)

机构地区：[1]中国地质科学院郑州矿产综合利用研究所,河南郑州450006 [2]国家非金属矿资源综合利用工程技术研究中心,河南郑州450006 [3]河南省分子筛吸附分离工程技术研究中心,河南郑州450006 [4]郑州市吸附催化材料重点实验室,河南郑州450006 [5]洛阳新翎微纳新材料有限公司,河南洛阳471000

出　　处：《化工矿物与加工》2024年第1期15-20,共6页Industrial Minerals & Processing

基　　金：河南省重点研发与推广专项-科技攻关项目(212102210183)。

摘　　要：斜发沸石具有较强的吸附和离子交换能力,在重金属和油污废水去除、制糖、造纸净化、抗菌抗癌药物助剂制备、石油化工催化裂化、国防以及CO_(2)脱除等领域应用广泛。为了获得纯度较高的斜发沸石,以NaOH、KOH、Al(OH)_(3)、Na_(2)O·nSiO_(2)、H_(2)O为原料,采用水热法制备了斜发沸石,并通过XRD和晶面分析,研究了斜发沸石的合成条件,结果表明:合成斜发沸石的最佳条件为n(SiO_(2))/n(Al_(2)O_(3))=11、n(OH-)/n(SiO_(2))=0.55、n(H_(2)O)/n(SiO_(2))=25~55、温度150℃、时间6 d,合成的斜发沸石呈片状结构,特征峰完整,纯度较高,其晶胞组成为Na_(0.36)K_(6.58)[(AlO_(2))6(SiO_(2))_(25.26)]·6.71H_(2)O,n(SiO_(2))/n(Al_(2)O_(3))约为8.5,属中硅铝比沸石。SEM分析结果显示,其粒径在1.3μm以下,表明粒度非常细;其静态水吸附量为34.3%,达到了HG/T 2690-2012《13X分子筛》中的一等品指标要求。研究成果可为高纯度细粒斜发沸石的精准合成提供借鉴。Clinoptilolite has strong adsorption and ion exchange capabilities,and is widely used in heavy metal and oil wastewater removal,sugar production,paper purification,preparation of anti-bacterial and anti-cancer drug additives,petrochemical catalytic cracking,national defense and CO_(2)removal.In order to obtain high-purity clinoptilolite,the clinoptilolite was prepared by hydrothermal method with NaOH,KOH,Al(OH)_(3),Na_(2)O·n SiO_(2)and H_(2)O as raw materials.The synthesis conditions of clinoptilolite were studied by XRD and crystal surface analysis.The results show that the optimum conditions for synthesis of clinoptilolite are n(SiO_(2))/n(Al_(2)O_(3))=11,n(OH-)/n(SiO_(2))=0.55,n(H_(2)O)/n(SiO_(2))=25~55,temperature 150℃,time 6 d.The synthesized clinoptilolite exhibited a sheet-like structure,complete characteristic peak and high purity.Its crystal cell composition is Na_(0.36)K_(6.58)·6.71H_(2)O,n(SiO_(2))/n(Al_(2)O_(3))about 8.5,which belongs to the middle Si-Al ratio zeolite.The SEM analysis results show that the particle size is below 1.3μm,indicating that the particle size is very fine.Its static water adsorption capacity is 34.3%,which meets the first-class requirements in HG/T 2690-2012"13X Molecular Sieve".The research results can provide reference for the precise synthesis of high-purity fine clinoptilolite.

关 键 词：斜发沸石 水热法 特征峰 硅铝比 合成条件 静态水吸附 晶面分析 

分 类 号：TQ424.25[化学工程]