Ultrasonik Destekli Asit Hidrolizi ile Nanokristalin Selüloz Üretimi

Selüloz nanokristalin (SN) atkestanesi tohumu kabuğundan asit hidrolizi ile ekstrakte edilmiştir. Ham kabuklar küçük parçalara bölünmüş, alkali işleme tabi tutulmuş, ağartılmış ve sülfirik asit ile muamele edilmiştir. Hidroliz reaksisyonunun süresinin elde edilen SN’lerin yapısına, kristalinitesine, termal, morfolojik ve topolojik özelliklerine etkisi araştırılmıştır. Fouriere kızıl ötesi spektrumları incelendiğinde ligninin ve hemiselülozun alkali ve ağartma işlemleri sırasında üretilen ürünlerin yapısından tamamen uzaklaştırıldığı görülmüştür. Üretilen SN’lerin kristalinite dereceleri artan reaksiyon sürei ile birlikte önce artmış ve 20 dakikadan sonra azalmaya başlamıştır. Atkestanesi kabuğundan SN üretiminde optimal isolasyon süresi 20 dakika (45 °C’de ve % 50’lik sülfirik asit çözeltisi içerisinde) olarak belirlenmiştir. Selüloz ve SN’nin morfolojik özellikler Taramalı Elektron Mikroskobu ilen incelenmiş ve selüloza göre SN’nin iğne benzeri değişmiş bir yapıya sahip olduğu gözlenmiştir. 585 nm’lik Ra değeri ile selülozun yüzey pürüzlülüğünün SN’ye göre (111 nm) dah yüzek olduğu Atomik Kuvvet mikrokobu ile karakterize edilmiştir. SN’lerin termal stabilitesi artan isolasyon süresi ile selüloza göre azalmıştır.

Anahtar Kelimeler:

atkestanesi, selüloz nanokristal, asit hidrolizi, kristalinite

Production of Nanocrystalline Cellulose by Ultrasonically Assisted Acid Hydrolysis

Cellulose nanocrystals (SN) were isolated from the shell of horse chestnut seed using sulfuric acid hydrolysis. The raw shells were broken into small pieces, treated alkali, bleached, and subjected to the sulphuric acid process. The effect of hydrolysis time on the structure, crystallinity, thermal properties, morphology, and topology of cellulose and SNs were investigated. The lignin and hemicellulose contents were almost entirely removed from the produced cellulose through the alkali and bleaching treatments demonstrated to Fourier transform infrared spectroscopy. The crystallinity of SNs was increased firstly with increasing reaction time and then along with the reaction times longer than 20 minutes decreases. The optimal isolation time for SN production was found to be 20 min at 45 °C in a 50 % sulfuric acid solution. The morphology of the cellulose and SN were investigated by Field Emission Scanning Electron Microscopy and revealed a changed needle-like surface structure of SN relative to cellulose. The surface roughness of cellulose with a Ra value of 585 nm is higher than the cellulose nanocrystalline with a Ra value of 111 nm, which were characterized using Atomic Force Microscopy. The thermal stability of SNs was decreased during increased extraction times compared with cellulose.

Keywords:

horse chestnut, cellulose nanocrystals, acid hydrolysis, crystallinity,

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