Synthesis Of Carboxymethyl Cellulose Research Articles

Extraction of Lignocellulose from Rice Straw and Its Carboxymethylation When Activated by Microwave Radiation.

The paper presents the process of cellulose extraction from rice straw using water-alkaline solution treatment and the subsequent process of carboxymethylation of the obtained product when activated by microwave radiation. After mercerization of rice straw, the obtained product contained 89.2% cellulose and 6.7% lignin. The X-ray diffraction pattern of the obtained lignocellulose shows three diffraction peaks in the region typical for the polymorphic modification of cellulose Iβ (2θ = 15.50(78), 21.70(145), 34.70(52)). The degree of crystallinity was 65%. The product was heat-stable up to 247 °C. The synthesis of carboxymethylcellulose (CMC) based on the obtained product included successive processes of thermostating in alcohol-alkali solution and cellulose esterification reaction using monochloroacetic acid. To activate the carboxymethylation process, microwave radiation was used (350 W for 90 s), which made it possible to reduce the reaction time by more than 100 times. Functional group analysis of the carboxylated lignocellulose from rice straw was carried out using an FTIR spectrometer. In the IR spectra, a band with a maximum of 1742 cm-1 was recorded, corresponding to stretching vibrations of >C(O)OH groups. The degree of polymerization was recorded by mass spectrometry.

Nipah Frond Waste as a Renewable Source for Carboxymethyl Cellulose

Nipah frond is one of the wastes that has not been widely utilized by community. Nipah frond contain a relatively high cellulose content that can be used as renewable source for carboxymethyl cellulose production. This research focus on the extraction of cellulose from nipah fronds, followed by synthesis of carboxymethyl cellulose through alkalization and carboxymethylation processes. In the process of the synthesis carboxymethyl cellulose, cellulose was carried out by alkalization and carboxymethylation using sodium hydroxie (NaOH), and trichloroacetic acid. Characterization of carboxymethyl cellulose (CMC) was carried out by Fourier Transform Infrared (FTIR). The degree of substitution (DS) was determined using the rasio of -OH and ether absorption. The effect of various concentrations of trichloroacetic acid on the DS of CMC was analyzed. DS of CMC obtained through variations in trichloroacetic acid concentration shows a decreasing trend in DS value due to the formation of by-product that inhibit the carboxymethylation. The maximum DS of 0.92 was obtained when the carboxymethylation process with 15% of trichloroacetic acid. The result of the analysis using FT-IR spectrophotometer showed there is a stretching O-H group at the wave number of 3333 cm-1, and supported with the ether vibration in the 1024 cm-1 and the presence of the carbonyl group COO- at 1601 cm-1.

Ultrasonic-assisted synthesis for the production of green and sustainable hemp carboxymethyl cellulose

Hemp fiber (Cannabis sativa) is being widely used to produce carboxymethyl cellulose (CMC). This study focused on synthesizing carboxymethyl cellulose from bleached hemp fiber to investigate the impact of different factors, i.e., chemical concentration and synthesis time, on its characteristics. The fiber morphology analysis revealed desirable properties, which are essential for high-quality CMC production. Optimal condition for CMC synthesis were investigated, which involved using 20 % NaOH (w/v), the shortest total synthesis time (2.30h), and using 0.9 g MCA (w/w). This resulted in a non-significantly high DS (0.80) in both nonspray-dried and spray-dried hemp carboxymethyl cellulose, representing a high CMC content around 96 %. Moreover, the use of ultrasonic assistance and spray drying techniques significantly improved the hemp carboxymethyl cellulose properties, indicating a decreased molecular weight (2.65 × 104 g/mol) and a decreased particle size (7.82 μm). Thermal analysis revealed that spray-dried hemp carboxymethyl cellulose had lower thermal stability than hemp fiber and nonspray-dried hemp carboxymethyl cellulose. FTIR and 13C NMR analyses confirmed the successful CMC synthesis. Additionally, XRD and SEM analyses demonstrated changes in the crystalline structure and hemp carboxymethyl cellulose surface morphology. This revealed advanced techniques that could enhance hemp carboxymethyl cellulose quality and properties, making it suitable for various industrial applications.

