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Preparation method of 2, 3-dipicolinic acid

A technology of dipicolinic acid and concentrated sulfuric acid is applied in chemical instruments and methods, alkali metal oxides/hydroxides, inorganic chemistry, etc. Good adsorption effect

Inactive Publication Date: 2021-05-14
SINOCHEM HEBEI FUHENG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

When sodium chlorate is used as an oxidant to prepare 2,3-pyridinedicarboxylic acid, chlorine and carbon dioxide will be generated during the oxidation reaction, which requires tail gas absorption treatment, resulting in an increase in the production cost of 2,3-pyridinedicarboxylic acid

Method used

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  • Preparation method of 2, 3-dipicolinic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A kind of preparation method of 2,3-pyridinedicarboxylic acid, comprises the steps,

[0023] Step (1): Add 50g of quinoline with a mass fraction of 98%, 98g of concentrated sulfuric acid with a mass fraction of 98%, 160g of copper sulfate pentahydrate, and 92.8g of water into the oxidation reaction kettle, and continuously feed into the oxidation reaction kettle Oxygen, keep the pressure of the reactor at 4MPa, react at 70°C for 4h, obtain the precipitation of copper picolinate, and centrifuge to obtain filter cake A and mother liquor B;

[0024] Step (2): Mix 50g of water, the filter cake A, and 31g of sodium hydroxide into an alkali fusion kettle, react at 90°C for 1 hour, and filter while hot with a plate and frame filter press to obtain filter cake C and filtrate D ;

[0025] Step (3): Add the filtrate D into the neutralization and decolorization reaction kettle, add 8 g of non-magnetic ordinary activated carbon and stir for 20 minutes, and filter to obtain filter ...

Embodiment 2

[0028] Step (1): Evaporating and concentrating the mother liquor B obtained in Example 1, cooling the evaporated water vapor, crystals precipitated in the obtained concentrated solution K, and filtering to obtain a filter cake M and a filtrate N. The filtrate N, circulating water, 3g water, 50g mass fraction are 98% quinoline, 38g mass fraction are 98% concentrated sulfuric acid, 95g copper sulfate pentahydrate, continuously feed oxygen into the oxidation reactor to keep the reactor pressure It was 4MPa, and reacted at 70°C for 4h to obtain precipitation of copper pyridine acid salt, which was centrifuged to obtain filter cake A and mother liquor B.

[0029] Step (2): Mix 50g of water, the filter cake A, and 31g of sodium hydroxide into an alkali fusion kettle, react at 90°C for 1 hour, and filter while hot with a plate and frame filter press to obtain filter cake C and filtrate D ;

[0030] Step (3): Add the filtrate D into the neutralization and decolorization reaction kett...

Embodiment 3

[0033] The difference between Example 3 and Example 1 is that in step (1), oxygen is continuously fed into the oxidation reactor to keep the pressure of the reactor at 3 MPa, and the rest of the method for preparing the finished product of 2,3-pyridinedicarboxylic acid is the same as that of Example 1.

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Abstract

The invention relates to the field of fine chemical synthesis, in particular to a preparation method of 2, 3-dipicolinic acid. According to the method, oxygen is adopted to oxidize quinoline under the reaction pressure of 2-4 MPa in the presence of sulfuric acid and copper sulfate, the finished product of 2, 3-dipicolinic acid is obtained through filtration, alkali fusion, decoloration, acid pickling and drying, waste liquid generated in the reaction can be directly applied to the production process of 2, 3-dipicolinic acid, and the yield is increased to 83% or above. According to the method, the magnetic activated carbon prepared from the cotton straw is adopted as the adsorbent to perform decoloration and impurity removal on the 2, 3-dipicolinic acid crude product, the adsorption effect is good, the 2, 3-dipicolinic acid product is a white crystal, and the product purity is as high as 99.97%.

Description

technical field [0001] The invention relates to the field of fine chemicals, in particular to a preparation method of 2,3-pyridinedicarboxylic acid. Background technique [0002] 2,3-pyridinedicarboxylic acid is an important raw material for the synthesis of pesticides, medicines and dyes. At present, there are many methods for preparing 2,3-pyridinedicarboxylic acid, mainly including quinoline oxidation method, quinoline derivative oxidation method and other substances (such as 2,3-dialdehyde pyridine and 2-methyl-3-carboxy pyridine) oxidation. Among them, the quinoline oxidation method is the most commonly used method for the synthesis of 2,3-pyridinedicarboxylic acid, and the oxidant mainly uses potassium permanganate, hydrogen peroxide, ozone, sodium chlorate and oxygen. [0003] Karlheinz Giselbrecht disclosed a kind of preparation technology (US 20020062025 A1) of a kind of 2,3-pyridine dicarboxylic acid on May 23, 2002, adopt 140g quinoline, 1770g distilled water, 2...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/80C07D213/807B01J20/20B01J20/30B01J20/28
CPCB01J20/20B01J20/28009B01J2220/4825C07D213/80C07D213/807
Inventor 任建坡李灏张兵兵李东方车立光马丹丹
Owner SINOCHEM HEBEI FUHENG CO LTD
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