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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

Active Publication Date: 2018-11-23
湖北金玉兰医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] But, when adopting the quinoline oxidation method of prior art to produce quinolinic acid, the yield and the purity of quinolinic acid are low, need its refining
In the production process, there are effective components in the oxidation reaction mother liquor and the acid precipitation reaction mother liquor, which are usually discharged as wastewater after treatment, and the effective ingredients are lost in vain, which not only reduces the yield of quinolinic acid, but also increases the treatment of wastewater. difficulty
The prior art also has a simple method of applying mechanically, and the oxidation reaction mother liquor is applied mechanically to the production of the next batch of quinolinic acid. However, the impurity ions in the above two mother liquors are also introduced into the reaction system, which reduces the purity of the quinolinic acid.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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PUM

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Abstract

The invention provides a quinolinic acid production method. Quinolinic acid is produced through the following steps: preparing quinoline acid copper through an oxidizing reaction, treating an oxidation reaction mother liquid, preparing quinoline acid sodium through an alkaline hydrolysis reaction, decolouring, preparing quinolinic acid through an acid separation reaction, and treating an acid separation reaction mother liquid. The oxidation reaction mother liquid, alkaline hydrolysis reaction filter cake washing water and the acid separation reaction mother liquid are comprehensively and effectively treated; active ingredients, including copper ions, quinolinic acid and the like, in each mother liquid and washing water are recycled and are utilized into the production of the next batch of the quinolinic acid; the control on an acid separation reaction is optimized, and the yield of the quinolinic acid is improved. When the active ingredients are applied, the recycled copper oxide and the recycled basic copper carbonate are purified; the yield of the quinoline acid is improved; meanwhile, the purity of the quinoline acid is ensured; refining steps of the quinoline acid are reduced; the production cost is reduced. Through the treatment of each mother liquid and the application of the washing water, water resources are saved; the wastewater discharge is reduced; the pressure on the environment is relieved.

Description

Technical field [0001] The invention relates to a method for producing chemical raw materials, in particular to a method for producing quinolinic acid, and belongs to the technical field of chemical engineering. Background technique [0002] Quinolinic acid, also known as 2,3-pyridinedicarboxylic acid, is an important intermediate of pesticides, medicines and dyes. It can be used to synthesize fluorophenethyl ether, moxifloxacin, imidazolinone herbicides, and quinolone antibiotics; nicotinic acid obtained by decarboxylation of quinolinic acid at high temperature can be used to synthesize various hypertension, skin diseases and coronary heart diseases It can also be used as a drug intermediate to synthesize inositol nicotinate, isoniazid, etc. [0003] There are many production methods of quinolinic acid, including: 1. Quinoline oxidation method, which uses quinoline as raw material. The main oxidants are potassium permanganate, hydrogen peroxide, ozone and sodium chlorate; 2. Quin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/80C07D213/803C07D213/807
CPCC07D213/80C07D213/803C07D213/807
Inventor 曾庆伟缪建军金惠军王安进
Owner 湖北金玉兰医药科技有限公司
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