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Method for preparing 2,3-dichloro-5-(dichloro fluoro methyl) pyridine through DCTF rectification short steaming residues

A technology of dichlorofluoromethyl and chloropyridine, applied in the field of preparation 2, which can solve the problems of non-combustibility or combustibility, difficulty in harmless treatment, etc.

Inactive Publication Date: 2015-11-11
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-(dichloro fluoro methyl) pyridine through DCTF rectification short steaming residues
  • Method for preparing 2,3-dichloro-5-(dichloro fluoro methyl) pyridine through DCTF rectification short steaming residues

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Experimental program
Comparison scheme
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-(dichlorofluoromethyl)pyridine, 2,3-dichloro-5-(difluorochloromethyl)pyridine, 2,5,6-trichloro-3-trifluoromethylpyridine, 2,3-dichloro-5-trichloromethylpyridine, 2,3,4,6-tetrachloro-5-trifluoromethylpyridine, 2,3,6-trichloro-5-(dichlorofluoromethyl)pyridine, 2,3,6-trichloro-5- (Di...

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-(dichlorofluoromethyl)pyridine, 2,3-dichloro-5-(difluorochloromethyl)pyridine, 2,5,6-trichloro-3-trifluoromethylpyridine, 2,3-dichloro-5-trichloromethylpyridine, 2,3,4,6-tetrachloro-5-trifluoromethylpyridine, 2,3,6-trichloro-5-(dichlorofl...

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

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Abstract

The resource utilization rate can be increased when 2,3-dichloro-5-(dichloro fluoro methyl) pyridine is prepared through DCTF rectification short steaming residues. According to the process, due to the catalytic degrading function of catalysts composed of aluminum oxide, silica, zirconia, 4A zeolite, magnesium oxide, mordenite and HZSM-5 zeolite on polymers in the DCTF rectification short steaming residues, crude oil containing the 2,3-dichloro-5-(dichloro fluoro methyl) pyridine is obtained by converting polymers in the residues into small-molecule compounds through in-place catalytic cracking and vacuum distillation; the crude oil containing the 2,3-dichloro-5-(dichloro fluoro methyl) pyridine is sequentially washed through an alkaline assistant aqueous solution, and subjected to depressurizing rectification, distillates generated at the temperature of 130-160 DEG C and at the pressure of 1.33-2.67 kPa, and the 2,3-dichloro-5-(dichloro fluoro methyl) pyridine product with the mass percentage larger than 95% can be obtained with the yield being 1-10% of the DCTF rectification short steaming residues.

Description

technical field [0001] A method for preparing 2,3-dichloro-5-(dichlorofluoromethyl)pyridine by using DCTF rectification and short-distillation residue involved in the present invention is a novel method for the preparation of fine organic chemicals in the field of fine organic synthesis. A method to achieve efficient resource utilization of chemical by-products. 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 medici...

Claims

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Application Information

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