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Method for synthesizing alkyl pyrroles

A technology for alkyl pyrroles and compounds, which is applied in the field of synthesizing alkyl pyrroles, can solve problems such as the synthesis of alkyl pyrroles that are not involved, and achieves the effects of high added value of products, simple and convenient operation process, and mild reaction conditions

Inactive Publication Date: 2016-06-15
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0031] In summary, the existing patents and published documents do not involve the synthesis of alkylpyrrole compounds under the combined action of plasma and catalysts using a mixture of methanol and ammonia as a raw material.

Method used

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  • Method for synthesizing alkyl pyrroles
  • Method for synthesizing alkyl pyrroles
  • Method for synthesizing alkyl pyrroles

Examples

Experimental program
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Effect test

Embodiment 1

[0070] Catalyst MnSiO 2 (20-40 mesh), with a loading capacity of 5%, filled in the discharge area of ​​the single-dielectric barrier discharge-wire barrel reactor, and the filling height is 50mm. At a pressure of 0.1MPa, ammonia gas and gaseous methanol are passed into the discharge area at a molar ratio of 4:1. After the gas flow is stable, the plasma power supply is turned on for dielectric barrier discharge. A cylindrical reactor made of quartz glass (also used as a barrier medium), in which the outer diameter of the outer tube is 11mm, the inner diameter is 9mm, the central electrode is stainless steel with a diameter of 2mm, the ground electrode is aluminum foil, and the distance between the two electrodes is 4mm. The effective discharge of the reactor The length is 50mm, the reactor structure, such as figure 1 shown.

[0071] The discharge parameters of the reactor are: discharge voltage 14.2kV, discharge power 36W, discharge frequency 12kHz, discharge zone temperature...

Embodiment 2

[0073] Repeat embodiment 1, fill the prepared CrSiO in the discharge area 2 The catalyst has a loading capacity of 5%, the particle size of the catalyst is 20-40 mesh, and the discharge zone temperature is 480-485°C. Then the reaction result is: the conversion rate of methanol is 53%. Product selectivity: formazan 9%, propionitrile 4%, N,N-dimethylaminoacetonitrile 7%, N,N-dimethylcyanamide 13%, aminoacetonitrile 7%, 2,3,5-tris Methyl pyrrole 3%, formamide 3%, methane 31%, CO 11%.

Embodiment 3

[0075] Repeat embodiment 1, fill the prepared ZnSiO in the discharge area 2 The catalyst has a loading capacity of 5%, the particle size of the catalyst is 20-40 mesh, and the discharge zone temperature is 486-487°C. Then the reaction result is: methanol conversion rate 67%, product selectivity: formazan 11%, propionitrile 3%, N,N-dimethylcyanamide 15%, aminoacetonitrile 7%, 2,3,5-trimethylcyanamide 1% pyrrole, 2%, 2,3,4,5-tetramethylpyrrole, 8% formamide, 23% methane, 28% CO.

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Abstract

The invention aims to provide a method for synthesizing high-added-value alkyl pyrroles from methanol and ammonia by a one-step process. The method is characterized in that a non-equilibrium plasma-catalyst coupled mode is adopted to activate the raw materials methanol and ammonia so as to obtain the alkyl pyrroles. The method has the advantages of cheap and accessible reaction raw materials, mild reaction conditions, and simple and convenient operating technique. The conditions can be further regulated to synthesize methyl isonitrile, N,N-dimethyl cyanamide, aminoacetonitrile, N,N-dimethyl aminoacetonitrile and the like. The invention provides a novel method for preparing high-added-value chemicals by converting methanol. Besides, the method is suitable for synthesizing high-added-value nitrogenous compounds from one or two of methanol, ethanol and propanol and ammonia gas in the presence of the dielectric barrier plasma and catalyst.

Description

technical field [0001] The invention belongs to the technical field of synthesis of alkylpyrrole compounds. Specifically, it relates to a method for synthesizing alkylpyrrole compounds under the condition of dielectric barrier discharge plasma and catalyst synergistic action by using methanol and ammonia as raw materials. Background technique [0002] Pyrrole is a nitrogen-containing five-membered heterocyclic compound, which has the properties of weak acid, weak base and aromatic ring. Pyrrole was first extracted from coal tar and bone oil, and it was mainly separated from the tar fraction into solid pyrrole potassium salt. Pyrrole compounds have good biological activity and pharmaceutical activity, and are widely used in organic synthesis, pharmaceutical industry and flavor and perfume industry. Among them, 2,5-dimethylpyrrole can be used as spices, food additives, organic synthesis intermediates, and can also be used for ethylene polymerization to produce 1-hexene. 2,3...

Claims

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Application Information

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IPC IPC(8): C07D207/323C07C291/10C07C253/00C07C255/25C07C261/04C07C1/20C07C9/04C07C255/03C07C231/10C07C233/03C07C209/02C07C211/04C07D213/06
CPCC07C1/20C07C209/02C07C231/10C07C253/00C07C261/04C07C291/10C07D207/323C07D213/06C07C255/25C07C9/04C07C255/03C07C233/03C07C211/04
Inventor 郭洪臣王旬旬易颜辉王丽于晓蕾张睿祝全仁闫金辉
Owner DALIAN UNIV OF TECH
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