Transactions of Nonferrous Metals Society of China The Chinese Journal of Nonferrous Metals

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中国有色金属学报

ZHONGGUO YOUSEJINSHU XUEBAO

第29卷    第8期    总第245期    2019年8月

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文章编号:1004-0609(2019)-08-1790-11
以锡矿尾矿为原料ZSM-5分子筛的水热合成
张鹏举,黄太铭,何华杰,韦夏夏,赵梦梦,阮 乐,唐富顺

(桂林理工大学 化学与生物工程学院,广西有色金属隐伏矿床勘查及材料开发协同创新中心,桂林 541004)

摘 要: 以有色金属锡矿尾矿为原料、通过乙醇的绿色导向法水热合成ZSM-5分子筛,并以XRD、SEM、FT-IR、XRF、ICP等多种物理化学表征手段对晶种、体系pH、晶化温度、晶化时间及醇添加剂等对合成产物的影响因素进行系统考察。结果表明:以有色金属锡矿尾矿为原料,采用绿色水热合成导向法,可以合成出高结晶度、具有规整八面体外形及良好热稳定性能的ZSM-5产物;合成体系中乙醇和晶种均可有效加速晶体晶化速率,但乙醇不具结构导向作用;体系pH对产物的生成速度及纯度具有决定性作用,过高晶化温度及较长晶化时间容易导致产物中杂晶相的出现,体系中乙醇和正丁醇对ZSM-5的相对结晶度及外貌形状影响不大。添加的晶种量为合成体系中SiO2投料量的0.62%(摩尔分数),醇的添加量与合成体系中SiO2投料量摩尔比为0.50,合成体系pH为10.8,170 ℃及24 h晶化条件下,可获得高结晶度及收率的ZSM-5产物。

 

关键字: 锡矿尾矿;资源化;ZSM-5;绿色合成;乙醇

Hydrothermal synthesis of ZSM-5 using tin ore tailing as raw material
ZHANG Peng-ju, HUANG Tai-ming, HE Hua-jie, WEI Xia-xia, ZHAO Meng-meng, RUAN Le, TANG Fu-shun

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

ISSN 1004-0609
CN 43-1238/TG
CODEN: ZYJXFK

ISSN 1003-6326
CN 43-1239/TG
CODEN: TNMCEW

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