Method for preparing pyridine-2-carbonitrile by using 2-OP rectification residue

A 2-OP and rectification technology, applied in organic chemistry and other fields, can solve the problems of large energy consumption and ineffective utilization of resources

Active Publication Date: 2019-01-22
YANCHENG INST OF TECH
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Problems solved by technology

For the residues generated during these rectification processes, the existing treatment methods are as hazardous solid wastes, which are treated as hazardous solid wastes through high-temperature incineration and then landfilled or mineralized. This treatment method not only consumes a lot of energy, but also It is often not possible to truly achieve the harmlessness of the distillation residue
At the same time,

Method used

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  • Method for preparing pyridine-2-carbonitrile by using 2-OP rectification residue
  • Method for preparing pyridine-2-carbonitrile by using 2-OP rectification residue
  • Method for preparing pyridine-2-carbonitrile by using 2-OP rectification residue

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Embodiment Construction

[0015] A kind of method that utilizes 2-OP rectification residue to prepare pyridine-2-carbonitrile involved in the invention is characterized in that a kind of figure 1 The pyridine-2-carbonitrile of the shown structure, by using 2-OP rectification residue as raw material, phosphorylated zeolite and / or phosphorylated silica gel as in-situ catalytic cracking catalyst, is made of aluminum oxide, zinc oxide, boric acid, cobalt acetate and The mixture composed of silicon dioxide is a catalytic dehydration catalyst, and the mixture composed of sulfamic acid, phosphorus pentasulfide, phosphorus pentoxide and bis(trichloromethyl)carbonate is a dehydrating agent. After in-situ catalytic cracking and vacuum distillation process, Processes including catalytic dehydration, vacuum distillation process and rectification process are prepared.

[0016] (1) In-situ catalytic cracking and vacuum distillation process of 2-OP rectification residue: Zeolite or silica gel is soaked in 30%~80% pho...

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Abstract

According to the present invention, 2-OP rectification residue is used as a raw material, phosphorylated zeolite and/or phosphorylated silica is used as an in-situ catalytic cracking catalyst, a mixture of alumina, zinc oxide, boric acid, cobalt acetate and silica is used as a catalytic dehydration catalyst, a mixture of sulfamic acid, phosphorus pentasulfide, phosphorus pentoxide and bis(trichloromethyl)carbonate is used as a dehydration agent, and a process comprising an in situ catalytic cracking and pressure reducing distillation process, a catalytic dehydration and pressure reducing distillation process and a rectification process is performed to obtain the pyridine-2-carbonitrile product with the mass percentage of more than or equal to 99%, wherein the yield is 40-60% based on the mass of the 2-OP rectification residue.

Description

technical field [0001] The method for preparing pyridine-2-carbonitrile by using 2-OP rectification residue involved in the present invention is a novel method for resourceful and efficient utilization of chemical by-products in the field of organic synthesis for the preparation of fine organic chemicals. Background technique [0002] 2-OP, the chemical name is 2-cyanopyridine, pyridine-2-carbonitrile, 2-pyridinecarbonitrile, the CAS number is 100-70-9, it is a white to light brown needle with a melting point of 24-27°C A crystalline solid. As an important intermediate, 2-OP is widely used in the synthesis of various fine organic chemicals such as medicines, pesticides and dyes. These typical fine organic chemicals synthesized from 2-OP can show many outstanding properties: for example, the new herbicide picloram synthesized from 2-OP has low dosage, high selectivity, low toxicity, It has the characteristics of small residual amount and short residual period in soil and pl...

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Application Information

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IPC IPC(8): C07D213/84
CPCC07D213/84
Inventor 沈莉莉蔡照胜于敬华徐盼丁鸽杨中烈黄旭娟卞金玉陈云徐鹏
Owner YANCHENG INST OF TECH
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