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Method for preparing piperidine and piperidine derivative

A technology for derivatives, piperidine, which is applied in the field of hydrogenation to prepare piperidine and piperidine derivatives, can solve the problem of high price of raw material pyridine, improve selectivity and production capacity, increase processing capacity, and reduce preheating and cooling. Effect

Inactive Publication Date: 2011-06-15
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the price of raw material pyridine is higher

Method used

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  • Method for preparing piperidine and piperidine derivative

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The catalyst used is Pd-Ru / Al 2 o 3 . Catalyst weight composition is: Pd=0.5% and Ru=0.003%, the rest is carrier Al 2 o 3 . The carrier adopts commercial Al 2 o 3 , and the catalyst active component Pd and additive Ru were loaded on the carrier Al by the conventional impregnation method 2 o 3 (Al 2 o 3 The particle size is 20-40 mesh). 5.0 grams (about 8ml) of the catalyst was activated by hydrogen before the reaction, and the activation conditions were: GHSV=2500h -1 , Atmospheric pressure, 300°C, reduction time 5 hours. Choose a fixed bed reactor. The reaction temperature is 150°C, the hydrogen pressure is 8.0MPa, pyridine / H 2 The molar ratio is 1:150, and the liquid space velocity of pyridine is 0.5h -1 , H 2 The reaction time is 50 hours (h), and samples are taken for analysis. Samples were analyzed by gas chromatography, HP-15 capillary column, and FID detector.

Embodiment 2

[0020] The liquid space velocity of ethanolamine is 0.35h -1 , other conditions are identical with embodiment 1.

Embodiment 3

[0022] The liquid space velocity of ethanolamine is 0.65h -1 , other conditions are identical with embodiment 1.

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Abstract

The invention discloses a method for preparing piperidine and a piperidine derivative. A reaction system consists of the piperidine, or the piperidine derivative, hydrogen and a catalyst; the reaction temperature is between 100 DEG C and 200 DEG C; the reaction pressure is between 1.0 MPa and 10.0 MPa; the liquid space velocity of the piperidine or the piperidine derivative is between 0.05 h<-1> and 2.5 h<-1>; the molar ratio of H2 to the piperidine or the piperidine derivative is 100-250; the catalyst takes Al2O3, active carbon, ZrO2 or SiO2 as a carrier; a load active component can be one or more of Pd, Ni, Cu, Fe, Co, Ru or / and TiO2; and the piperidine or the piperidine derivative can be transformed into piperidine and alkyl piperidine products respectively at high activity and high selectivity under the action of a catalyst.

Description

technical field [0001] The present invention relates to a method for preparing piperidine and piperidine derivatives by hydrogenation using pyridine or pyridine derivatives as raw materials, specifically a method for directly using pyridine or alkylpyridines (such as 2-picoline, 2 , 4-lutidine and 3,5-lutidine) as raw materials (without any solvent), hydrogenation is converted into piperidine and alkylpiperidine (such as 2-methylpiperidine, 2,4- Dimethylpiperidine and 3,5-dimethylpiperidine) method. technical background [0002] Piperidine, also known as hexahydropyridine or azacyclohexane, is a colorless liquid. Has a peppery smell. Density 0.8606. Melting point -7~-9℃. The boiling point is 106°C. Soluble in water, ethanol and ether. A strong organic base that reacts with inorganic acids to form salts. Can be volatile together with steam. Piperidine is mainly used as organic synthesis raw material, pharmaceutical raw material, solvent, epoxy resin curing agent, chem...

Claims

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Application Information

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IPC IPC(8): C07D211/02C07D211/06C07D211/12
Inventor 丁云杰朱何俊金明程显波
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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