Catalyst for preparing 3-trifluoromethyl pyridine

A technology of trifluoromethylpyridine and methylpyridine, which is applied in the field of preparation of 3-trifluoromethylpyridine, can solve the problems of poor selectivity of 3-trifluoromethylpyridine, large reaction energy consumption, etc., and achieves improved activity and Selectivity, low reaction temperature, the effect of improving selectivity and yield

Active Publication Date: 2015-11-04
中化蓝天氟材料有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, the selectivity of 3-trifluoromethylpyridine is poor, while generating 3-trifluoromethylpyridine, also generate a large amount of by-products 2-chloro-5-trifluoromethylpyridine, 2-chloro-3-trifluoromethylpyridine, Fluoromethylpyridine and 2,6-dichloro-3-trifluoromethylpyridine, Example 9 discloses the highest content of 3-trifluoromethylpyridine in the product, only 66.9%
At the same time, in order to achieve a better implementation effect, this method needs to maintain the range temperature at 400-430°C, and the reaction consumes a lot of energy.

Method used

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  • Catalyst for preparing 3-trifluoromethyl pyridine
  • Catalyst for preparing 3-trifluoromethyl pyridine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Example 1 Catalyst preparation

[0032] The inner diameter of the reaction tube is 19mm, the length is 700mm, the material is stainless steel, and the catalyst filling height is 140mm. The catalyst bed is composed of 55.5%MgF 2 -40.0%Co 2 O 3 -0.55% CeO 2 (55.5%, 40%, 0.5% are the mole percentages of metal atoms, which are the ratio of the number of moles of metal atoms of each component to the total number of moles of metal atoms, the same below), the catalyst is formed into a diameter of 3mm and a height of 4mm Of the cylinder. Heat the reaction tube to 235°C, control the feed rate of anhydrous hydrogen fluoride to 10.00g / h (0.500mol / h), pass in HF for 3 hours to activate the catalyst, and then use nitrogen as the carrier gas to vaporize 3-methyl Pyridine and chlorine gas are introduced into the reaction tube. Among them, the flow rate of 3-picoline is controlled to 4.00g / h (0.043mol / h), the flow rate of chlorine is controlled to 6.0L / h (0.268mol / h), and the flow rate ...

Embodiment 2

[0037] Fill the reaction tube described in Example 1 with 55.5% MgF 2 -40%ZnO-0.5%K 2 O catalyst, the catalyst is shaped into a cylinder with a diameter of 3mm and a height of 4mm. Heat the reaction tube to 260°C, control the feed rate of anhydrous hydrogen fluoride to 10.00g / h (0.500mol / h), pass in HF for 3 hours to activate the catalyst, and then use nitrogen as the carrier gas to vaporize 3-methyl The pyridine and chlorine gas are introduced into the reaction tube. Among them, the flow rate of 3-picoline is controlled to 4.00g / h (0.043mol / h), the flow rate of chlorine is controlled to 6.0L / h (0.268mol / h), and the flow rate of nitrogen is maintained at 12.0L / h (0.536mol / h). / h). The molar feed ratio of the reactants is 3-picoline:chlorine gas:hydrogen fluoride:nitrogen=1:6.2:11.6:12.5, and the reaction is 8 hours.

[0038] The exhaust gas leaving the reaction tube was treated as in Example 1. 51.80 g of oily product was obtained, which was analyzed by gas chromatography. The...

Embodiment 3

[0043] Fill the reaction tube described in Example 1 with 77.0% MgF 2 -20.0%Bi 2 O 3 -2.0%Na 2 O catalyst, the catalyst is shaped into a cylinder with a diameter of 3mm and a height of 4mm. Heat the reaction tube to 220°C, control the feed rate of anhydrous hydrogen fluoride to 10.00g / h (0.500mol / h), pass in HF for 3 hours to activate the catalyst, and then use nitrogen as the carrier gas to vaporize 3-methyl The pyridine and chlorine gas are introduced into the reaction tube. Among them, the flow rate of 3-picoline is controlled to 4.00g / h (0.043mol / h), the flow rate of chlorine is controlled to 6.0L / h (0.268mol / h), and the flow rate of nitrogen is maintained at 12.0L / h (0.536mol / h). / h). The molar feed ratio of the reactants is 3-picoline:chlorine gas:hydrogen fluoride:nitrogen=1:6.2:11.6:12.5, and the reaction is 8 hours.

[0044] The exhaust gas leaving the reaction tube was treated as in Example 1. 51.91 g of oily product was obtained, which was analyzed by gas chromatogr...

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Abstract

The invention discloses a catalyst for preparing 3-trifluoromethyl pyridine. The catalyst comprises a main catalyst, a first catalyst promoter and a second catalyst promoter. The catalyst for preparing the 3-trifluoromethyl pyridine, disclosed by the invention, is high in selectivity, safe to operate and environmentally friendly.

Description

Technical field [0001] The invention relates to a catalyst for the preparation of 3-trifluoromethylpyridine and a preparation method of 3-trifluoromethylpyridine. Background technique [0002] 2-Chloro-5-trifluoromethylpyridine and 2-chloro-3-trifluoromethylpyridine are both very important fluorine-containing pyridine chemical raw materials. 2-Chloro-5-trifluoromethylpyridine (abbreviated as 2,5-CTF) is an important trifluoromethylpyridine intermediate used in the preparation of pharmaceuticals, agrochemicals and biological preparations. It prepares many compounds with special purposes, such as: 2-amino-5-trifluoromethylpyridine, 2-hydroxy-5-trifluoromethylpyridine, 2-mercapto-5-trifluoromethylpyridine, 2,3 -Dichloro-5-trifluoromethylpyridine and the like. In terms of pesticides, 2-chloro-5-trifluoromethylpyridine is used to produce the insecticide acetamiprid, the high-efficiency herbicide diflufenop-p-ethyl (trade name Jingwenshade) and oxypentalop-p-ethyl and high-efficiency...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/138B01J27/132B01J27/128C07D213/26
Inventor 于万金徐娇刘武灿
Owner 中化蓝天氟材料有限公司
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