硼酸锌对氧化插层法制备膨胀石墨的影响  

Effect of Zinc Borate on the Preparation of Expanded Graphite by Oxidative Intercalation Method

作　　者：陈伟[1] 王磊[1] Chen Wei;Wang Lei(Tangshan Key laboratory of Green Specialty Chemicals,Department of Chemistry,Tangshan Normal University,Tangshan,Hebei 063000)

机构地区：[1]唐山师范学院化学系,唐山市绿色专用化学品重点实验室,河北唐山063000

出　　处：《非金属矿》2022年第2期10-14,共5页Non-Metallic Mines

基　　金：河北省高等学校科学技术研究项目(Z2020241);唐山师范学院科研基金(2020C05、2022C41)。

摘　　要：采用化学氧化插层法,以天然鳞片石墨为原料,高锰酸钾为氧化剂,硝酸、磷酸和硼酸锌(ZB)为插层剂,微波膨胀制备膨胀石墨,并通过傅里叶红外光谱(FTIR)仪和场发射扫描电镜(SEM)等手段对样品进行表征。对比不同插层体系的膨胀效果,探究最佳插层体系的最佳制备条件,考察辅助插层剂硼酸锌对制备膨胀石墨的影响。结果表明,高锰酸钾-硝酸和磷酸混酸+ZB体系的膨胀效果最佳;取1 g石墨、0.3 g高锰酸钾、18 mL混酸(硝酸与磷酸的体积比为1∶2)、0.25 g硼酸锌,在40℃下搅拌反应40 min,微波膨胀30 s,膨胀石墨(EG6)膨胀体积最大,约为364 mL/g;与未加硼酸锌时膨胀石墨(EG3)相比,膨胀体积提升约40%。由FTIR分析可知,插层剂硝酸、磷酸、硼酸锌进入了石墨层间。由SEM表征结果可知,在高锰酸钾-混酸体系中,添加辅助插层剂硼酸锌,膨胀石墨的孔隙更发达,膨胀效果良好。Expanded graphite was prepared by chemical oxidation intercalation method and microwave expansion with natural flake graphite as raw material,potassium permanganate as oxidant,nitric acid,phosphoric acid and zinc borate as intercalation agent,and characterized by FTIR and SEM.The expansion effects of different intercalation systems were compared,the optimal preparation conditions of the optimal intercalation system were explored,and the effect of auxiliary intercalation agent zinc borate on the preparation of expanded graphite was investigated.The results show that the expansion effect of oxidation intercalation system with potassium permanganate as oxidant and nitric acid,phosphoric acid and ZB as intercalation agent is best;the maximum expansion volume is about 364 mL/g,when natural flake graphite is 1 g,potassium permanganate is 0.3 g,mixed acid is 18 mL,the volume ratio of nitric acid to phosphoric acid is 1∶2,zinc borate is 0.25 g,intercalation reaction is 40 min at 40℃ and microwave expansion is 30 s.the expansion volume of EG6 is about 40%higher than that without zinc borate(EG3).The FTIR results show that the intercalators such as nitric acid,phosphoric acid and zinc borate are successfully intercalated between graphite layers.The SEM results show that the expanded graphite prepared by adding the auxiliary intercalator zinc borate to the potassium permanganate-mixed acid system has more developed pores and good expansion effect.

关 键 词：化学氧化插层法 膨胀石墨 硼酸锌 硝酸 磷酸 

分 类 号：TQ569[化学工程—炸药化工]