Simultaneous isolation of cellulose and lignin from wheat straw and catalytic conversion to valuable chemical products
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- Measurements
Determination and calculation
The contents (purities) of cellulose, hemicellulose, lignin and ash were determined according to the previously reported procedures [ 27 ]. The determinations were based on the averages of three replicates. The yields of cellulose and lignin, theoretical yield of lignin and removal rates of components, such as hemicellulose, lignin and ash, were calculated as follows. Componenet yield (% ) = Mass of component isolated from wheat straw Mass of EWS × 100%, Removal rate (% ) = 1 − Amount of component in isolated cellulose Total amount of component in EWS × 100%, Theoretical yield of lignin (% ) = Removal rate of lignin × Lignin content in EWS × Mass of EWS Mass of EWS ×100%, Measurements Infrared (IR) spectroscopy was performed on an EQUI- NOX 55 spectrometer in the range of 500–4000 cm −1 . Prior to analysis, the solid samples were grounded with dried KBr powder and compressed into a disk. X-ray dif- fraction (XRD) was performed on a χ’Pert Pro diffrac- tometer with CuKα radiation at 40 kV and 40 mA in the range from 10° to 80°, and the scanning rate was 5°/min. The surface morphologies of wheat straw and its deriva- tives were observed using a scanning electron micros- copy (SEM) microscope (Hitachi N-3000 apparatus), and a thin layer of gold was sputtered onto the sample prior to imaging. Elemental analysis (EA) was performed on a Vario EL III elemental analyzer. Specific surface areas were calculated using the BET model on a NOVA 2000e fully automatic specific surface and porosity analyzer. X-ray photoelectron spectroscopy (XPS) was recorded on a Kratos XSAM800 spectrometer with MgKα radia- tion (1253.6 eV), which was operated at 12 kV and 10 mA without a monochromator. The qualitative anal- ysis of sugars was performed on a LC-100 PLUS HPLC equipped with a Rezex ROA column (Phenomenex) and a refractive index detector (Shimadzu Corp., Kyoto, Japan) at 63 °C using H 2 SO 4 (4 mM) as an eluent at a flow rate of 0.6 mL/min. HPLC–MS was performed on Waters Arc HPLC-2998 PDA-QDa equipped with YMC ODS-A (5 µm, 4.6 × 250 mm) using 85 wt% acetonitrile–water as the mobile phase at a flow rate of 1.0 mL/min. Nuclear magnetic resonance (NMR) including 1 H NMR and 13 C NMR spectra were acquired on a Unity-Inova 600 at 50 °C using DMSO-d6 as solvent and tetramethylsilane as internal standard. The molecular weight of lignin was determined using Waters E2695 GPC (see Additional file 1 ). Recovery rate (% ) = Yield Component content of EWS × 100%. Page 4 of 13 Yu et al. Appl Biol Chem (2021) 64:15 The quantitative analysis of HMF derived from wheat straw cellulose was determined by a GC2020 gas chro- matography equipped with a HP-1 capillary column (30 m × 0.25 mm × 0.25 μm). The initial temperature was retained at 50 °C for 3 min, then ramped to 230 °C at 10 °C/min, and held at this final temperature for 5 min. The gasification and detector temperatures were 240 and 260 °C, respectively. Glucose derived from cellulose was determined by DNS method using a UV measurement at 540 nm [ 28 ]. The quantitative analysis of the reaction product derived from lignin was performed on a LC-100 PLUS HPLC equipped with reversed-phase Novapak- C18-100 silica column (4.6 × 150 mm, 4 μm) and UV detector. The mixture of acetonitrile: 1 wt% phosphoric acid solution (12:88, v/v) was employed as mobile phase at the flow rate of 1.2 mL/min with column temperature at 32 °C. Download 2.27 Mb. Do'stlaringiz bilan baham: |
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