Synthesis and Characterization of Carboxymethyl Cellulose from Eichhornia crassipes and Pennisetum purpureum as Potential Source of Sustainable Drilling Mud Additives

I. Emenike, C. Leo, M. Onojake
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Abstract

Cellulose extracted from Eichhornia crassipe (Water hyacinth) and Pennisetum purpureum (elephant grass) yielded 21.88% and 31.39% respectively. Cellulose extracted was used to synthesize carboxymethyl cellulose (CMC) under heterogeneous condition with ethanol as the supporting medium. Effect of concentration of sodium hydroxide (NaOH) on the modification of cellulose to yield CMC was investigated. It was observed that percentage CMC yield increased with increase in NaOH concentration. Comparative studies of the two biomass samples through physico-chemical analyses in terms of degree of substitution (DS), water absorption capacity, water loss, pH, conductivity and analytical characterization using SEM-EDX, FT-IR and EDXRF spectroscopy of the extracted cellulose and synthesized CMC were done. The DS of CMC obtained by alkalization reaction of cellulose from E. crassipe and P. purpureum with monochloroacetic acid was in the range of 0.54-0.75 which showed that it is highly soluble. Fourier Transform-Infrared (FT-IR) spectrophotometer showed changes of functional group from cellulose to CMC. The absorption at 3283 cm-1 and 3320 cm-1 as observed in E. crassipe and P. purpureum spectra showed OH vibration of polymeric compounds. The presence of bands at 1592 cm-1 and 1417 cm-1 in E. crassipe spectrum and bands at 1566 cm-1 and 1410 cm-1 observed in P. purpureum spectrum showed the presence of –COO group as a result of carboxymethylation reaction on cellulose during modification process. EDXRF was applied for quality control and product development due to the unavailability of the elemental composition of elephant grass and water hyacinth in the literature. The morphology and elemental compositions on the surface of the biomass were analyzed by SEM-EDX and among the chemical elements detected were C, O, Na, Mg, Al, S, Cl, K, Ca, Fe Si and Zr which confirms the elements identified with EDXRF spectroscopy. XRF spectra show high peaks at Fe, K and Sn for untreated P. purpureum samples and high peaks at Ca, Fe and Sr for untreated E. crassipe fiber. Both samples are rich in Iron (Fe). Samples were free from some toxic elements such as Pb, As, Hg, V and Ni which makes them safe for use as novel raw materials for industrial applications. Also very low concentration of Sulphur in the samples, make them safe to be considered as additives in drilling mud formulation.
石竹和狼尾草羧甲基纤维素的合成与表征
水葫芦(Eichhornia crassipe)和象草(Pennisetum purpureum)纤维素提取率分别为21.88%和31.39%。以纤维素提取物为原料,以乙醇为载体,在非均相条件下合成羧甲基纤维素(CMC)。研究了氢氧化钠(NaOH)浓度对纤维素改性产CMC的影响。结果表明,随着NaOH浓度的增加,CMC的产率增加。通过物理化学分析,对两种生物质样品在取代度(DS)、吸水量、失水量、pH值、电导率等方面进行了比较研究,并对提取的纤维素和合成的CMC进行了SEM-EDX、FT-IR和EDXRF光谱分析表征。用一氯乙酸碱化芥菜和紫花苜蓿纤维素,得到的CMC的DS在0.54 ~ 0.75之间,具有较好的可溶性。傅里叶变换红外(FT-IR)分光光度计显示纤维素到CMC的官能团变化。在3283 cm-1和3320 cm-1处观察到的紫荆和紫荆光谱的吸收显示聚合物的OH振动。E. crassipe光谱中1592 cm-1和1417 cm-1波段的存在,P. purpureum光谱中1566 cm-1和1410 cm-1波段的存在表明纤维素在改性过程中发生羧甲基化反应而存在-COO基团。由于文献中无法获得象草和水葫芦的元素组成,因此将EDXRF应用于质量控制和产品开发。利用SEM-EDX分析了生物质表面的形态和元素组成,检测到的化学元素有C、O、Na、Mg、Al、S、Cl、K、Ca、Fe、Si和Zr,与EDXRF光谱鉴定的元素一致。XRF光谱显示,未经处理的紫堇样品的Fe、K和Sn峰较高,未经处理的紫堇纤维的Ca、Fe和Sr峰较高。两个样品都富含铁(Fe)。样品中不含Pb、as、Hg、V和Ni等有毒元素,可作为新型工业原料安全使用。样品中硫的浓度也很低,可以作为钻井泥浆配方中的添加剂。
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