A post-processing method for preparing hydroquinone by diazotization hydrolysis method of p-aminophenol
A technology of p-aminophenol and hydroquinone, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of difficult operation, pipeline blockage and energy consumption, etc., achieve simple process and reduce production cost With environmental pressure, the effect that there is little tar
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Embodiment 1
[0034] (1) Combine 800g of the extracted oil phase of the reaction part (the content of hydroquinone is 3.5%, the content of impurities is 0.39%) and 480g of the extracted oil (the content of hydroquinone is 10.27%), and the mixture obtained from the above combination is 1280g, of which methyl The content of isobutyl ketone is 93%. Then, under the condition of nitrogen protection, desolvate DS1 to a concentration of 40% under normal pressure, and then slowly lower the temperature to 25°C to crystallize hydroquinone in methyl isobutyl ketone, and recover 963.6g of methyl isobutyl ketone And 23g precipitation recovery water;
[0035] (2) After separating the crystallization mixture from F1, 49.5g of crude hydroquinone and 254.8g of crystallization mother liquor were obtained;
[0036](3) Add 110g of raffinate water, 1.5g of activated carbon, 0.6g of sodium metabisulfite, 0.1g of zinc powder, and 0.3g of sulfuric acid to 49.5g of crude hydroquinone for decolorization DC. After h...
Embodiment 2～5
[0042] Different stripping temperatures were adopted, and other operating conditions were the same as in Example 1, and the obtained results are shown in Table 1.
[0043] Table 1 Effect of stripping temperature on stripping efficiency
[0044]
Embodiment 6
[0046] (1) Merge the extracted oil phase of 800g reaction part (the content of hydroquinone is 3.5%, miscellaneous
[0047] content of 0.39%) and 545g of extracted oil (hydroquinone content is 8.89%), the above combined 1345g of the resulting mixture, the content of n-butyl acetate in the mixture is 93.4%. Then under the condition of nitrogen protection, desolvate DS1 to a concentration of 35% at normal pressure, and then slowly cool down to 20°C to crystallize hydroquinone in n-butyl acetate, recover 1056.8g of n-butyl acetate solvent and 34g desolvent Dissolve water;
[0048] (2) After separating the crystallization mixture from F1, 52.7g of crude hydroquinone and 232.1g of crystallization mother liquor were obtained;
[0049] (3) Add 110g of raffinate water, 1.5g of activated carbon, 0.6g of sodium thiosulfate, 0.1g of zinc powder, and 0.3g of hydroquinone to 52.7g of crude hydroquinone for decolorization DC. Reflux for 1 hour; then separate F2 while it is hot, wash the f...
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