Optimization of synthesis method for carboxymethylcellulose (CMC) from agro-food wastes by response surface methodology (RSM) using D-Optimal algorithm

Carboxymethylcellulose (CMC) has wide commercial applicability for oil drilling fluids, cosmetics, food, and pharmaceutical industries, but the current industrial process for its synthesis from eucalyptus wood has low sustainability and efficiency. This work reports the statistical optimization for the synthesis of CMC from waste biomass celluloses with special reactivity, extracted from sugarcane bagasse (SB) and corn cob (CC). The combined mild acid/peroxide-alkali (APA) treatment, followed by bleaching, was efficient for the extraction of low-crystallinity pulps, which were further converted into CMC. A set of carboxymethylation tests with variable reaction conditions determined by a D-Optimal design of experiments (DoE) were carried out by assessing the factors Activation Time (AT), Reaction Time (RT), NaOH concentration (NaOH%) and Cellulose (SBCel or CCel). Characteristic CMC absorption features were observed via FTIR and Raman spectra, and the deconvolution of X-ray diffractograms showed that the mild APA treatment is able to produce pulps with significant content of amorphous and type II celluloses, whose have higher reactivity and reflects in the optimal results of the DoE. Analysis of variance (ANOVA) and response surface methodology (RSM) results from DoE data proved with high precision (F=184.81; p-value<0.0001; R2=0.9911; SD<1.0×10–5) and accuracy (low regression residuals) that the waste celluloses extracted are promising to produce CMC under milder conditions in comparison to literature, yielding up to 227 % (w CMC/w cellulose) of water-soluble CMC at lower AT and RT. The optimized process is more sustainable, low-cost, and efficient for producing this high valued-added cellulose derivative in the concept of biorefinery.

Facile synthesis of carboxymethyl cellulose from Indonesia's coconut fiber cellulose for bioplastics applications

AbstractCoconut fibers contain many lignocellulosic components; therefore, they have the potential to be used as cellulose‐based materials. This study aims to synthesize carboxymethyl cellulose (CMC) for bioplastic applications from coconut fiber cellulose obtained from South Tangerang, Indonesia. The isolation of cellulose was conducted in two key stages: alkaline treatment using a delignification reactor and bleaching with hydrogen peroxide (H2O2). The facile synthesis of CMC involved two important steps: alkaline treatment and carboxymethylation of isolated cellulose. The yield of cellulose isolated from coconut fiber was 16.39% for biomass and 64.84% for delignification products. The cellulose produced exhibited a crystallinity index (C.I.) of 89%. The yield of CMC was 14.67%, with a C.I. was 56.66%. The CMC obtained was categorized as having a medium molecular weight of 249,048 Da with a polymerization degree of 1046. Cellulose starts to decompose at a temperature interval of 292.05–381.45°C, whereas CMC decomposes at a lower temperature interval of 245.42–299.73°C. Thermochemical calculations were conducted by using the density functional theory (DFT), confirming a spontaneous reaction with a Gibbs free energy of −5.25 kJ mol−1. Bioplastics were fabricated in two stages: blending with carboxymethyl chitosan (CMChi) and plasticizing with glycerol. The addition of CMCh increased the C.I. and tensile strength, while the addition of glycerol to CMC/CMChi (80/20) blend‐based bioplastic reduced the C.I. and tensile strength, but enhanced the relative contact angle.Highlights Cellulose was isolated from coconut fibers through a two‐stage process involving delignification and bleaching; Carboxymethyl cellulose was synthesized by reacting the cellulose of coconut fibers with monochloroacetic acid in isopropanol with NaOH as the catayst; The optimum condition for achieving the highest elongation at break among the blending compositions was found in the CMC/CMChi (80/20) blend bioplastic; Adding up to 30 wt% glycerol decreased the tensile strength and increased the elongation at break; The addition of glycerol enhanced the hydrophobic properties of CMC/CMCh blend‐based bioplastics.

