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One-step process for producing tetrachloropyridine in high content

A technology of tetrachloropyridine and pyridine, which is applied in the field of one-step production of tetrachloropyridine

Inactive Publication Date: 2007-01-03
HAINING QIANJIANGHUIGU JINGHUA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Other patents, such as CN 1160334C, also reported that pyridine catalytic chlorination can produce a certain amount of 2,3,5,6-tetrachloropyridine, but due to the wide distribution of pyridine chlorination products, it is impossible to directly prepare more than 90% of 2 in one step. 3,5,6-tetrachloropyridine products

Method used

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  • One-step process for producing tetrachloropyridine in high content
  • One-step process for producing tetrachloropyridine in high content

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Load the catalyst 2% FeCl in the reaction tube 3 -3% CuCl 2 -6% BaCl 2 / C 35g (the content of the active ingredient is the mass percentage, the same below), feed nitrogen, and adjust the gas space velocity to 500h -1 , heat the temperature of the reaction tube to 380°C and keep it warm for 1.5h, then heat the reaction tube to 390°C, pass in chlorine gas to activate the catalyst, raise the temperature of the reaction tube to 420°C after 1h, and preheat and vaporize the pyridine Add the reaction tube with a metering pump to make it react with chlorine gas. The preheating temperature of pyridine is 160° C., n (pyridine): n (nitrogen): n (chlorine)=1:8:12. The reaction product was directly cooled to a white solid powder. The product is analyzed by high-performance liquid chromatography. The mass percentage of pentachloropyridine is 11-12%, 2,3,5,6-tetrachloropyridine is 87-88%, and there are about 0.5% trichloropyridine and dichloropyridine Chloropyridine, no raw mater...

Embodiment 2

[0013] Load the catalyst 1% AlCl in the reaction tube 3 -3% FeCl 3 -4% CuCl 2 -5% BaCl 2 / C 35g, feed nitrogen, adjust the gas space velocity to 800h -1 , heat the temperature of the reaction tube to 400°C and keep it warm for 1 hour, then pass chlorine gas at 400°C to activate the catalyst, after 1.5 hours, lower the temperature of the reaction tube to 390°C, and add the preheated vaporized pyridine to the reaction with a metering pump The tube is mixed with chlorine gas for reaction, wherein the preheating temperature of pyridine is 170° C., n (pyridine): n (nitrogen): n (chlorine) = 1:6:10. The reaction product was directly cooled to a white solid powder. The product is analyzed by high-performance liquid chromatography. The mass percentage of pentachloropyridine is 8.5-9.5%, 2,3,5,6-tetrachloropyridine is 90-91%, and there are about 0.5% trichloropyridine and dichloropyridine. Chloropyridine, no raw material pyridine remains. Afterwards, the preheated and vaporized p...

Embodiment 3

[0015] Load the catalyst 5% FeCl in the reaction tube 3 -4%AlCl 3 -4% BaCl 2 / C 35g, feed nitrogen, adjust the gas space velocity to 1000h -1 , heat the reaction tube temperature to 370°C and keep it warm for 1h, then heat the reaction tube to 380°C and pass chlorine gas to activate the catalyst, after 1h, lower the temperature of the reaction tube to 350°C, and measure the preheated and vaporized pyridine The pump is added to the reaction tube to mix with chlorine gas for reaction, wherein the preheating temperature of pyridine is 160°C, n (pyridine): n (nitrogen): n (chlorine) = 1:7:8.5, and the reaction product is directly cooled to a white solid powder . The product is analyzed by high-performance liquid chromatography. The mass percent content of pentachloropyridine is 4-5.5%, 2,3,5,6-tetrachloropyridine is 93-94%, and there are about 2-6% trichloropyridine And dichloropyridine, pyridine remains about 1%. Afterwards, the preheated and vaporized pyridine is continuous...

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Abstract

The present invention is one-step process for producing 2, 3, 5, 6-tetracloropyridine with chlorine gas and pyridine as material in a fixed catalyst bed. The process uses supported solid catalyst with carrier of great specific surface area silica or active carbon and three or four active components selected from aluminum chloride, copper chloride, iron chloride and barium chloride. Chlorine gas and pyridine in the molar ratio of 4.5-12 are preheatd to 160-180 deg.c and reacted at 340-420 deg.c while using nitrogen gas to regulate gas space velocity in 500-1000 / hr. The product contains 2, 3, 5, 6-tetracloropyridine in 87-99.5 wt%.

Description

Technical field: [0001] The invention relates to a new process for producing tetrachloropyridine in one step. Background technique: [0002] 2,3,5,6-tetrachloropyridine, referred to as tetrachloropyridine, the English name is 2,3,5,6-tetrachloropyridine, the molecular formula is C 5 HCl 4 N, the structural formula is: [0003] [0004] The molecular weight of 2,3,5,6-tetrachloropyridine is 216.87, and its appearance is white or light yellow powder or crystal. Melting point is 90-91°C, boiling point is 251-252°C, slightly soluble in water and alcohol. [0005] 2,3,5,6-Tetrachloropyridine is a very important pesticide and pharmaceutical intermediate, widely used in the production and preparation of various herbicides, fungicides and insecticides, especially for the production of new high-efficiency, low-toxicity pesticides The key intermediate of insecticide chlorpyrifos and herbicide triclopyr. Because the chlorpyrifos and triclopyr produced by this product have the c...

Claims

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Application Information

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IPC IPC(8): C07D213/61
Inventor 曾楚怡马炎夏晓明裘国寅谭慧孙杰黎小兵
Owner HAINING QIANJIANGHUIGU JINGHUA
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