A method for producing 2,2'-bipyridine in a membrane reactor

A technology of membrane reactor and bipyridine, which is applied in chemical instruments and methods, organic chemistry, chemical/physical processes, etc., can solve the problems of large energy consumption, difficult separation, low single conversion rate, etc., to prolong life, pyridine High conversion effect

Active Publication Date: 2020-12-04
NANJING REDSUN BIOCHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There are two main methods suitable for industrialized preparation of 2,2'-bipyridine, one is the Ullmann method (M.Tiecco et al., Communications, 1984, 736-738), using 2-halopyridine as raw material, under the action of catalyst A coupling reaction occurs to generate 2,2'-bipyridine. The advantages of this method are high conversion rate and mild reaction conditions. The disadvantage is that the amount of three wastes is large and has been gradually eliminated.
The advantage of this method is high atom utilization rate and environmental protection, but the single conversion rate is low. The patent GB897473 uses Raney nickel to prepare 2,2'-bipyridine in a Soxhlet reactor at normal pressure and 100-120 ° C. The highest The conversion rate is less than 1%; US5416217 uses loaded nickel to prepare 2,2'-bipyridine in a fixed-bed reactor at a temperature of 175-240°C and a pressure of 0.9-1.5Mpa. Although the catalyst life of this method reaches 500h, the conversion rate remains below 1%
The low conversion rate makes the separation of the product 2,2'-bipyridine and the raw material pyridine cumbersome. For example, the separation by rectification requires a lot of energy, and the difficulty of separation also restricts the industrialization of this method.

Method used

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  • A method for producing 2,2'-bipyridine in a membrane reactor
  • A method for producing 2,2'-bipyridine in a membrane reactor
  • A method for producing 2,2'-bipyridine in a membrane reactor

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Experimental program
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Effect test

Embodiment 1-6

[0034] Put 60g of Raney nickel into the reactor of the above-mentioned device for producing 2,2'-bipyridine, gaseous pyridine enters the reactor at a certain flow rate, passes through the catalyst bed, and passes through the catalyst bed at a temperature of 300-600°C. Under the catalysis of Raney nickel, the reaction produces 2,2'-bipyridine, and the reaction liquid is extracted through the gas-liquid separator; the gas generated by the reaction enters the membrane tube, and nitrogen gas is introduced into the membrane tube from the inlet tube to overflow from the lower part of the membrane tube, blowing Sweep the gas in the membrane tube, and the mixed gas is discharged from the upper part of the membrane tube.

Embodiment 7-12

[0036] In the reactor of the above-mentioned device for producing 2,2'-bipyridine, load 60g of loaded nickel, wherein the nickel content of loaded nickel is 20%, the carrier is alumina, and the specific surface area is 120-250m 2 / g, the pore volume is 0.6m 3 / g. Gaseous pyridine enters the reactor at a certain flow rate, passes through the catalyst bed, and reacts to generate 2,2'-bipyridine under the catalysis of loaded nickel. The reaction liquid is extracted through the gas-liquid separator; Nitrogen gas is introduced into the air pipe to overflow from the lower part of the membrane tube, and the gas in the membrane tube is purged, and the mixed gas is discharged from the upper part of the membrane tube.

[0037] Table 1 is the conversion rate of pyridine for different catalysts at different temperatures, pressures, flow rates, and reaction times.

[0038] Table 1

[0039]

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Abstract

The invention discloses a method used for producing 2,2'-dipyridyl using a membrane reactor. The method comprises following steps: pyridine is subjected to preheating gasification, pyridine gas is delivered into a reactor, and is delivered through a catalyst bed layer, so that 2,2'-dipyridyl is obtained under the action of a dehydrogenation catalyst; 2,2'-dipyridyl and a part of unreacted pyridineare collected via condensation using a gas-liquid separator; hydrogen gas obtained via reaction and most unreacted pyridine are delivered into a membrane pipe through a membrane porous material pipeinserted into the catalyst bed layer so as to realize separation from 2,2'-dipyridyl, nitrogen is introduced through the bottom of the membrane pipe for blowing of gas state pyridine and hydrogen, andan obtained mixed gas is discharged through the upper part of the membrane pipe. The method is high in pyridine conversion rate, instant separation of unreacted raw materials and products can be realized, and catalyst service life is prolonged.

Description

technical field [0001] The invention belongs to the fields of fine chemical industry and organic synthesis, and in particular relates to a method for preparing 2,2'-bipyridine in a membrane reactor. Background technique [0002] 2,2'-Bipyridine is an important intermediate in chemical and pharmaceutical synthesis. Due to its unique chelation effect, it can be used as a ligand for metal catalysts, a photosensitizer, and an indicator for detecting metal ions. [0003] There are two main methods suitable for industrialized preparation of 2,2'-bipyridine, one is the Ullmann method (M.Tiecco et al., Communications, 1984, 736-738), using 2-halopyridine as raw material, under the action of catalyst A coupling reaction occurs to generate 2,2'-bipyridine. The advantage of this method is high conversion rate and mild reaction conditions. The disadvantage is that the amount of three wastes is large, and it has been gradually eliminated. Another method is to use pyridine as a raw mater...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/22C07D213/127B01J8/02
Inventor 罗超然王文魁薛谊陈新春周典海
Owner NANJING REDSUN BIOCHEM CO LTD
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