Synthesis of Carboxymethyl Cellulose from Mangrove Nipah (Nypa fruticans) as Vitamin C Coating for Drug Delivery System

Vitamin C is one of the substances needed by the human body which acts as an antioxidant that effectively overcomes the effects of free radicals that damage cells in the body, but vitamin C has properties that are easily oxidized so that innovation is needed to coat (encapsulate) vitamin C in the form of capsules as a drug delivery system. One polymer that can be used for vitamin C encapsulation is cellulose. The cellulose content can be found in the skin and nipah fruit and then synthesized into carboxymethyl cellulose as a vitamin C coating. The microencapsulation method was carried out by mixing 3 g of carrageenan-CMC mixture with variations in the ratio of 1:0; 1:0.5 and 1:1 (%b/b). The encapsulated small beads were made in 200 mL of 2M KCl-CaCl solution by extrusion technique. The microencapsulant was then drained and continued with the crosslinking stage using Glutaraldehyde (GA) 1%. In this in vitro oral simulation study, the encapsulation ratio that produced the best treatment with the highest percentage of drug solubility in the intestine was the ratio (1:0.5), followed by (1:1) and the smallest (1:0) with percentage values of 15.42; 14.06; and 1.67 percent, respectively.

Synthesis of carboxymethyl cellulose from coconut fibers and its application as solid polymer electrolyte membranes

AbstractCarboxymethyl cellulose (CMC) is one of the important cellulose derivatives, and it can be developed as a host polymer for solid polymer electrolyte (SPE) membrane. This study aimed to synthesis of CMC from coconut fiber cellulose and it was applied to prepare the SPE membranes. Cellulose isolation was conducted through the delignification and bleaching process, while the CMC synthesis was conducted through alkalization and carboxymethylation treatments. SPE membranes were prepared by blending CMC with carboxymethyl chitosan (CMCh) (80/20) and mixed with various weight percentages of LiOAc at room temperature. SPE membranes characterizations were conducted using FTIR, EIS, XRD, SEM, and tensile testing. Cellulose and CMC yields were 23.1% and 65.44%, respectively. Incorporating 20 wt% LiOAc into the CMC/CMCh (80/20) SPE membrane yielded the highest ionic conductivity of 1.37 × 10−3 S/cm. Based on the results, CMC obtained from coconut fibers has the potential to produce solid polymer electrolyte membranes with some modification.

Synthesis of carboxymethyl cellulose using bacterial cellulose produced by kombucha scoby (symbiotic culture of bacteria and yeast) using three different solvents

RESUMO A carboximetilcelulose de sódio (CMC) é um sal celulósico obtido por meio da alcalinização da celulose e posterior eterificação do álcali celulósico com excesso de solvente orgânico. A CMC é utilizada como agente espessante, umectante, aglutinante, entre outros. Comumente ela é sintetizada a partir da celulose vegetal ou também a partir de celulose bacteriana (CB). O objetivo deste estudo foi sintetizar a CMC utilizando CB produzida pelo scoby de kombucha, para valorizar esse resíduo, utilizando 3 diferentes solventes orgânicos, isopropanol, butan-1-ol e pentan-1-ol. Após a síntese, as CMCs foram caraterizadas por rendimento, teor de umidade, grau de substituição (GS), pH, viscosidade, espectroscopia no infravermelho com transformada de Fourier (FTIR), difratometria de raios-x (DRX), termogravimetria e termogravimetria derivada (TG/DTG). Os resultados comprovaram a síntese das CMCs e apresentaram diminuição da temperatura de degradação e da cristalinidade em comparação à CB pura. Por fim, a CMC produzida com isopropanol obteve melhores resultados em comparação à literatura, apresentado maior rendimento (197,62%), maior grau de substituição (0,26 ± 0,05), maior viscosidade (11,33 ± 0,48 cP) e menor cristalinidade (32,45%). No entanto, é necessário um estudo utilizando um número maior de amostras para que se obtenha resultados mais precisos acerca do melhor solvente.

