(桂林理工大學(xué) 化學(xué)與生物工程學(xué)院，廣西有色金屬隱伏礦床勘查及材料開(kāi)發(fā)協(xié)同創(chuàng)新中心，桂林 541004)
摘 要: 以有色金屬錫礦尾礦為原料、通過(guò)乙醇的綠色導(dǎo)向法水熱合成ZSM-5分子篩，并以XRD、SEM、FT-IR、XRF、ICP等多種物理化學(xué)表征手段對(duì)晶種、體系pH、晶化溫度、晶化時(shí)間及醇添加劑等對(duì)合成產(chǎn)物的影響因素進(jìn)行系統(tǒng)考察。結(jié)果表明：以有色金屬錫礦尾礦為原料，采用綠色水熱合成導(dǎo)向法，可以合成出高結(jié)晶度、具有規(guī)整八面體外形及良好熱穩(wěn)定性能的ZSM-5產(chǎn)物；合成體系中乙醇和晶種均可有效加速晶體晶化速率，但乙醇不具結(jié)構(gòu)導(dǎo)向作用；體系pH對(duì)產(chǎn)物的生成速度及純度具有決定性作用，過(guò)高晶化溫度及較長(zhǎng)晶化時(shí)間容易導(dǎo)致產(chǎn)物中雜晶相的出現(xiàn)，體系中乙醇和正丁醇對(duì)ZSM-5的相對(duì)結(jié)晶度及外貌形狀影響不大。添加的晶種量為合成體系中SiO2投料量的0.62%(摩爾分?jǐn)?shù))，醇的添加量與合成體系中SiO2投料量摩爾比為0.50，合成體系pH為10.8，170 ℃及24 h晶化條件下，可獲得高結(jié)晶度及收率的ZSM-5產(chǎn)物。
關(guān)鍵字: 錫礦尾礦；資源化；ZSM-5；綠色合成；乙醇
（College of Chemistry and Bioengineering, Guilin University of Technology, Collaborative Innovation Center for Exploration of Hidden Nonferrous Metal Deposits and Development of New Materials in Guangxi, Guilin 541004, China）
Abstract:The ZSM-5 zeolite was hydrothermally synthesized using non-ferrous metal tin ore tailings as raw material through ethanol green oriented method, and the influences of seed, synthesis pH, crystallization temperature, crystallization time and alcohol additives, etc. on synthetic product were investigated systematically by various physical and chemical methods, such as XRD, SEM, FT-IR, XRF, ICP, etc. The results show that the ZSM-5 products with high crystallinity, regular octahedron shape and good thermal stability can be hydrothermally synthesized from non-ferrous metal tin ore tailings by using ethanol green oriented method. In the synthesis system, both ethanol and crystal species can effectively accelerate the crystallization rate of crystals, but ethanol has no structural guidance. System pH plays a decisive role in the generating rate and purity of product. Higher crystallization temperature and longer crystallization time may lead to the appearance of heterocrystalline phase in the product. Ethanol and n-butyl alcohol in the system have little influence on the relative crystallinity and morphology of ZSM-5. High crystallinity and yield of ZSM-5 product can be obtained under the conditions of seed dosage n(seed)/n(SiO2)feed=0.62%, n(alcohol)/n(SiO2)feed=0.50, pH=10.8, crystallization temperature of 170 ℃ and time of 24 h, respectively.
Key words: tin ore tailings; recycling; ZSM-5; green synthesis; ethanol
