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2-chloro pyridine preparation method

A technology of chloropyridine and pyridine, which is applied in the field of preparation of 2-chloropyridine, can solve the problems of lengthy route, low conversion rate, and many steps, so as to improve conversion rate and selectivity, reduce the chance of secondary chlorination, reduce The effect of reaction temperature

Pending Publication Date: 2016-02-17
山东谦诚工贸科技有限公司
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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 2-chloro pyridine preparation method. Pyridine and water are mixed according to the molar ratio of 1:1.5-3.6, an activator is added, pyridine and chlorine are fed into a glass reactor according to the molar ratio of 1:0.70-0.80 after vaporization, chlorination reaction is performed under the effect of an ultraviolet light source at the temperature of 150-170 DEG C, the reaction time is 3-5 seconds, and the reaction mixture undergoes cooling and gas-liquid separation. The separated gas phase is absorbed with water to produce hydrochloric acid, the separated liquid phase is neutralized and then is distilled to obtain pyridine, 2-chloro pyridine and 2,6-dichloro pyridine, and a water jacket is distilled out for the next batch of production. Due to the fact that the activator is added in the process of chlorination reaction, the activation energy and reaction temperature required by the chlorination reaction are reduced, and a process cycle is shortened. By the adoption of the glass reactor provided with a spiral packing in the inside and the ultraviolet light source matched with the glass reactor in wavelength, the probability that the 2-chloro pyridine is secondarily chlorinated is reduced, and the conversion rate and selectivity of the 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
CPCC07D213/61
Inventor 陈友来郝磊
Owner 山东谦诚工贸科技有限公司
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