Synthesis and Characterization of Carboxymethyl Cellulose (CMC) from Palm Leaf Fronds (Borassus Flabellifer)

Palm frond fibers are one of the wastes that are underutilized by society and have a cellulose content of 54.27% so they have the potential to be made into carboxymethyl cellulose (CMC). This research was conducted to determine the process of synthesizing CMC from palm frond fibers and the characteristics of CMC from palm frond fibers. The methods used in this research are synthesis and characterization. The CMC synthesis process consists of alkalization and carboxymethylation processes. Characteristics of palm frond fiber CMC include yield, color, pH and FITR test. The results showed that the CMC characteristics of palm leaf fiber produced a yield of 90%, pH 6.83 and a grayish white color. FTIR CMC results from palm leaf fiber show the -OH group in the absorption area of 3331.36 cm-1, C-H in the absorption area of 2891.5 cm-1, and the -COC- group in the absorption area of 1000-1300 cm-1. Keywords: Palm Frond Fiber, Carboxymethyl Cellulose (CMC), Cellulose, Color

Synthesis and characterization of carboxymethyl cellulose from pine needles for biomedical and regenerative medicine applications

______________________________________________________________________________________Carboxymethyl cellulose (CMC) is one of the most widely used components of hydrogel for biomedical applications as its precursor cellulose is the most abundant biological macromolecule on the Earth. Recent years have seen a remarkable increase in CMC synthesis from various plant sources. In the present study we have utilised cheer pine needles (Pinus spp.) due to its abundance and easy availability in Himalayan regions across India. The cellulose was extracted from pine needles. Then, the etherification process was used to prepare CMC from pine needle cellulose, with sodium hydroxide and monochloroacetic acid (MCA). CMC yield, degree of substitution, water retention capacity, oil retention capacity, ash content, and CMC content were determined by comparing obtained CMC to standard CMC. The purity of the synthesised CMC is represented by CMC content. The prepared CMC had a purity of 10 % and a yield of 110 %. The degree of substitution, water retention capacity, and oil retention capacity were all determined to be 0.02, 8.4 g/g, and 4g/g, respectively. The ash content of the synthesised CMC was calculated to be 6 %. The majority of characteristics were either equivalent to commercial CMC or superior to it therefore the synthesised product can be used as a potential component to fabricate biomaterials for biomedical applications.

Study on synthesis of carboxymethyl cellulose from pineapple leaf waste and its potential applications as a thickener

In this study, cellulose and hemicellulose were successfully extracted from pineapple leaf waste at yields of 58.8 and 16.1% by dried weight, respectively. Carboxymethyl cellulose (CMC) was synthesised from pineapple leaf cellulose by an esterification process using sodium hydroxide (NaOH) and monochloroacetic acid (MCA) with isopropanol as the supporting medium. Preparation of CMC was investigated by varying three free factors, namely, NaOH concentration, MCA dose, and cellulose size. The carboxymethylation process was optimised to produce CMC with differing degrees of substitution (DS). The highest DS of CMC (0.86) was obtained with 15% (w/v) NaOH solution, 0.6 g of MCA/g cellulose, and 50 μm cellulose. The obtained CMC were characterised by FTIR spectroscopy, SEM images and XRD diffractions. Moreover, the thickening performance of obtained CMC was also determined. The influence of the CMC’s molecular weight and degree of substitution on the viscosity of 1% (w/v) aqueous solution was tested. The experimental results suggest that the viscosity of the solution increases with increasing molecular weight and degree of substitution of CMC.

