Method for removing impurities from oxidation products
A product and impurity technology, applied in the field of products obtained by oxidation of halogenated ortho-xylene, can solve problems such as cost increase, yield loss, color increase, etc.
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Embodiment 1
[0063] Synthesis of 4- and 7- Chlorinated 2-benzo[c]furanone (produced by reduction of 3-chlorophthalic anhydride) mixture A 35% by weight solution of crude chlorophthalic acid in water was prepared. The mixture was stirred at about 60°C for 2 hours. After stirring, all the chlorophthalic anhydride had been hydrolyzed to chlorophthalic acid, as shown by gas chromatographic analysis (GC), which showed There is no anhydride in the organic phase. preparing vials each containing 5 milliliters (ml) of an aqueous phase containing a concentration of crude chlorophthalic acid (5% to 35% by weight, based on the weight of the total aqueous phase), and Optional acetic acid (0% to 36% by weight, based on the weight of the entire aqueous phase). Each vial was then treated with 5 ml of toluene, o-dichlorobenzene (ODCB) or o-xylene. These vials were then shaken vigorously on a mechanical shaker at a specific temperature (22°C, 42°C or 60°C) for 50 minutes. The phases were allowed to sepa...
Embodiment 2
[0068] The procedure of Example 1 was repeated, but the extraction was carried out at 22° C. with an initial chlorophthalic acid concentration of 22% by weight in the presence of different contents of acetic acid. Data are presented in Table 2.
[0069] Table 2
[0070]
[0071] These data show that increasing the acetic acid addition decreases the K and β values when using toluene or ODCB as the extractant under these conditions. Similar trends were observed when xylene was used as the extraction solvent at 30 °C and 60 °C.
Embodiment 3
[0073] The procedure of Example 1 was repeated, but the extraction was performed without acetic acid at different wt% initial chlorophthalic acid concentrations at 60°C.
[0074] table 3
[0075]
[0076] These data show that under these conditions, when using toluene or ODCB as the extractant, in the absence of acetic acid, the K value of the extraction increases with increasing temperature, while the selectivity increases or decreases depending on the extraction solvent. . When xylene or 4-chloro-o-xylene was used as the extraction solvent at 30°C, the K value and the selectivity value were similar and decreased with the increase of chlorophthalic acid content in the aqueous phase. Similar trends were observed when xylene was used as the extraction solvent at 60 °C, moreover, K values and selectivity values were lower than those obtained at 30 °C.
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