Preparation method of 2-chloropyridine

A technology of chloropyridine and pyridine, which is applied in the field of preparation of 2-chloropyridine, can solve the problems of low conversion rate, long route, three waste pollution, etc., reduce the chance of secondary chlorination, improve conversion rate and selectivity, increase The effect of dwell time

Inactive Publication Date: 2010-09-15
YANCHENG HUAOU IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are many synthesis routes of 2-chloropyridine, and the industrial synthesis technology mainly includes the following four types according to the raw material routes: one is the multi-step substitution method, in which one of the raw materials of the reaction, sodium amide, is a first-class flammable, explosive , not in contact with air and water, the biggest problem with this method is that there are many steps and the conversion rate is low
The second is the pyridine N-oxide method, which is to react pyridine with hydrogen peroxide to generate pyridine N-oxide, then react with chlorine gas to generate 2-chloropyridine N-oxide, and obtain 2-chloropyridine after reduction; This method is a traditional synthetic method, the technology is mature and simple, but the route is lengthy, there are certain three wastes pollution, and the yield is low
The third is the 2-hydroxypyridine method. The 2-hydroxypyridine is chlorinated with chlorinating agents such as thionyl chloride and phosphorus pentachloride, and the hydroxyl group and the chlorine atom undergo a displacement reaction to obtain 2-chloropyridine. The process of the method is simple, but the raw material The source of 2-hydroxypyridine is limited
Although this method shortens the process flow compared with the original gas-phase photochlorination method, the operation of the reaction process is easy to control, the total yield is improved, and the waste liquid discharge is reduced, but it still needs further improvement.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] After mixing 790g of pyridine with 360ml of water (at a molar ratio of 1:2.0), add activator ammonia, the molar ratio of pyridine and ammonia is 1:0.15, and they are input into a heat exchanger together to be vaporized by steam. Pyridine and chlorine gas enter the glass reactor together, and the molar ratio of pyridine and chlorine gas is 1:0.7, and the chlorination reaction is carried out in the light chlorination area by the initiation of an ultraviolet light source with a wavelength of 426nm; the glass reactor is provided with a spiral Glass tube packing, the diameter of the spiral glass tube is 6.5mm, and the pitch is 18cm, which can quickly collect the 2-chloropyridine liquid generated by the reaction downwards, reducing the chance of 2-chloropyridine being secondary chlorinated, and greatly increasing The residence time of the raw material in the reactor is controlled at 3 to 5 seconds, which improves the conversion rate and selectivity of the raw material; the rea...

Embodiment 2

[0015] After mixing 790g of pyridine and 504.ml of water (according to the molar ratio of 1:2.8), add the activator ammonia gas, the molar ratio of pyridine and ammonia gas is 1:0.2, and input them together into the heat exchanger for vaporization by steam. The final pyridine enters the glass reactor together with chlorine, and the molar ratio of pyridine and chlorine is 1:0.78, and the chlorination reaction is carried out by the initiation of the ultraviolet light source with a wavelength of 426nm in the photochlorination area; Spiral glass tube filler, the diameter of the spiral glass tube is 7.5mm, and the pitch is 22cm, which can quickly collect the 2-chloropyridine liquid generated by the reaction downwards, reducing the chance of 2-chloropyridine being secondary chlorinated, and greatly The residence time of raw materials in the reactor is increased, controlled at 4 to 5 seconds, and the conversion rate and selectivity of raw materials are improved; the reaction mixture p...

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Abstract

The invention provides a preparation method of 2-chloropyridine. The method comprises the following steps of: mixing pyridine and water by a molar ratio of 1:(1.5-3.6) and adding an activating agent; vaporizing, then leading the pyridine and the water into a glass reactor by a molar ratio of 1:(0.70-0.80) to carry out a chlorination reaction for 3-5 seconds at 150-170 DEG C in the presence of an ultraviolet light source and carrying out cooling and gas-liquid separation on an obtained reaction mixture; absorbing the separated gas phase to form hydrochloric acid by using water; and neutralizing the separated liquid phase and then distilling to obtain pyridine, 2-chloropyridine and 2,6-dichloropyridine, wherein distilled water is applied to the production of a next batch. Because the activating agent is added in the process of the chlorination reaction, activation energy and reaction temperature which are required by the chlorination reaction are reduced, and the process period is shortened. By adopting the glass reactor with a built-in helical filler and the ultraviolet light source the wavelength of which is matched with the glass reactor, the probability of secondary chlorination of the 2-chloropyridine is reduced, and the conversation rate and the selectivity of raw materials are improved.

Description

technical field [0001] The invention relates to a preparation method of chemical products, in particular to a preparation method of 2-chloropyridine. Background technique [0002] 2-Chloropyridine is a colorless or light yellow transparent liquid, insoluble in water, soluble in ether, ethanol, chloroform and other organic solvents, is an important special fine chemical intermediate, mainly used in the synthesis and Additives for daily chemical products have important applications in the pyridine organic synthesis industry. [0003] At present, there are many synthesis routes of 2-chloropyridine, and the industrial synthesis technology mainly includes the following four types according to the raw material routes: one is the multi-step substitution method, in which one of the raw materials of the reaction, sodium amide, is a first-class flammable, explosive , not in contact with air and water, the biggest problem with this method is that there are many steps and the conversio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/61
Inventor 陈汝祝
Owner YANCHENG HUAOU IND
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