A kind of production method of quinolinic acid
A production method, the technology of quinolinic acid, applied in the direction of organic chemistry, etc., can solve the problems of low yield and purity of quinolinic acid, increasing the difficulty of wastewater treatment, reducing the yield of quinolinic acid, etc., so as to increase the difficulty of treatment and alleviate the environment Pressure, effect of reducing refining steps
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Embodiment 1
[0054] A production method of quinolinic acid is carried out according to the following steps:
[0055] Step 1. Oxidation reaction to prepare copper quinolinate:
[0056] Add 1720kg of water, 95kg of copper oxide and 400kg of concentrated sulfuric acid into the reaction kettle, stir and keep at 50℃ for 1h, then add 235kg of quinoline to the reactor, and add dropwise sodium chlorate solution with a concentration of 45% by weight at 98℃ 1535kg, dripping time is 17h, after dripping, keep it at 100℃ for 4h, then cool to 25℃, keep it for 1h, centrifuge, and wash the solid to neutrality to obtain copper quinolinate. The filtrate is the mother liquor of oxidation reaction.
[0057] Step 2: Oxidation reaction mother liquor treatment:
[0058] Add sodium carbonate to the oxidation reaction mother liquor, adjust the pH value to neutral, then add flake caustic soda or liquid caustic soda, adjust the pH value to 9, press filtration, and wash the filter cake with water to obtain recovered basic co...
Embodiment 2
[0071] A production method of quinolinic acid is carried out according to the following steps:
[0072] Step 1. Oxidation reaction to prepare copper quinolinate:
[0073] Add 1800kg of water, 105kg of copper oxide and 440kg of concentrated sulfuric acid to the reaction kettle, stir, keep at 60℃ for 2h, then add 265kg of quinoline to the reactor, and add 50wt% sodium chlorate solution dropwise at 102℃ 1600kg, dripping time is 18h, after dripping, keep at 105℃ for 5h, then cool to 20℃, keep for 2h, centrifuge, solid water wash until neutral to obtain copper quinolinate, filtrate is oxidation reaction mother liquor.
[0074] Step 2: Oxidation reaction mother liquor treatment:
[0075] Add sodium carbonate to the oxidation reaction mother liquor, adjust the pH value to neutral, then add flake caustic soda or liquid caustic soda, adjust the pH value to 10, press filter, and wash the filter cake to obtain recovered basic copper carbonate.
[0076] The recovery of basic copper carbonate is ap...
Embodiment 3
[0088] A production method of quinolinic acid is carried out according to the following steps:
[0089] Step 1. Oxidation reaction to prepare copper quinolinate:
[0090] Add 1750kg of water, 100kg of copper oxide and 410kg of concentrated sulfuric acid to the reactor, stir, keep at 55℃ for 2h, then add 250kg of quinoline to the reactor, add dropwise sodium chlorate solution with a concentration of 46wt% at 100℃ 1560kg, dripping time is 18h, after dripping, keep at 105℃ for 5h, then cool to 25℃, keep for 2h, centrifuge, solid water wash until neutral to obtain copper quinolinate, filtrate is oxidation reaction mother liquor.
[0091] Step 2: Oxidation reaction mother liquor treatment:
[0092] Add sodium carbonate to the oxidation reaction mother liquor, adjust the pH value to neutral, then add flake caustic soda or liquid caustic soda, adjust the pH value to 10, press filter, and wash the filter cake to obtain recovered basic copper carbonate.
[0093] The recovery of basic copper car...
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