Continuous Purification of Biodiesel with Deep Eutectic Solvent in a Laboratory Karr Column
<p>Geometry of the pulsation plates column and plates: (<b>a</b>) stainless steel (plate A) and PETG (plate B); (<b>b</b>) PETG (plate C).</p> "> Figure 2
<p>Influence of the pulsation rate on Sauter mean diameter, <span class="html-italic">d</span><sub>32</sub>, and surface area, <span class="html-italic">a</span>, (<span class="html-italic">m</span>(DES)/<span class="html-italic">m</span>(BD2) = 0.24).</p> "> Figure 3
<p>Influence of DES to BD2 mass flowrate ratio on the maximum droplet size (<span class="html-italic">Af</span> = 0.02 ms<sup>−1</sup>).</p> "> Figure 4
<p><sup>1</sup>H NMR spectra of biodiesel 1—influence of extraction time (<span class="html-italic">n</span> = 800 rpm; <span class="html-italic">m</span>(DES)/<span class="html-italic">m</span>(BD) = 0.25).</p> "> Figure 5
<p><sup>1</sup>H NMR spectra of biodiesel 1—influence of extraction time (<span class="html-italic">Af</span> = 0.027 m/s; <span class="html-italic">m</span>(DES)/<span class="html-italic">m</span>(BD) = 0.32).</p> "> Figure 6
<p><sup>1</sup>H NMR spectra of biodiesel 1—influence of agitation rate and DES to biodiesel mass ratio (<span class="html-italic">t</span> = 25 min).</p> "> Figure 7
<p>FTIR spectra of biodiesel 2 (plate A, <span class="html-italic">φ</span><sub>V</sub> = 0.2; <span class="html-italic">Af</span> = 0.02 m/s).</p> "> Figure 8
<p><sup>1</sup>H NMR spectrum of biodiesel 2 (<span class="html-italic">Af</span> = 0.013 m/s; <span class="html-italic">m</span>(DES)/<span class="html-italic">m</span>(BD) = 0.24).</p> "> Figure 9
<p><sup>13</sup>C NMR spectrum of biodiesel 2 (<span class="html-italic">Af</span> = 0.013 m/s; <span class="html-italic">m</span>(DES)/<span class="html-italic">m</span>(BD) = 0.24).</p> "> Figure 10
<p>2D HMQC NMR spectrum of biodiesel 2 (<span class="html-italic">Af</span> = 0.013 m/s; <span class="html-italic">m</span>(DES)/<span class="html-italic">m</span>(BD) = 0.24).</p> ">
Abstract
:1. Introduction
2. Materials and Methods
2.1. Chemicals
2.2. Biodiesel Synthesis
2.3. Characterization of DES and Biodiesel
2.4. Liquid–Liquid Extraction
2.4.1. Batch Extraction
2.4.2. Continuous Extraction
2.5. 3D Printing
3. Results and Discussion
3.1. Physical and Surface Properties of Phases
3.2. Drop Size
3.3. Extraction Efficiency
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Data Availability Statement
Conflicts of Interest
References
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Chemical | Manufacturer | CAS Number |
---|---|---|
Methanol, HPLC grade | J.T.Baker | 67-56-1 |
Potassium hydroxide, p.a. | Kemika | 1310-58-3 |
Choline chloride, 99% | Acros Organics | 67-48-1 |
Ethylene glycol, p.a. | Lach-Ner | 107-21-1 |
Phase | ρ, kg m−3 | μ, Pa s | σ, mN m−1 | γ (DES/BD), mN m−1 |
---|---|---|---|---|
DES | 1117.06 | 0.0355 | 43.74 | |
Biodiesel 1 | 876.79 | 0.0039 | 27.80 | 0.17 |
Biodiesel 2 | 878.25 | 0.0043 | 26.36 | 14.96 |
OW (mJ m−2) | Wu (mJ m−2) | AB (mJ m−2) | |||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Water | FA 1 | DIM | γ | γd | γp | γ | γd | γp | γ | γd | γA | γB | |
Steel | 77.4 | 72.8 | 54.6 | 33.0 | 26.3 | 6.7 | 37.1 | 28.3 | 8.8 | 31.5 | 31.5 | 0.0 | 11.8 |
PETG | 74.7 | 49.6 | 31.3 | 46.2 | 41.6 | 4.6 | 49.3 | 40.4 | 8.9 | 45.8 | 43.7 | 0.2 | 6.7 |
Phase | Steel | PETG m−1 | ||
---|---|---|---|---|
θ (90 ms), ° | θ (2000 ms), ° | θ (90 ms), ° | θ (2000 ms), ° | |
