Process for the production of phenol
A technology of phenol and by-products, which is applied in the production of bulk chemicals, chemical instruments and methods, and the addition of hydrocarbons with simultaneous hydrogenation, etc., which can solve the problems of dehydration catalyst deactivation and other issues
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Embodiment 1
[0103] Embodiment 1 (contrast): use H 2 SO 4 catalyst for alcohol dehydration
[0104] A first feed solution (Solution A) was prepared with the following composition:
[0105]
[0106] 5.0 g of solution A was added to a round bottom test tube equipped with a magnetic stirrer and different amounts of H were added in three separate experiments 2 SO 4 (50, 150 and 300 ppm by weight). Each mixture was heated in a silicone oil bath at a temperature of 120° C., and the liquid portion was sampled by gas chromatography (GC). figure 1 The conversion of cyclohexanone in wt % is shown as a function of time-on-time (T.O.S.) in minutes, where curves 101, 103 and 105 correspond to 50 ppm, 150 ppm and 300 ppm of H 2 SO 4 . The data show an undesirably high conversion of cyclohexanone product and only low conversion of phenylcyclohexanol.
[0107] With higher H 2 SO 4 Concentrations (500 ppm by weight) were repeated as described. show on figure 2 The phenylcyclohexanol convers...
Embodiment 2
[0108] Example 2 (Comparative): Alcohol Dehydration Using Zeolite Y Catalyst
[0109] 5.0 grams of solution A was added to a round bottom test tube equipped with a magnetic stirrer, to which was added 0.5 grams of powdered zeolite Y catalyst. The mixture was heated in a silicone oil bath at a temperature of 120°C, and the liquid portion was sampled by GC. The data is summarized in image 3 and 4 middle. image 3 Alcohol conversion in wt % is shown as a function of time-on-time (T.O.S.) in minutes, where curves 301 and 303 correspond to zeolite Y and MoO, respectively 2 / ZrO 2 (described in detail in Example 3 below). Figure 4 The yield of phenylcyclohexene in mol % is shown as a function of the conversion of alcohol in wt %, where curves 401 and 403 correspond to zeolite Y and MoO, respectively 2 / ZrO 2 (described in detail in Example 3 below).
Embodiment 3
[0110] Embodiment 3 (comparison): use MoO 2 / ZrO 2 catalyst for alcohol dehydration
[0111] MoO was prepared by the following steps 2 / ZrO 2 Catalyst: First, 500 grams of ZrOCl 2 ·8H 2 O was dissolved in 3.0 L of distilled water with stirring. Alternatively, prepare 260 g concentrated NH 4 OH, 66 g (NH4 ) 6 Mo 7 o 24 4H 2 O and 3.0 L of distilled water. Both solutions were heated to 60°C, and the heated solutions were combined using nozzle mixing at a rate of 50 ml / min. The pH of the final complex was adjusted to approximately 9 by addition of concentrated ammonium hydroxide. The resulting slurry was then placed in a polypropylene bottle and placed in a steam box (100°C) for 72 hours. The product formed was recovered by filtration, washed with excess water and dried overnight at 85°C. A sample of the dried product was calcined to 800° C. for 3 hours in flowing air to produce an acidic oxide catalyst.
[0112] Add 5.0 g of solution A to a round bottom test tube ...
PUM
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