宁东煤气化细渣固相碱熔制备单一相A型沸石  

Preparation of Single Phase Zeolite A by Solid Phase Alkali Fusion Synthesis of Fine Slag From Ningdong Coal Gasification

作　　者：赵鹏德 吉文欣[1,2] 张世越 张莎莎 马玉龙[2] ZHAO Pengde;JI Wenxin;ZHANG Shiyue;ZHANG Shasha;MA Yulong(State Key Laboratory of High-Efficiency Coal Utilization and Green Chemical Engineering,Ningxia University,Yinchuan 750021,China;College of Chemistry and Chemical Engineering,Ningxia University,Yinchuan 750021,China)

机构地区：[1]宁夏大学省部共建煤炭高效利用与绿色化工国家重点实验室,宁夏银川750021 [2]宁夏大学化学化工学院,宁夏银川750021

出　　处：《石油学报（石油加工）》2020年第5期1031-1038,共8页Acta Petrolei Sinica(Petroleum Processing Section)

基　　金：国家自然科学基金项目(21663019);宁夏回族自治区重点研发计划东西部合作专项(2019BFH02014)资助。

摘　　要：以宁东煤气化细渣(CGS)为原料,采用固相碱熔方法制备单一相A型沸石,对固相碱熔过程中碱与煤气化细渣质量比(m(NaOH)/m(CGS))、固相碱熔温度、水热反应时间、水热反应温度、去离子水体积与起始反应混合物质量之比(简称液/固比,mL/g)等反应条件进行优化研究。采用X射线粉末衍射(XRD)、场发射扫描电子显微镜(SEM)、傅里叶变换红外光谱(FT-IR)、比表面积分析(BET)等原位技术对由煤气化细渣合成的A型沸石进行表征。确定了固相、绿色合成制备单一相A型沸石的最佳条件。结果表明:当m(NaOH)/m(CGS)为1.2、固相碱熔温度为823 K、水热反应温度为353 K、水热反应时间为12 h、液/固比为4.5 mL/g时,所合成的A型沸石相对结晶度最高达到93.1%,其阳离子交换能力(CEC)为268.4 mmol/100 g,BET比表面积为61.1 m2/g。Single phase type A zeolite was prepared by solid phase alkali fusion from the fine slag of Ningdong coal gasification(CGS).The optimum conditions for single phase zeolites A preparation by solid phase and green phase synthesis(e.g.,mass ratio of alkali to coal gasification fine slag(m(NaOH)/m(CGS)),solid phase alkali fusion temperature,hydrothermal reaction time and temperature,deionized water and initial reaction mixture ratio,etc.)were investigated and confirmed experimentally.Zeolite A synthesized from coal gasification fine slag was further characterized by X-ray powder diffraction(XRD),field emission scanning electron microscopy(SEM),Fourier transform infrared spectroscopy(FT-IR)and specific surface area analyzer(BET).Experimental results showed,under the conditions of m(NaOH)/m(CGS)ratio 1.2,solid phase alkali fusion temperature 823 K,hydrothermal reaction temperature 353 K,reaction time 12 h and liquid/solid ratio 5 mL/g,the synthesized zeolite A had the highest relative crystallinity 93.1%,the cation exchange capacity(CEC)268.4 mmol/100 g,and BET specific surface area 61.1 m2/g.

关 键 词：煤气化细渣 固相碱熔 单相 A型沸石 

分 类 号：O643[理学—物理化学]