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Method for preparing 2,3-dichloro-5-trichloromethylpyridine from DCTF distillation and rapid-steaming residues

A technology of trichloromethylpyridine and chloropyridine, which is applied in organic chemistry and other fields, and can solve problems such as difficult harmless treatment, non-combustibility or flammability

Inactive Publication Date: 2017-01-11
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 2,3-dichloro-5-trichloromethylpyridine from DCTF distillation and rapid-steaming residues
  • Method for preparing 2,3-dichloro-5-trichloromethylpyridine from DCTF distillation and rapid-steaming residues

Examples

Experimental program
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Effect test

Embodiment 1

[0013]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 2,3-dichloro-5-trichloromethylpyridine, 2,5 , 6-trichloro-3-trifluoromethylpyridine, 2,3,4,6-tetrachloro-5-trifluoromethylpyridine, 2,3,6-trichloro-5-(dichlorofluoromethyl ) pyridine, 2,3,6-trichloro-5-(difluorochloromethyl)pyridine, 5,6-dichloro-3-hydroxymethylpyridin-2-ol, 2,3-dichloro-5- (Dic...

Embodiment 2

[0015] 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 2,3-dichloro-5-trichloromethylpyridine, 2,5 , 6-trichloro-3-trifluoromethylpyridine, 2,3,4,6-tetrachloro-5-trifluoromethylpyridine, 2,3,6-trichloro-5-(dichlorofluoromethyl ) pyridine, 2,3,6-trichloro-5-(difluorochloromethyl)pyridine, 5,6-dichloro-3-hydr...

Embodiment 3

[0017] 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 2,3-dichloro-5-trichloromethylpyridine, 2,5 , 6-trichloro-3-trifluoromethylpyridine, 2,3,4,6-tetrachloro-5-trifluoromethylpyridine, 2,3,6-trichloro-5-(dichlorofluoromethyl ) pyridine, 2,3,6-trichloro-5-(difluorochloromethyl)pyri...

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Abstract

The invention provides a method for preparing a pesticide and medical intermediate, i.e., 2,3-dichloro-5-trichloromethylpyridine, from DCTF rectification and rapid-steaming residues so as to improve the utilization rate of resources. The method comprises the following step: in virtue of the catalytic degradation function of a catalyst composed of aluminum oxide, silicon dioxide, zirconium oxide, 4A zeolite, magnesium oxide, mordenite and HZSM-5 zeolite on polymers in DCTF distillation and rapid-steaming residues, allowing the polymers in the residues to be converted into small molecular compounds and crude oil containing 2,3-dichloro-5-trichloromethylpyridine to be obtained through in-situ catalytic cracking and vacuum distillation; subjecting the crude oil containing 2,3-dichloro-5-trichloromethylpyridine to washing with an aqueous alkaline solution containing sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate, ammonium bicarbonate and sodium hydroxide; and then carrying out pressure-reduced distillation so as to obtain the 2,3-dichloro-5-trichloromethylpyridine product with mass percentage content of more than 95% relative to the mass yield of 1 to 12% of the DCTF rectification and rapid-steaming residues.

Description

technical field [0001] The present invention relates to a method for preparing 2,3-dichloro-5-trichloromethylpyridine by using DCTF rectification short-distillation residue, which is a new type of realization of fine organic chemicals in the field of fine organic synthesis. A method for efficient utilization of by-product resources. 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 prod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/61
CPCC07D213/61
Inventor 蔡照胜丁成朱雪梅张怀红
Owner YANCHENG INST OF TECH
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