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United States Patent Office Patiented Apr 3,029,292 United States Patent Office Patiented Apr. 10, 1982 2 3,029,292 tionally steam distilling the treated phenol and subse PEENO PUERFECATION quently collecting a phenol material which may or may Joseph R. Nixon, Jr., Pitman, N.J., assignor to Hercules not be the product phenol but which will be a phenol Powder Company, Wilmington, Dei, a corporation of material purified to the extent of substantial removal of Yelaware the genetic impurities. No Drawing. Fied Aug. 19, 1960, Ser. No. 50,579 Of the specific impurities listed above, mesityl oxide 8 Caisas. (C. 260-622) and biacetyl were the first to be identified, and they were found to be inseparable from phenol by ordinary frac This invention relates to the purification of phenol, tional distiliation. Identification of the 2-methylbenzo and more particularly to the purification of phenoi ob O furan impurity was next and was difficult, but after the tained by oxidation of cumene and subsequent cleavage identification had been accomplished, several additional of the hydroperoxide produced. findings were made, namely, that the compound could When cumene hydroperoxide is cleaved by contacting inot be separated from phenol by ordinary fractional dis it with acidic catalysts such as sulfuric acid and acid tiliation, that it was steam-volatile and separable from treated clays, the cleavage mixture contains phenol and phenol by fractional steam distillation, and that it was acetone as the principal products. However, the mix formed by reaction between phenol and biacetyl, one of ture also contains a-methylstyrene, acetophenone, di the previously known genetic impurities. Before the methylph&nylcarbinol and cumylphenol as byproducts, method of formation of 2-methylbenzofuran had been and it may contain some unreacted cumene. testablished, it had been found in accordance with the The components of the cleavage mixture are prefer 20 present invention that the process resulted in formation ably recovered therefrom by fractional distillation. Fun of additional amounts of 2-methylbenzofuran and that damentally, the distillation results in obtaining an acetone the total could be removed by fractional steam distilla fraction, a phenol fraction and a residue comprising tion. Furthermore, it was found that biacetyl was not cumylphenol. In more detail, the distiilation may be the only precursor to 2-methylbenzofuran, and it also carried out to obtain a first fraction comprising acetone, became apparent that there were other alkyl-substituted a second fraction comprising c-methyistyrene, any unre benzofurans, the alkyl substituents being in the furan ring, acted cunene, if present, and water, a third fraction which should give rise to undesirable coloration on comprising phenol, and a residue comprising aceto chlorination of phenol obtained by cumene hydroperoxide phenone, dimethylphenylcarbinol, cumylphenol and some cleavage. - . resinous matter formed by polymerization of c-methyl 30 The overall findings may now be generalized. Dis styrene. Alternatively, the cumene and O-methylstyrene coioration on chlorination of cumene hydroperoxide phe may be collected with the acetone fraction or the phenol nol occurs primarily due to the presence therein of one fraction and separated therefrom by subsequent distilia or more alkyl-substituted benzofurans, such as 2-methyl-, tion. In any event, the phenol fraction is a crude phenol 3-methyl- and 2-isopropyl-benzofuran. The alkyl-sub which must be subjected to further distillation for puri stituted benzofurans are those compounds which are fication purposes. benzofuran substituted by one alkyl substituent in the The distillation procedures described above may be op furan ring, either at the 2- or 3- position. The alkyl erated batchwise, but are more conveniently carried out group will contain between one and about nine carbon on a continuous basis in a series of columns, the various atoms. Ordinarily, six carbon atoms will be a maxi fractions being obtained as overhead materials. The mun, and most of the substituted benzofurans will con Crude phenol fraction so obtained may then be distilled tain either one-carbon or three-carbon alkyl substituents. either continuously or in a batchwise operation to purify Nevertheless, discoloration also is contributed to by it. When operating batchwise, the crude phenol is stored mesityl oxide and one or more of the precursors of the and periodically removed from the storage tank for alkyl-substituted benzofurans. These precursors are charging to the batch still. compounds Such as biacetyl, hydroxyacetone, 4-methyl Early in the development of suitable distillation tech 2,3-pentanedione, and acetoin. In turn, the hydroxy niques for the isolation of pure phenol from cumene acetone may be formed by partial hydrogenation of meth hydroperoxide cleavage mixtures it was found that the ylglyoxal, which is an a-ketoaldehyde, and the 4-methyl product phenol, although otherwise pure and meeting 2,3-pentanedione may be formed by hydrogenation of standard specifications, contained certain