Method for preparing pure p-cresol and pure m-cresol by separating industrial mixed p-cresol and m-cresol
A technology for p-cresol and mixed cresol is applied in the field of separating industrial p-cresol to prepare pure p-cresol and pure m-cresol. Efficiency, low equipment requirements, improved safety effects
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Embodiment 1
[0027] Use inter-industrial p-cresol (purchased from Xingtai Xuyang Coal Chemical Co., Ltd.) as raw material, including m-cresol (58.5wt%), p-cresol (27.8wt%), 2,4-xylenol ( 5.7wt%), 2,5-xylenol (4.2wt%), also contains some o-cresol, phenol and 2-ethylphenol. First, add oxalic acid (Beihua Reagent Factory) in the glass three-necked flask, the amount of oxalic acid added is 0.6 times of the molar weight of p-cresol in the raw material mixed cresol, then add solvent cyclohexane, the amount of cyclohexane added is mixed 1 times the volume of cresol, heated to boiling, maintained for 0.5 hours, added raw materials mixed with cresol, kept the reaction solution boiling, maintained for 2 hours, stopped heating, naturally cooled down to 4°C, maintained for 4 hours. Filtration, the solid-liquid mixture is filtered and separated to obtain p-cresol oxalic acid crystals, and the filtrate is cyclohexane and by-product mixed cresol 1. After the obtained p-cresol crystals are drained, they ...
Embodiment 2
[0031] The experimental device and operation are the same as in Example 1, except that in the m-cresol extraction step, the molar ratio of the addition of urea to the m-cresol in mixed cresol 1 is 1:1, and p-cresol extraction efficiency, p-cresol purity, The composition of mixed cresol 1, the extraction efficiency of m-cresol, and the analysis results of m-cresol purity are shown in Table 1.
Embodiment 3
[0033]The experimental device and operation are the same as in Example 1, except that in the p-cresol extraction step, dihydrate oxalic acid is replaced by anhydrous oxalic acid, and the molar amount of anhydrous oxalic acid added remains unchanged; The molar ratio of m-cresol in cresol 1 was changed to 1:1, the extraction efficiency of p-cresol, the purity of p-cresol, the composition of mixed cresol 1 and the extraction efficiency of m-cresol, and the analysis results of m-cresol purity are shown in Table 1.
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