A continuous production device and production method for synthesizing 2,2'-bipyridine
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A production device and a technology for bipyridine, applied in 2 fields, can solve the problems of low single-pass conversion rate of pyridine, no practical application value, low reaction production efficiency, etc., to facilitate control of reaction conditions, realize high-efficiency production process, and improve stability. and operational safety
Active Publication Date: 2020-09-25
HEFEI UNIV OF TECH
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But the production efficiency of these two kinds of fixed-bed reactors is low, the operation is complicated, the equipment is expensive, and has no practical application value
[0006] In summary, relatively few devices have been reported for the continuous production of direct coupling synthesis of 2,2'-bipyridine, and they all have the disadvantages of low conversion rate of pyridine per pass, low reaction production efficiency, etc. The 2,2'-bipyridine can easily lead to catalyst poisoning, so these devices have no practical industrial production application value
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Embodiment 1
[0080] Example 1: Loading method Pd@γ-Al 2 o 3 Metal nanocatalysts catalyze reactions
[0081] (1) Catalyst
[0082] The Pd content in the catalyst is 23%.
[0083] (2) Catalytic synthesis of 2,2'-bipyridine
[0084] Carry out according to aforementioned device and operation process (a), catalyst consumption is 20g. with O 2 The pressure of the reaction system was adjusted to 15Mpa; the temperature of the preheater was 300°C, the reaction temperature was 800°C, and the delivery rate of pyridine was 40ml / min, so that the yield of 2,2'-bipyridine was 5%.
Embodiment 2
[0085] Example 2: Loading method Pd-Cu@γ-Al 2 o 3 Metal nanocatalysts catalyze reactions
[0086] (1) Catalyst
[0087] The Pd content in the catalyst is 23%, Pd:Cu=3:1 (molar ratio).
[0088] (2) Catalytic synthesis of 2,2'-bipyridine
[0089] Carry out according to aforementioned device and operation process (a), catalyst consumption is 20g. with O 2 The pressure of the reaction system was adjusted to 15Mpa; the temperature of the preheater was 300°C, the reaction temperature was 800°C, and the delivery speed of pyridine was 40ml / min, so that the yield of 2,2'-bipyridine was 8%.
Embodiment 3
[0090] Example 3: Loading method Pd-Ni@γ-Al 2 o 3 Metal nanocatalysts catalyze reactions
[0091] (1) Catalyst
[0092] The Pd content in the catalyst is 23%, Pd:Ni=2:1 (molar ratio).
[0093] (2) Catalytic synthesis of 2,2'-bipyridine
[0094] Carry out according to aforementioned device and operation process (a), catalyst consumption is 20g. with O 2 The pressure of the reaction system was adjusted to 15Mpa; the temperature of the preheater was 300°C, the reaction temperature was 800°C, and the delivery speed of pyridine was 40ml / min, so that the yield of 2,2'-bipyridine was 28%.
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Abstract
The invention relates to a continuous production device for synthesizing 2,2'-dipyridyl and a production method. The production device comprises a reaction system, wherein the reaction system comprises a fixed bed reactor for synthesizing 2,2'-dipyridyl from pyridine through direct coupling; a pyridine conveying system and a gas carrying system are connected with the inlet of the fixed bed reactor; a product condensation separation system and a circulation system which is for feeding back unreacted pyridine into the pyridine conveying system are sequentially connected with the outlet of the fixed bed reactor; the product condensation separation system comprises a condenser A and a gas-liquid separator which are arranged in sequence; a membrane separator for separating product hydrogen is mounted at a gas phase outlet of the gas-liquid separator; a recycling system for recycling the product, namely the 2,2'-dipyridyl, is connected with a liquid-phase outlet of the gas-liquid separator;the outlet of the recycling system is connected with the circulation system. By adopting the continuous production device, the conversion per pass of the 2,2'-dipyridyl is greatly increased, high-efficiency production process can be achieved, and a technique is provided for continuous industrial direct-coupling production of 2,2'-dipyridyl.
Description
technical field [0001] The invention belongs to the technical field of 2,2'-bipyridine synthesis, in particular to a continuous production device and production method for synthesizing 2,2'-bipyridine. Background technique [0002] In recent years, the technology of direct coupling synthesis of 2,2'-bipyridine with pyridine has received extensive attention, and a large number of studies have been carried out, but the method of direct coupling synthesis of 2,2'-bipyridine generally has a single-pass conversion rate of It is relatively low, and the production efficiency is also low, and the direct coupling production of 2,2'-bipyridine in a batch tank reactor is limited in industrial application. Therefore, various direct coupling synthesis 2,2'-bipyridine continuous production devices have been reported both at home and abroad. [0003] A variety of direct coupling synthesis 2,2'-bipyridine continuous production devices have been reported at home and abroad, mainly including...
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