genetic impuri 50 the carbon-carbon double bond in mesity oxide and oxi ties which were usually present in only minute amounts, dation of the resulting methyl isobutyl ketone. Similarly, but which were of such a nature that the phenol con the acetoin may be formed by partial hydrogenation of taining them developed an undesired red color when biacetyl, which is an a-diketone. The cz-diketones and Subjected to chlorination with elementary chlorine and the partial hydrogenation products thereof and of ox also developed an unwanted reddish amber color when 5 5 ketoaldehydes are all comparatively low molecular weight Sulfonated with concentrated sulfuric acid. These im compounds containing no more than about twelve, and purities obviously were not separable from the phenol usually no more than about nine, carbon atoms. The by ordinary fractional distillation, and their presence ef o-diketone and a-ketoaldehyde partial hydrogenation fectively prevented complete purification of the phenol products are those whereia one of the keto groups in the by this procedure alone. diketones and the aldehyde group in the ketoaldehydes The nature of the genetic impurities is now known, have been reduced to the corresponding alcohol groups, and a process of purifying phenol containing them has thus giving o-ketoalcohols as products. been discovered. The genetic impurities include mesityl Accordingly, it is now apparent that the inventive proc oxide, compounds which are a-diketones, such as bi ess is one wherein the prescribed catalysts promote sub acetyl, compounds which are partial hydrogenation prod 65 stantially complete reaction between phenol and the alkyl licts of (x-diketones or cy-ketoaldehydes, such as acetoin Substituted benzofuran precursors and wherein the total and hydroxy-acetone, and compounds which are alkyl alkyl-substituted benzofuran content is removed by ef substituted benzofurans such as 2-methylbenzofuran. ficient fractional steam distillation. The process is one comprising the particular steps of con The purification process of this invention therefore tacting a phenol, containing the genetic impurities, in constitutes an improvement in the method for the recovery the liquid phase with certain acidic catalysts at a tem of phenol by fractional distillation from the mixture pro perature in the range of about 45 to about 200 C., frac duced by cleavage of cumene hydroperoxide, which mix 3,029,292 3 é. ture comprises acetone and phenol as principal compo and was maintained at 120° C. for 70 hours, after which nents. The improvement comprises the steps of subject the 2-MBF content was 268 p.p.m. ing a cumene hydroperoxide cleavage mixture, from which A sample of the treated phenol was separated into two the acidic catalyst has been substantially removed, as portions, one of which was subjected to ordinary batch by neutralization or extraction, to fractional distillation 5 distillation, with the charge being added to the still pot. to remove acetone and then contacting in the liquid phase The other portion was fractionally steam distilled using any substantially acetone-free, predominantly phenol a modified inverted batch still technique, in which distilled containing material, which material contains genetic im water was charged to the still pot and brought to reflux, purities comprising mesityl oxide, an alkyl-substituted and then the treated phenol was pumped continuously into benzofuran and at least one precursor of said alkyl-sub O the top of the still while maintaining water refux. Thus, stituted benzofuran, under acidic conditions with an acidic all of the phenol was contacted with steam as it flowed catalyst selected from the group consisting of boron tri down and across all of the trays of the column. After fluoride and the halides, sulfates and nitrates of platinum all the charge had been added, distillation was carried out and those heavy metals of groups II B, III A, V, V A in the normal manner. and VIII of the periodic table having an atomic number The phenol obtained from each distillation was chlo less than 52, at a temperature in the range of about 45° rinated according to the chlorination test set forth herein to about 200° C., fractionally steam distilling the treated after. The phenol from ordinary distillation had a color phenol-containing material, and subsequently collecting a of 12 absorbance units at 540 Mu, whereas that from purified phenol-containing material, preferably by frac steam distillation contained 8 p.p.m. 2-MBF and had a tonally distilling in the absence of water. color of 0.33 at 510 mg, and 0.4 at 540 Inu. In other words, the improvement of this invention in EXAMPLE 2 volves treatment with the prescribed catalysts of any pre dominantly phenol-containing material existing in the The procedure of Example 1 was substantially dupli distillative recovery system after the acetone has been . cated except that after about five hours of reaction in removed from the cleavage mixture, which itself is not the presence of the ferric chloride there was added to the effectively improved by the treatment.
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