the production of thymoquinone from thymol and carvacrol
the production of thymoquinone from thymol and carvacrol
the production of thymoquinone from thymol and carvacrol
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6.1. Materials<br />
CHAPTER 6<br />
EXPERIMENTAL<br />
Metal nitrates (nitrates <strong>of</strong> Cr(III), Fe(III), Bi(III), Ni(II), Zn(II)), <strong>carvacrol</strong> (5-<br />
isopropyl-2-methylphenol), <strong>thymol</strong> (2-isopropyl-5-methylphenol), <strong>thymoquinone</strong> (2-<br />
isopropyl-5-methyl-p-benzoquinone), salicylaldehyde, 1,3-diamino-propane <strong>and</strong><br />
hydrogen peroxide (30%) were purchased <strong>from</strong> Sigma-Aldrich. O<strong>the</strong>r reagents <strong>and</strong><br />
solvents used were HPLC grade <strong>and</strong> obtained <strong>from</strong> Sigma-Aldrich. Essential oil was<br />
purchased <strong>from</strong> Arifo ulları company. Zeolite-NaY (CBV100, SiO2/Al2O3 5.1) that<br />
contained 13.0 wt% Na2O was purchased <strong>from</strong> Zeolyst International Company in <strong>the</strong><br />
form <strong>of</strong> powder with <strong>the</strong> sizes less than one micron. The surface area <strong>of</strong> <strong>the</strong> zeolite<br />
powder was 900 m 2 g -1 . The unit cell formula <strong>of</strong> this sample was Na54(AlO2)54(SiO2)138<br />
when dehydrated. Zeolite-NaY was activated at 500 °C in an oven for at 5h <strong>and</strong> cooled<br />
to room temperature in a desiccator before use.<br />
6.2. Methods<br />
6.2.1. Catalyst Preparations<br />
H2salpn, metal exchanged zeolite Y, <strong>and</strong> encapsulated complexes were prepared<br />
by following a procedure similar to one described in <strong>the</strong> literature (Maurya et al. 2002).<br />
6.2.1.1. Preparation <strong>of</strong> Lig<strong>and</strong> (H2Salpn)<br />
Salicylaldehyde (12.2 g, 0.1 mol) was dissolved in 65 ml methanol <strong>and</strong> mixed<br />
with a solution <strong>of</strong> 1,3-diamino-propane (3.65 g, 0.05 mol) in 25 ml methanol. Solution<br />
was refluxed in a water bath for 1 hour. After reducing <strong>the</strong> volume <strong>of</strong> solution to 50 ml,<br />
flask was kept at ambient temperature for 2 hours. Yellow shining plates were filtrated,<br />
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