宁东煤气化细渣固相碱熔制备单一相A型沸石

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。

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

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.