Process for the production of furfural using a water immiscible organic solvent
a technology of immiscible organic solvent and production process, applied in the field of furan derivative production, can solve the problems of affecting heat transfer characteristics and affecting the fouling of exposed reactor surfaces
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[0072]Unless otherwise specified, all the reagents are available from the Sigma-Aldrich Chemical Co (St. Louis, Mo.) and / or Alfa Aesar (Ward Hill, Mass.).[0073]In the examples, the following abbreviations are used:[0074]MN—1-methyl naphthalene[0075]2TBP—2-tert-butyl phenol[0076]2SBP—2-sec-butyl phenol[0077]NP—p-nonyl phenol
example a
[0078]Determination of the stability of the water immiscible solvent at reaction temperatures.
[0079]Three organic solutions were prepared by combining 1-methylnaphthalene (MN) with the desired alkyl phenol. 1 weight percent of tert-butylbenzene and sulfolane were added as dual internal standards to the organic solutions (only tert-butylbenzene was needed for quantitative analysis), making these solutions 74 weight percent 1-methylnaphthalene, 24 weight percent of the alkyl phenol and 2 weight percent internal standard. The desired alkyl phenols were 2-tertbutylphenol (2TBP), 2-sec-butylphenol (2SBP) and p-nonylphenol (NP). 1 milliliter of each solution was added to 8 different metal tube reactors. To each tube reactor was added 10 microliters (1 volume percent) of an aqueous acidic solution containing between 25 and 80 weight, percent sulfuric acid.
[0080]The metal tubes were sealed and were then put into a hot oil bath (initially set at 170° C., this cooled to about 150° C. upon loa...
example b
[0085]Water uptake in a water immiscible organic solvent
[0086]An excess of water (greater than 20 wt %) was added to the organic solvents and the mixtures were vigorously agitated for several minutes. The samples were allowed to sit overnight before being separated by centrifugation at 4000 rpm for 5 min. The water content, of the organic solvent samples was then measured by adding a known mass of the solvent sample to a Mettler Toledo DL31 Karl Fischer Titrator. The titrator used AQUASTARO CombiTitrant 5 titrant and HYDRANALO Methanol Dry solvent. Samples were run in sets of four, and the average value of the four runs is reported in TABLE 2.
TABLE 2Water inAromaticorganicPhenolhydrocarbonAromaticsolventExample(wt %)Phenol(wt %)hydrocarbon(wt %)25 52TBP95MN0.126 102TBP90MN0.227 252TBP75MN0.428 502TBP50MN1.0Comparative1002TBP 04.0AComparative1002TBP 04.2B
[0087]The results in TABLE 2 show that the water immiscible organic solvent of the disclosure absorbs a significantly less amount o...
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