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A kind of preparation method of picolinic acid compound

A technology of picolinic acid and compounds, which is applied in the field of preparation of picolinic acid compounds, can solve the problems of high cost, heavy pollution, complicated process, etc., and achieve the effects of low cost, high yield and short process flow

Active Publication Date: 2020-07-10
河北美邦工程科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to provide a preparation method of picolinic acid compounds to solve the problems of complex process, high cost and large pollution in the existing preparation method

Method used

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  • A kind of preparation method of picolinic acid compound
  • A kind of preparation method of picolinic acid compound

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Effect test

preparation example Construction

[0030] The preparation method of picolinic acid compounds provided by the invention comprises the following steps:

[0031] Add catalysts and picoline compounds into the slurry bed reactor, and feed protective gas, start the agitator and circulation pump, establish circulation, and then feed gas oxidant into the static mixed gas, in the pre-reactor, a The base pyridine compound is oxidized by the gas oxidant in the presence of the catalyst, and the reaction is completed in the reactor to obtain the reaction solution of the picolinic acid compound. Among them, the picoline compound, protective gas and gas oxidant are all raw materials that are pretreated to the reaction temperature and pressure, and the molar ratio of the picoline compound to the oxidizing component in the gas oxidant is 1:0.05~5, The catalyst can catalyze the oxidation of picoline compounds to generate picolinic acid compounds. The mass concentration of the catalyst is 1%~8%, the reaction temperature in the re...

Embodiment 1

[0037] (1) Raw material pretreatment

[0038] Heat and pressurize 2-picoline to a temperature of 160 °C and a pressure of 1.5 MPa;

[0039] The air is formulated into air with an oxygen mass content of 20%, and then filtered and compressed to a pressure of 1.5MPa, and then preheated to 160 °C;

[0040] Compress nitrogen to a pressure of 1.5 MPa, and then preheat to a temperature of 160 °C.

[0041] (2) Oxidation reaction

[0042] The pretreated 2-picoline, prepared air, and nitrogen in step (1) are continuously sent to the slurry bed oxidation reaction system equipped with a catalyst for catalytic oxidation reaction, and the reaction liquid of 2-pyridinecarboxylic acid is generated . During the reaction process, the reaction temperature was controlled at 160 °C, the pressure was 1.5 MPa, the residence time was 30 min, the molar ratio of 2-picoline to oxygen molecules in the prepared air was 1:0.5, and the mass concentration of the catalyst was 3% (need According to the uni...

Embodiment 2

[0047] (1) Raw material pretreatment

[0048] Heat and pressurize 3-picoline to a temperature of 170 °C and a pressure of 1.6 MPa;

[0049] The air is formulated into air with an oxygen mass content of 30%, and then filtered and compressed to a pressure of 1.6MPa, and then preheated to 170 °C;

[0050] Compress nitrogen or cycle tail gas to a pressure of 1.6 MPa, and then preheat to a temperature of 170 °C. At the beginning of the reaction, nitrogen is used as a protective gas. After the reaction has been carried out for a period of time, the tail gas (mostly nitrogen, containing a very small amount of prepared air) discharged from the slurry bed oxidation reactor is recycled, that is, the circulating tail gas is heated. Autoclave to reaction temperature and pressure.

[0051] (2) Oxidation reaction

[0052] The pretreated 3-picoline, prepared air, and nitrogen (or circulating tail gas) in step (1) are continuously sent to the slurry bed oxidation reaction system equipped w...

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Abstract

The invention provides a preparation method of picolinic acid compounds. The preparation method comprises steps as follows: (1), pretreatment of raw materials: methylpyridine compounds, a gas oxidizing agent and protective gas are subjected to pressurizing and heating treatment respectively until reaction temperature and reaction pressure are reached; (2), catalytic oxidation reaction: the raw materials treated in the step (1) are fed into a slurry reactor oxidation reaction system containing a catalyst for catalytic oxidation reaction respectively, and a reaction solution of the picolinic acid compounds is produced; (3), membrane separation: the reaction solution of the picolinic acid compounds obtained in the step (2) is separated by an inorganic membrane, and a filtrate of the picolinicacid compounds is obtained. The preparation method has the advantages of mild conditions in technological process, simple operation, high efficiency, low raw material cost, high yield and low energyconsumption, is free of harmful waste gas and waste liquid in the preparation process, can be widely applied to industrial production of the picolinic acid compounds and has good economic and social benefits.

Description

technical field [0001] The invention relates to a method for preparing organic matter, in particular to a method for preparing picolinic acid compounds. Background technique [0002] 2-pyridinecarboxylic acid, nicotinic acid (3-pyridinecarboxylic acid) or isonicotinic acid (4-pyridinecarboxylic 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-picolinate and herbicides; Essential B vitamins 3 Niacin is used as an intermediate to produce dozens of drugs, and it is also used to synthesize nicotinamide, nicotinic acid triazine, herbicides and insecticides; isonicotinic acid is mainly used to prepare anti-tuberculosis drugs Niacinazine is also used to synthesize derivatives such as amides, hydrazides and esters. [0003] At present, the synthesis methods of picolinic acid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/79C07D213/80C07D213/807
CPCC07D213/79C07D213/80C07D213/807
Inventor 马东兴刘晓东赵松钊吴迪王勐王晓动王素霞宛悍东张玉新
Owner 河北美邦工程科技股份有限公司
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