Synthesis of carboxymethyl cellulose (CMC) from delignified Dyera Costulata

Synthesis of carboxymethyl cellulose (CMC) from delignified Dyera Costulata

Facile and Green Synthesis of Carboxy Methyl Cellulose Stabilized Bio-Functionalized Gold Nanoparticles and Its Catalytic Activity

Gold nanoparticles (AuNP’s)are synthesized in sustainable green method using Carboxy Methyl Cellulose (CMC) and employed as catalyst in the reduction of p-nitro aniline with NaBH4 to p-phenylene diamine. It is observed that the speed of reaction was fast due to their size, as particle size decreases surface area increases. It is also observed that the rate of reaction is fast with comparison with the other catalyst. This is because the nanoparticles have more effective surface area and posses less steric hindrance with p-nitro aniline and NaBH4 when compared to nanoparticles due to their shape. The recyclability of nanoparticles shows it is potential recyclable catalyst for industrial applications.

Study of the kinetics of carboxymethyl cellulose synthesis in a screw reactor

The object of research is the reactor for the synthesis of carboxymethyl cellulose. An important indicator of the quality of sodium carboxymethyl cellulose, which determines the field of its application, is the degree of polymerization. However, obtaining a product with a specific parameter under industrial conditions is associated with a number of difficulties. Therefore, important research tasks are the development of a mathematical model of the kinetics of carboxymethyl cellulose synthesis, experimental studies to determine the rate constants of synthesis reactions, modeling of a screw reactor for the synthesis of carboxymethyl cellulose, and computer studies. When studying the kinetics of reactions of carboxymethyl cellulose, one of the possible approaches was to use a quasi-homogeneous model, which is widely used in modeling processes on a catalyst grain. This approach is used to describe and analyze individual stages; however, a number of difficulties arise in heterogeneous reactions of cellulose. In the course of these reactions, the properties of the solid phase change and the processes, respectively, are unsteady in time. The reaction does not take place on the surface of hard particles, but in the entire volume of the fibers. The concentration and reactivity of cellulose hydroxides, water, and products formed during the reaction remain approximately constant; therefore, the use of a quasi-homogeneous model is quite acceptable and does not cause additional mathematical difficulties. As a result of these experiments, according to the obtained integral curves, the method of least squares was used to find the constants. To determine the values of the kinetic constants, an experiment was carried out in an integral isothermal reactor. During the experiments, the degree of substitution of carboxymethyl cellulose and the concentration of free alkali were measured. As a result of numerous implementations of the search task, the values of the constants and activation energies were obtained. This kinetic modeling approach can be used in the synthesis of other cellulose ethers. The rate constant of the synthesis reaction depends on the process conditions. Using the proposed approach to describing the interaction of cellulose with a reagent, the reaction mixture considered as a quasi-homogeneous system can be described using a single-phase flow model.

Synthesis of carboxymethylcellulose from corn straw waste: comparison between pre-treatments with sodium hydroxide and low-cost ionic liquid

Synthesis of carboxymethylcellulose from corn straw waste: comparison between pre-treatments with sodium hydroxide and low-cost ionic liquid

CARBOXYMETHYL CELLULOSE SYNTHESIS FROM TREATED OIL PALM EMPTY FRUIT BUNCH USING IONIC LIQUID AND HYDROGEN PEROXIDE

The synthesis of carboxymethyl cellulose (CMC) generally uses isolated crude cellulose with alkaline or acid pretreatment followed by bleaching with sodium chlorite. In this study, the simple [BMIM][Cl] ionic liquid was used as a solvent in the pretreatment process before conduct the bleaching process with hydrogen peroxide (H2O2) to isolate cellulose from empty fruit bunch (EFB) for further synthesis of CMC. The isolated crude EFB cellulose obtained was converted to CMC by adding 30 wt.% NaOH and various concentrations of sodium monochloroacetic acid (SMCA) at 55 °C for 3 h. The effects of SMCA concentration on the degree of substitution (DS) and CMC yield were investigated. The physicochemical properties of the CMC products were characterized using proton nuclear magnetic resonance, scanning electron microscope-energy dispersive spectrometry, X-ray diffraction, and thermogravimetric analysis. Based on the results, CMC was demonstrated to be synthesized using ionic liquid pretreatment with H2O2 bleaching. Carboxymethyl cellulose synthesized in this study showed a high DS of 0.82. The CMC synthesized from EFB cellulose through ionic liquid pretreatment presented good chemical and physical properties as that reported in other studies.

