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Method for producing 2-chloropyridine and 2,6-dichloropyridine with inorganic solvent process

A technology of inorganic solvent and dichloropyridine, which is applied in the field of producing 2-chloropyridine and 2 by inorganic solvent method, can solve the problems of low economic benefit, by-products, and difficult source of 2-hydroxypyridine, and achieve high economic value and easy separation effect

Inactive Publication Date: 2014-02-05
山东谦诚工贸科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The source of 2-hydroxypyridine is difficult, and phosgene needs to be introduced, so the operability is not good, and it is not conducive to environmental protection
[0013] The raw materials are easy to obtain, but there are protective gases such as nitrogen and carbon dioxide and catalysts, high process requirements, by-products, low single-pass yield, etc., and low economic benefits

Method used

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  • Method for producing 2-chloropyridine and 2,6-dichloropyridine with inorganic solvent process
  • Method for producing 2-chloropyridine and 2,6-dichloropyridine with inorganic solvent process
  • Method for producing 2-chloropyridine and 2,6-dichloropyridine with inorganic solvent process

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Embodiment 1

[0030] Pyridine and deionized water are mixed according to the mass ratio of 0.8:1 to prepare 20Kg of pyridine aqueous solution, and the pyridine aqueous solution is vaporized to make vaporized product; the vaporized product and chlorine gas are mixed according to the mass ratio of 1.5:1. The amount of feed is sent to the quartz reactor at a rate of 5Kg / h to make it react under the irradiation of an ultraviolet lamp. The reaction pressure is controlled at -0.3 to -0.5KPa, and the reaction temperature is controlled at 310-340°C. cooling to obtain the reaction solution; neutralize the pH value of the reaction solution to 10 with sodium hydroxide solution, then distill the reaction solution to obtain a mixed solution of organic matter and water; leave the mixed solution to separate layers, take out the organic phase, and then The organic phase was rectified under the condition of -0.08 to -0.085MPa, and the fractions in the temperature range of 110-113°C were collected to obtain 9...

Embodiment 2

[0032] Pyridine and deionized water are mixed according to the mass ratio of 0.3:1 to prepare 20Kg of pyridine aqueous solution, and the pyridine aqueous solution is vaporized to make vaporized product; the vaporized product and chlorine gas are mixed according to the mass ratio of 5:1 to obtain The amount of feed is sent to the quartz reactor at a rate of 8Kg / h to make it react under the irradiation of an ultraviolet lamp. The reaction pressure is controlled at -0.3 to -0.5KPa, and the reaction temperature is controlled at 260-290°C. cooling to obtain the reaction solution; neutralize the pH value of the reaction solution to 10 with sodium hydroxide solution, then distill the reaction solution to obtain a mixed solution of organic matter and water; leave the mixed solution to separate layers, take out the organic phase, and then The organic phase was rectified under the condition of -0.08 to -0.085MPa, and the fractions in the temperature range of 110-113°C were collected to o...

Embodiment 3

[0034] Pyridine and deionized water are mixed according to the mass ratio of 0.5: 1 to prepare 20Kg of pyridine aqueous solution, and the pyridine aqueous solution is vaporized to make vaporized product; the vaporized product and chlorine gas are mixed according to the mass ratio of 3: 1 to obtain The amount of feed is sent to the quartz reactor at a rate of 6Kg / h to make it react under the irradiation of an ultraviolet lamp. The reaction pressure is controlled at -0.3 to -0.5KPa, and the reaction temperature is controlled at 280-300°C. cooling to obtain the reaction solution; neutralize the pH value of the reaction solution to 10 with sodium hydroxide solution, then distill the reaction solution to obtain a mixed solution of organic matter and water; leave the mixed solution to separate layers, take out the organic phase, and then The organic phase was rectified under the condition of -0.08 to -0.085MPa, and the fractions in the temperature range of 110-113°C were collected to...

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Abstract

The invention discloses a method for producing 2-chloropyridine and 2,6-dichloropyridine with an inorganic solvent process. The method comprises the following steps: mixing pyridine with water to form a pyridine water solution, and vaporizing the pyridine water solution to prepare a vaporized substance; mixing the vaporized substance with chlorine and introducing into a reactor to react, and cooling to prepare a reaction solution after the reaction is finished; adjusting the pH (potential of Hydrogen) value of the reaction solution to 9-11, and steaming the organic substance out to prepare the mixed solution of the organic substance and the water; (4) standing the mixed solution to layer, taking an organic phase out, rectifying with the organic phase, collecting a fraction within the temperature range of 110-113 DEG C to obtain the 2-chloropyridine, and collecting the fraction within the temperature range of 142-146 DEG C to obtain the 2,6-dichloropyridine. According to the method, direct chlorination of the pyridine can be performed under the conditions of no protective gas, no added noble metal catalyst and no high pressure, the yield is high, and the main byproduct, namely the 2,6-dichloropyridine, of the process is also an important chemical raw material, is easy to separate and has higher economic value.

Description

technical field [0001] The invention relates to a method for producing 2-chloropyridine and 2,6-dichloropyridine by an inorganic solvent method. Background technique [0002] Pyridine is an important organic chemical raw material. Pyridine and its derivatives are widely used in medicine and pesticides due to their high efficiency, spectrum and low residue characteristics. Pyridine chloride is an important drug intermediate. 2-Chloropyridine is used in the production of shampoo and is widely used in the field of daily chemicals; The raw material of the medicine. 2. 6-Dichloropyridine has a great potential for development. Synthesis of drug intermediates is used as a fungicide, synthesis of Pirozadil is used to lower blood lipids and anti-platelet aggregation drugs; synthesis of muskpyridine, etc. [0003] The synthesis of 2-chloropyridine began in 1891. With the continuous improvement of experimental conditions and the gradual improvement of chemical theory, many new synthe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/61
CPCC07D213/61
Inventor 单永华孟庆浩
Owner 山东谦诚工贸科技有限公司
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