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Method for preparing pentachloropyridine from DCTF rectifying short steaming residues

A technology of pentachloropyridine and chloropyridine, which is applied in the field of preparing pentachloropyridine from DCTF rectification and short-distillation residue, which can solve the problems of difficult harmless treatment, non-combustibility or flammability, etc.

Inactive Publication Date: 2016-01-13
YANCHENG INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since the substances in this rectification short-distillation residue are mostly substituted pyridine compounds and their polymers containing multiple halogen atoms in the molecular structure, these substituted pyridine compounds and their polymers containing multiple halogen atoms do not have The flammability or flammability is extremely low, so it is difficult to perform harmless disposal by simple incineration

Method used

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  • Method for preparing pentachloropyridine from DCTF rectifying short steaming residues
  • Method for preparing pentachloropyridine from DCTF rectifying short steaming residues
  • Method for preparing pentachloropyridine from DCTF rectifying short steaming residues

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Experimental program
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Effect test

Embodiment 1

[0014]1000 grams of DCTF rectification short-distillation residue and 100 grams are made of aluminum oxide, silicon dioxide, zirconia, 4A zeolite, magnesium oxide, mordenite, and HZSM-5 zeolite in a mass ratio of 0.01: 30: 10: 20: 10 : The catalyst composed of 0.01:0.1 is added into the reactor together, stirred and under the conditions of 0.01MPa vacuum degree and 400°C, the in-situ catalytic cracking and vacuum distillation of the DCTF rectification and short distillation residue are realized, so that the The polymers formed by the chloropyridine compounds, fluorochloropyridine compounds and fluoropyridine compounds in the residue under high temperature conditions are converted into pentachloropyridine, 2,5,6-trichloro-3-trifluoromethane Basepyridine, 2,3-dichloro-5-trichloromethylpyridine, 2,3,4,6-tetrachloro-5-trifluoromethylpyridine, 2,3,6-trichloro-5-(two Chlorofluoromethyl)pyridine, 2,3,6-trichloro-5-(difluorochloromethyl)pyridine, 5,6-dichloro-3-hydroxymethylpyridin-2-...

Embodiment 2

[0016] 1000 grams of DCTF rectification short-distillation residue and 50 grams of aluminum oxide, silicon dioxide, zirconia, 4A zeolite, magnesium oxide, mordenite, and HZSM-5 zeolite are in a mass ratio of 0.1:2:1:0.1:3 : The catalyst composed of 0.1:0.01 is added into the reactor together, stirred and under the conditions of 0.05MPa vacuum degree and 350°C, the in-situ catalytic cracking and vacuum distillation of the short-distillation residue of DCTF rectification are realized, so that the short-distillation residue present in DCTF rectification The polymers formed by the chloropyridine compounds, fluorochloropyridine compounds and fluoropyridine compounds in the residue under high temperature conditions are converted into pentachloropyridine, 2,5,6-trichloro-3-trifluoromethane Basepyridine, 2,3-dichloro-5-trichloromethylpyridine, 2,3,4,6-tetrachloro-5-trifluoromethylpyridine, 2,3,6-trichloro-5-(two Chlorofluoromethyl)pyridine, 2,3,6-trichloro-5-(difluorochloromethyl)pyri...

Embodiment 3

[0018] 1000 grams of DCTF rectification short-distillation residue and 10 grams are made of aluminum oxide, silicon dioxide, zirconia, 4A zeolite, magnesium oxide, mordenite, and HZSM-5 zeolite in a mass ratio of 1: 0.2: 1: 0.01: 15 : The catalyst composed of 10:10 is added into the reactor together, stirred and under the conditions of 0.09MPa vacuum degree and 300 ℃ to realize the in-situ catalytic cracking and vacuum distillation of the DCTF rectification short distillation residue, so that the short distillation residue present in the DCTF rectification short distillation The polymers formed by the chloropyridine compounds, fluorochloropyridine compounds and fluoropyridine compounds in the residue under high temperature conditions are converted into pentachloropyridine, 2,5,6-trichloro-3-trifluoromethane Basepyridine, 2,3-dichloro-5-trichloromethylpyridine, 2,3,4,6-tetrachloro-5-trifluoromethylpyridine, 2,3,6-trichloro-5-(two Chlorofluoromethyl)pyridine, 2,3,6-trichloro-5-(...

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Abstract

Pentachloropyridine is a pesticide and medicine intermediate. A method for preparing pentachloropyridine from DCTF rectifying short steaming residues can improve the resource utilization rate. The method comprises the following steps: converting polymers in the residues through in situ catalytic cracking and vacuum distillation by using the catalytic degradation function of a catalyst formed by alumina, silica, zirconia, 4A zeolite, magnesium oxide, mordenite and HZSM-5 zeolite on the polymers in the DCTF rectifying short steaming residues in order to form micro-molecular compounds and obtain pentachloropyridine-containing crude oil; and washing the pentachloropyridine-containing crude oil by using an aqueous solution of an alkaline assistant formed by sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate, ammonium bicarbonate and sodium hydroxide, carrying out reduced pressure rectification, carrying out refrigerating crystallization, carrying out vacuum filtration or centrifuging separation, carrying out solvent washing, and carrying out vacuum drying treatment to obtain a pentachloropyridine product with the mass percentage content being greater than 95% at a yield being 1-15% of the mass of the DCTF rectifying short steaming residues.

Description

technical field [0001] The method for preparing pentachloropyridine by using DCTF rectification and short-distillation residue involved in the present invention is a novel method for realizing resource utilization of chemical by-products in the field of fine organic synthesis in the field of fine organic chemicals. Background technique [0002] DCTF, the chemical name is 2,3-dichloro-5-trifluoromethylpyridine, the CAS number is 69045-84-7, and it is a colorless and transparent liquid with a relative density of 1.55 (water is 1.0) at room temperature. As an important pesticide and pharmaceutical intermediate, DCTF can not only be used in the production of fluorinated herbicides such as fluazifop-p-p, chlorofluroxyfop, and haloxyfop-p Fluazuron and other fluorine-containing benzoylurea insecticides and high-efficiency fungicides such as fluazinam are also widely used in the production of pesticides and fluorine-containing medicines. These agrochemicals produced with DCTF as o...

Claims

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Application Information

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IPC IPC(8): C07D213/61
CPCC07D213/61
Inventor 蔡照胜闵邓昊丁成朱雪梅张怀红
Owner YANCHENG INST OF TECH
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