Method for continuously synthesizing quinones in tubular reactor and equipment
A tubular reactor and compound technology are applied in the preparation of organic compounds, chemical instruments and methods, preparation of quinone oxides, etc., which can solve the problems of high production cost, severe environmental protection pressure, unfavorable cost saving, etc., and achieve the goal of improving production efficiency. Effect
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Embodiment 1
[0048] Taking the synthesis of 1,4-naphthoquinone as an example, its synthetic method comprises the following steps:
[0049] Dissolve 20g of naphthalene in 180g of n-heptane for later use; bottle the electrolytic oxidation solution for later use; slowly pump the two liquids into the tubular reactor at a ratio of 1:3 using a peristaltic pump; the reactor The temperature is set at 50-55°C. Since the reactor is made of transparent material, the experimental phenomena can be well observed; continuous feeding, residence time 1h, sampling and detection at the outlet of the reactor, after the naphthalene is almost completely reacted, the n-heptane layer is detected by HPLC, the naphthalene Content <2%; filter the reaction solution after reaction to obtain yellow crystals which are 1,4-naphthoquinone, wash and dry it with 15ml of deionized water, and finally obtain 20.8g of 1,4-naphthoquinone, which is detected by HPLC The purity is 98.97%; the filtrate is separated from oil and wat...
Embodiment 2
[0061] Taking the synthesis of 1,4-naphthoquinone as an example, its synthetic method comprises the following steps:
[0062] Dissolve 20g of naphthalene in the n-heptane recovered in 180g of Example 1 for subsequent use; bottle the electrolyte solution recovered in Example 1 for subsequent use; use a peristaltic pump to slowly inject the two liquids in a ratio of 1:5 respectively In a tubular reactor; the reactor temperature is set at 50-55°C. Since the reactor is made of a transparent material, the experimental phenomena can be well observed; continuous feeding, residence time 1.2h, sampling and testing at the outlet of the reactor, after the naphthalene is almost completely reacted, do HPLC detection on the n-heptane layer, naphthalene The content of <2%; the reaction solution after the reaction was filtered to obtain yellow crystals that were 1,4-naphthoquinone, which were washed and dried with 25ml deionized water to finally obtain 21.2g of 1,4-naphthoquinone, which was d...
Embodiment 3
[0066] Taking the synthesis of 5-nitro-1,4-naphthoquinone as an example, its synthetic method comprises the following steps:
[0067] Dissolve 30g of 5-nitro-1,4-naphthalene in 200g of n-heptane recovered in Example 2 for subsequent use; bottle the electrolyte solution recovered in Example 2 for subsequent use; The ratio of 1:6.5 is slowly poured into the tubular reactor; the temperature of the reactor is set at 60-65°C. Because the reactor is a transparent material, the experimental phenomenon can be well observed; continuous feeding, residence time 1.2h, sampling and testing at the outlet of the reactor, after the raw materials are almost completely reacted, the n-heptane layer is detected by HPLC, 5 -The content of nitro-1,4-naphthalene is <2%; filter the reaction solution after reaction to obtain yellow crystals which are 5-nitro-1,4-naphthoquinone, wash and dry it with 25ml deionized water , finally obtained 30.1g of the product, and the purity of the product detected by...
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