DES | 83.0 | 63.7 | 77.6 | 58.2 |
Biodiesel 2 | 63.4 | 7.5 | 44.5 | 17.9 |
n, rpm | t, min | m(DES)/m(BD) | % FAME | A(Me)/A(OH) |
---|---|---|---|---|
400 | 30 | 0.25 | 95.20 | 3.31 |
600 | 30 | 0.25 | 95.57 | 6.88 |
800 | 15 | 0.25 | 98.19 | 9.90 |
30 | 0.25 | 98.60 | 9.99 | |
30 | 0.50 | 97.30 | 12.18 | |
30 | 0.75 | 97.09 | 19.23 | |
30 | 1.00 | 98.34 | 27.23 | |
45 | 0.25 | 97.04 | 11.94 | |
60 | 0.25 | 98.09 | 14.01 | |
1000 | 30 | 0.25 | 98.26 | 9.26 |
φD, % | m(DES)/m(BD) | Af, m s−1 | t, min | % FAME | A(Me)/A(OH) |
---|---|---|---|---|---|
20.0 | 0.32 | 0.027 | 5 | 98.55 | 1.29 |
15 | 98.12 | 3.14 | |||
25 | 97.11 | 6.18 | |||
20.0 | 0.32 | 0.040 | 5 | 97.53 | 1.37 |
15 | 97.15 | 4.29 | |||
25 | 96.88 | 6.59 | |||
33.3 | 0.64 | 0.027 | 5 | 96.78 | 1.53 |
15 | 96.78 | 8.61 | |||
25 | 96.92 | 11.68 |
Plate | φD, % | m(DES)/m(BD) | Af, m s−1 | FAME, % | MG, % | DG, % | Free Gly, % | Total Gly, % | A(Me)/A(OH) |
---|---|---|---|---|---|---|---|---|---|
A | 15.8 | 0.24 | 0.013 | 96.5 | 0.29 | 0.06 | 0.105 | 0.188 | 6.47 |
15.8 | 0.24 | 0.020 | 95.5 | 0.30 | 0.06 | 0.084 | 0.169 | 8.13 | |
15.8 | 0.24 | 0.027 | 99.3 | 0.29 | 0.06 | 0.099 | 0.182 | 6.45 | |
20.0 | 0.32 | 0.020 | 96.8 | 0.29 | 0.05 | 0.076 | 0.157 | 4.94 | |
25.0 | 0.42 | 0.020 | 97.3 | 0.26 | 0.05 | 0.036 | 0.110 | 5.48 | |
B | 15.8 | 0.24 | 0.013 | 97.4 | 0.29 | 0.06 | 0.092 | 0.175 | 9.48 |
15.8 | 0.24 | 0.020 | 97.8 | 0.28 | 0.06 | 0.067 | 0.147 | 6.45 | |
15.8 | 0.24 | 0.027 | 94.5 | 0.28 | 0.05 | 0.063 | 0.142 | 5.38 | |
20.0 | 0.32 | 0.020 | 98.5 | 0.29 | 0.06 | 0.074 | 0.157 | 8.19 | |
25.0 | 0.42 | 0.020 | 97.4 | 0.29 | 0.06 | 0.075 | 0.158 | 7.20 | |
C | 15.8 | 0.24 | 0.020 | 97.9 | 0.27 | 0.05 | 0.120 | 0.196 | 9.12 |
20.0 | 0.32 | 0.020 | 99.1 | 0.27 | 0.05 | 0.047 | 0.123 | 10.44 | |
25.0 | 0.42 | 0.020 | 99.5 | 0.26 | 0.05 | 0.048 | 0.122 | 7.36 |
Method | Feedstock | xinitial(FG 1), % | m(DES)/m(BD) | n, rpm or Af, m s−1 | xfinal(FG), % | Ref. |
---|---|---|---|---|---|---|
Batch | Palm oil | 0.04093 | 0.21–0 86 | 200 rpm | <0.005 | [6] |
Animal fats | 0.349–3.026 | 0.50–3.00 | 500 rpm | <0.005–1.210 | [26] | |
Sunflower oils | 0.659–1.939 | 0.25–1.00 | 150–700 rpm | 0.018–0.087 | [9] | |
Waste coffee ground oils | 0.748–1.647 | 1.00 | 500 rpm | 0.024–0.029 | [10] | |
Continuous—Karr column | Sunflower oil | 1.939 | 5.00 | 0.036–0.084 m s−1 | <0.005 | [9] |
Waste coffee ground oil | 1.107 | 1.40 | 0.048 m s−1 | 0.02 | [10] | |
Continuous—microreactor | Sunflower oil | 0.09 | 1:0.65 (vol. flow rate ratio) | - | 0.01 | [8] |
Waste cooking oil | 0.165 | - | <0.05 | [8] |
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Sander, A.; Petračić, A.; Vrsaljko, D.; Parlov Vuković, J.; Hršak, P.; Jelavić, A. Continuous Purification of Biodiesel with Deep Eutectic Solvent in a Laboratory Karr Column. Separations 2024, 11, 71. https://doi.org/10.3390/separations11030071
Sander A, Petračić A, Vrsaljko D, Parlov Vuković J, Hršak P, Jelavić A. Continuous Purification of Biodiesel with Deep Eutectic Solvent in a Laboratory Karr Column. Separations. 2024; 11(3):71. https://doi.org/10.3390/separations11030071
Chicago/Turabian StyleSander, Aleksandra, Ana Petračić, Domagoj Vrsaljko, Jelena Parlov Vuković, Patricija Hršak, and Antonija Jelavić. 2024. "Continuous Purification of Biodiesel with Deep Eutectic Solvent in a Laboratory Karr Column" Separations 11, no. 3: 71. https://doi.org/10.3390/separations11030071