**Ultrasonic Irradiation Coupled with Microwave Treatment for Eco-friendly Process of Isolating Bacterial Cellulose Nanocrystals**

#### **Endarto Yudo Wardhono 1,\*, Hadi Wahyudi 1, Sri Agustina 1, François Oudet 2, Mekro Permana Pinem 3, Danièle Clausse 3, Khashayar Saleh 3 and Erwann Guénin 3,\***


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Received: 17 September 2018; Accepted: 17 October 2018; Published: 20 October 2018

**Abstract:** The isolation of crystalline regions from fibers cellulose via the hydrolysis route generally requires corrosive chemicals, high-energy demands, and long reaction times, resulting in high economic costs and environmental impact. From this basis, this work seeks to develop environment-friendly processes for the production of Bacterial Cellulose Nanocrystals (BC-NC). To overcome the aforementioned issues, this study proposes a fast, highly-efficient and eco-friendly method for the isolation of cellulose nanocrystals from Bacterial Cellulose, BC. A two-step processes is considered: (1) partial depolymerization of Bacterial Cellulose (DP-BC) under ultrasonic conditions; (2) extraction of crystalline regions (BC-NC) by treatment with diluted HCl catalyzed by metal chlorides (MnCl2 and FeCl3.6H2O) under microwave irradiation. The effect of ultrasonic time and reactant and catalyst concentrations on the index crystallinity (CrI), chemical structure, thermal properties, and surface morphology of DP-BC and BC-NC were evaluated. The results indicated that the ultrasonic treatment induced depolymerization of BC characterized by an increase of the CrI. The microwave assisted by MnCl2-catalyzed mild acid hydrolysis enhanced the removal of the amorphous regions, yielding BC-NC. A chemical structure analysis demonstrated that the chemical structures of DP-BC and BC-NC remained unchanged after the ultrasonic treatment and MnCl2-catalyzed acid hydrolysis process.

**Keywords:** bacterial cellulose nanocrystals; ultrasonic irradiation; microwave treatment; catalyzed hydrolysis; crystallinity index
