Process and device for one-step air catalytic oxidation synthesis of picolinic acid type compounds

A technology for synthesizing picolinic acid and catalytic oxidation, applied in organic chemistry and other directions, can solve the problems of large pollutant discharge, low working efficiency of electrolyzer, consumption of caustic soda, etc., to reduce energy consumption, pollutant discharge, and raw material conversion rate. The effect of high product purity and avoidance of the use of oxidizing agents

Inactive Publication Date: 2014-10-22
ZHEJIANG UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the synthesis process of picolinic acid is relatively complicated, the conditions are harsh, the cost is high, and the pollutant discharge is large.
The chemical oxidation method uses nitric acid or potassium permanganate as the oxidant to oxidize picolinic acid to synthesize picolinic acid. The oxidant in this method is expensive, consumes a lot of energy, and the product has low purity and serious pollution, so it is not suitable for large-scale production.
Electrolytic oxidation method, low working efficiency of electrolytic cell, low yield and other key technical problems have not been solved, so it is still in the experimental stage
The ammonia oxidation method needs to consume liquid ammonia, which increases the production cost. On the other hand, the hydrolysis of nicotine nitrile not only consumes a large amount of caustic soda, but also produces a large amount of industrial wastewater

Method used

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  • Process and device for one-step air catalytic oxidation synthesis of picolinic acid type compounds
  • Process and device for one-step air catalytic oxidation synthesis of picolinic acid type compounds
  • Process and device for one-step air catalytic oxidation synthesis of picolinic acid type compounds

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Embodiment 1

[0036] Such as figure 1 As shown, the device of the present invention includes raw material storage tank V101, raw material preheater E101, fixed bed reactor R101, desublimator X102, cyclone separator X103, circulating compressor C101, product heat exchanger E102; raw material storage tank V101 The raw material metering pump P101 is connected to the bottom inlet of the raw material preheater E101, and the top outlet of the raw material preheater E101 is connected to the top raw material gas inlet of the fixed bed reactor R101, and the fixed bed reactor R101 is filled with V 2 o 5 / TiO 2 Catalyst, the bottom of the fixed bed reactor R101 is provided with a reaction gas outlet, the reaction gas outlet is connected to the inlet of the product heat exchanger E102, the outlet of the product heat exchanger E102 is connected to the reaction gas inlet at the upper end of the desublimer X102, and the bottom of the desublimer X102 There is a first collection product outlet, an air inl...

Embodiment 2

[0053] Reaction apparatus and flow process are the same as embodiment 1, and difference is, and reaction raw material is 2-picoline, and raw material 2-picoline, water vapor and air are fed by material amount ratio 1: 50: 60, 2-methylpyridine The mass space velocity of base pyridine feed is 0.02h -1 , the follow-up steps are the same as in Example 1, and the results show that the one-way conversion rate of 2-picoline is 88%, the selectivity to product 2-pyridinecarboxylic acid is 94%, and the one-way molar yield of 2-picolinic acid is 83%. Purity up to 99.5%, CO 2 The selectivity can be controlled at ≤3.0%.

Embodiment 3

[0055] Reaction apparatus and flow process are the same as embodiment 1, and difference is, and reaction raw material is 4-picoline, and raw material 4-picoline, water vapor and air are fed by material amount ratio 1: 70: 100, 4-methylpyridine The mass space velocity of base pyridine feed is 0.5h -1 , the follow-up steps are the same as in Example 1, and the results show that the single-pass conversion rate of 4-picoline is 85%, the selectivity to the product isonicotinic acid is 91%, the single-pass molar yield of isonicotinic acid is 77%, and the purity of isonicotinic acid reaches 99.5%. % for CO 2 The selectivity can be controlled at ≤3.0%.

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Abstract

The invention discloses a process for one-step air catalytic oxidation synthesis of picolinic acid type compounds, particularly picolinic acid type compounds comprising 2-picolinic acid, nicotinic acid and isonicotinic acid. According to the process, a continuous fixed bed reactor is adopted, air or oxygen-rich air is adopted as an oxidant, methylpyridine is prepared by one-step oxidation under the action of a catalyst and is then subjected to desublimation to obtain a picolinic acid product, and after the product in reaction gas is separated, the reaction gas is returned to the reactor, reacts and is recycled. The process has advantages of simple process operation, low raw material cost, high yield, low energy consumption, capability of being free of generation of harmful waste gas and waste liquid in the preparation process, capability of being widely used for industrial production of the picolinic acid, and the like.

Description

technical field [0001] The invention relates to the technical field of chemical intermediate synthesis, in particular to a method for synthesizing picolinic acid compounds by one-step air catalytic oxidation. Background technique [0002] 2-pyridinecarboxylic acid, nicotinic acid and isonicotinic acid are all important organic synthesis intermediates. Among them, 2-pyridinecarboxylic acid can be used to prepare carbocaine drugs and neurological drugs, and is widely used in nerve suppression and local anesthesia, and can also be used to synthesize 2-pyridinecarboxylic acid salts and herbicides; Vitamin B 3 , There are dozens of drugs produced with niacin as an intermediate, and it is also used in the synthesis of niacinamide, nicotinamide, niacin triazine, herbicides and insecticides; isonicotinic acid is mainly used for the production of antibiotics Isoniazid, a tuberculosis drug, is also used to synthesize derivatives such as amides, hydrazides, and esters. [0003] At p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/807C07D213/80C07D213/79
CPCC07D213/79C07D213/80C07D213/807
Inventor 陈银飞卢晗锋刘华彦夏智军胡小波姜木根姜胜男
Owner ZHEJIANG UNIV OF TECH
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