Method for manufacturing 4-alkylphenols
A technology for alkyl phenol and phenol, applied in the field of preparing 4-alkyl phenol, can solve the problems of low selectivity and no use, and achieve the effect of high selectivity
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Embodiment 1
[0055] (first step)
[0056] In a 4-necked flask with an inner volume of 100 mL equipped with a stirrer, a condenser and a thermometer, 50 g (531 mmol) of phenol and 12.5 g of proton-substituted β-zeolite (H-BEA-25, produced by Süd Chemie Group production), and the resulting mixture was stirred. The mixture was heated to 90° C., and 22.6 g (266 mmol) of TBA containing 13% by weight of water were added dropwise to the mixture using a syringe over 3 hours. The resulting mixture was further stirred at the same temperature for 5 hours to carry out an alkylation reaction. The reaction solution was analyzed by gas chromatography to determine the relative proportions of various compounds, the conversion rate of phenol, the selectivity and yield of 4-TBP. The results are shown in Table 1.
[0057] (second step)
[0058] Beta-type zeolite was removed from the reaction mixture obtained in the first step by filtration. The resulting filtrate was then distilled under reduced pressure...
Embodiment 2
[0063] (second step)
[0064] From the reaction mixture obtained in the first step of Example 1, β-type zeolite was removed by filtration. The resulting filtrate was then distilled under reduced pressure [26.7 to 4.7 kPa (200 to 35 mmHg), internal temperature 90 to 120° C.] to remove water. After removal of the water, the water concentration in the mixture was determined to be 0.1% by weight. Furthermore, the amount of phenol (reported as a molar ratio relative to the TBA consumed in the first step of the alkylation reaction) was 1.1.
[0065] (third step)
[0066] Into a 4-neck flask with an inner volume of 200 mL equipped with a stirrer, a condenser and a thermometer were added the dehydrated mixture obtained from the second step and 100 g of phenol. This allowed the amount of phenol (reported as the molar ratio relative to the TBA consumed in the first step of the alkylation reaction) to be adjusted to 6. Then 12.5 g of proton-substituted Y-type zeolite (as described ab...
Embodiment 3
[0069] (second step)
[0070] From the reaction mixture obtained in the first step of Example 1, β-type zeolite was removed by filtration. The resulting filtrate was then distilled under reduced pressure [26.7 to 4.7 kPa (200 to 35 mmHg), internal temperature 90 to 120° C.] to remove water. After removal of the water, the water concentration in the mixture was determined to be 0.1% by weight. Furthermore, the amount of phenol (reported as a molar ratio relative to the TBA consumed in the first step of the alkylation reaction) was 1.1.
[0071] (third step)
[0072] In a 4-neck flask with an inner volume of 10 mL equipped with a stirrer, a condenser and a thermometer, the dehydration mixture obtained from the second step and 12.5 g of acidic cation exchange resin (Amberlyst 15E, produced by Organo Corporation) were added, and the resulting The mixture was brought to 90 °C and then stirred for 1 h to carry out the rearrangement reaction. The reaction solution was analyzed by...
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