Optimization of synthesis conditions for carboxymethyl cellulose from pineapple leaf waste using microwave-assisted heating and its application as a food thickener

Pineapple leaf waste, with its high cellulose content, can serve as alternative starting material for the production of carboxymethyl cellulose (CMC). In this study, synthesis conditions of CMC from pineapple leaves via the use of microwave heating were optimized. Box-Behnken design and response surface methodology were applied to schedule the experiments and to optimize the synthesis condition, respectively. Preparation of CMC was investigated by varying three factors, namely, sodium hydroxide (NaOH) concentration, monochloroacetic acid (MCA) dose, and etherification time. The process of carboxymethylation was optimized to produce CMC with high degree of substitution (DS). Optimal condition for CMC synthesis was noted to be 50% (w/v) NaOH solution, 8 g of MCA/g cellulose, and etherification time of 16 min; such optimal condition resulted in the maximum DS of 0.78. Synthesized CMC was utilized as a thickener for liquid foods (water, orange juice, milk, and mushroom cream soup) where 2% (w/v) as-synthesized CMC increased the viscosity of the foods and changed their characteristics from thin to nectar-like liquids.

Optimization of synthesis conditions for carboxymethyl cellulose from pineapple leaf waste using microwave-assisted heating and its application as a food thickener

Pineapple leaf waste, with its high cellulose content, can serve as alternative starting material for the production of carboxymethyl cellulose (CMC). In this study, synthesis conditions of CMC from pineapple leaves via the use of microwave heating were optimized. Box-Behnken design and response surface methodology were applied to schedule the experiments and to optimize the synthesis condition, respectively. Preparation of CMC was investigated by varying three factors, namely, sodium hydroxide (NaOH) concentration, monochloroacetic acid (MCA) dose, and etherification time. The process of carboxymethylation was optimized to produce CMC with high degree of substitution (DS). Optimal condition for CMC synthesis was noted to be 50% (w/v) NaOH solution, 8 g of MCA/g cellulose, and etherification time of 16 min; such optimal condition resulted in the maximum DS of 0.78. Synthesized CMC was utilized as a thickener for liquid foods (water, orange juice, milk, and mushroom cream soup) where 2% (w/v) as-synthesized CMC increased the viscosity of the foods and changed their characteristics from thin to nectar-like liquids.

Pemanfaatan Selulosa dari Rumput Gajah (Pennisetum purpureum) pada Sintesis Karboksimetil Selulosa (CMC)

Cellulose from Pennisetum purpureum has been used as the main ingredient in the synthesis of carboxymethyl cellulose (CMC). The purpose of CMC synthesis from the cellulose of Pennisetum purpureum is to obtain CMC compounds with the best degree of substitution (DS) value and the highest yield. The study was conducted using a completely randomized design with a factorial pattern consisting of two independent variables, namely the concentration of trichloroacetic acid (10%, 20%, and 30%) and reaction time (3 and 4 hours). The results showed that the CMC with the highest DS value (0.839) was obtained using 20% trichloroacetic acid with a reaction time of 3 hours. The highest CMC yield was 30.15% which was obtained using 30% trichloroacetic acid with a reaction time of 4 hours.&#x0D; Keywords: Pennisetum purpureum, carboxymethyl cellulose, substitution degree.

Carboxymethyl cellulose synthesis from durian seed flour: The effect of sodium chloroacetate variation

Carboxymethyl Cellulose (CMC) is cellulose derivate that is soluble in water, CMC is synthesized by reacting cellulose with sodium hydroxide and chloroacetate acid or its salt. This study purpose is to see the effect of sodium chloroacetate salt in carboxymethylation reaction to the CMC degree of substitution. To test the quality of the CMC product, the analysis that is conducted in this study are: degree of substitution analysis as written in ASTM D 1439, FTIR, and SEM-EDX. The best result that is got from this study is producing the CMC with degree of substitutions of 0.42 with addition of 3 gr sodium chloroacetate salt.