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Method for synthesizing methenamine and N,N-dimethylcyanamide

A methanol and two-pole technology, applied in the field of plasma chemical synthesis, can solve the problems of low yield, high cost, and no involvement of dimethyl cyanamide, and achieve the effects of convenient operation, strong applicability, and mild conditions

Inactive Publication Date: 2015-08-19
DALIAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Its disadvantage is: it can only be synthesized with high-quality formaldehyde as raw material, and the cost is relatively high
The yield of dimethylcyanamide is very low
[0038] The above-mentioned publications and invention patents do not relate to the synthesis of N,N-dimethylcyanamide with methanol and NH3 as raw materials

Method used

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  • Method for synthesizing methenamine and N,N-dimethylcyanamide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Embodiment 1 (double dielectric barrier discharge --- wire cylinder reactor)

[0064] At a pressure of 0.2MPa, the temperature of the grounded water electrode is 90°C, ammonia gas and gaseous methanol are mixed at a molar ratio of 4:1, and after the gas flow is stable, the plasma power supply is turned on for dielectric barrier discharge. A cylindrical reactor made of hard glass (also used as a barrier medium), in which the outer diameter of the outer tube is 11mm, the inner diameter is 9mm, the outer diameter of the inner tube is 4mm, the inner diameter is 2mm, the center electrode is aluminum powder, and the grounding pole is a cylinder with a wall thickness of 3mm shaped water electrode. The effective discharge length of the reactor is 50mm.

[0065] The discharge parameters of the reactor are: discharge voltage 18kV, discharge power 60w, frequency 12kHz. Then the reaction result is: methanol conversion rate 57%, product selectivity: ethanol: 6%, formamide 5%, N,N-...

Embodiment 2

[0067] Repeat Example 1, change the reaction blocking medium to ceramic, discharge voltage: 18kV, power 57w, frequency: 12kHz. Then the reaction result is: methanol conversion rate 49%, product selectivity: ethanol: 9%, formamide 7%, N,N-dimethylcyanamide 21%, N,N-dimethylaminoacetonitrile 8%, Aminoacetonitrile 3%, urotropine 20%, ethylene glycol 9%, 1H-1,2,4-triazole 4%, methane 13% and hydrogen.

Embodiment 3

[0069] Repeat Example 1, change the discharge voltage of reaction, voltage 9kv, power 27w, frequency 12kHz; Then reaction result is: methanol conversion rate 23%, the selectivity of product: ethanol: 10%, formamide 11%, N,N- Dimethylcyanamide 16%, N,N-dimethylacetonitrile 7%, aminoacetonitrile 3%, urotropine 26%, ethylene glycol 13%, methane 11% and hydrogen.

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Abstract

The present invention provides a method for synthesizing nitrogen-containing organic matters with high added values by virtue of a one-step method by activating methanol and ammonia gas molecules by means of a non-equilibrium plasma technology, namely a method for synthesizing methenamine and N,N-dimethylcyanamide. The method provided by the present invention has the advantages of low price of reaction raw materials and abundant sources, and belongs to one-step method synthesis. Moreover, the method provided by the invention has the advantages of being environmental-friendly, mild in condition, convenient to operate, simple in process, high in adaptability and the like, and can be used for synthesizing ethanol, formamide, ethanamide, aminoacetonitrile, N,N-dimethylcyanamide, glycol and 1H-1,2,4-triazole by further changing the condition. In addition, the method is suitable for synthesizing the nitrogen-containing compounds with high added values by any one or two of methanol, ethanol and propanol and the ammonia under the condition of non-equilibrium plasmas.

Description

technical field [0001] The invention belongs to the technical field of plasma chemical synthesis, and relates to a method for synthesizing urotropine and N,N-dimethylcyanamide by using methanol and ammonia as raw materials under non-equilibrium plasma conditions. Background technique [0002] The molecular formula of urotropine is (CH 2 ) 6 N 4 , Widely used in the field of medicine and military fuel. In the field of medicine, urotropine can be used to produce chloramphenicol, and can also be taken directly or externally to play a bactericidal effect. In addition, urotropine can also be used as a curing agent for resins and plastics, a vulcanization accelerator (accelerator H) for rubber, and an anti-shrinkage agent for textiles. [0003] N,N-Dimethylcyanamide is a colorless liquid with the molecular formula C 3 h 6 N 2 , molecular weight M=70.11, is an important organic synthesis intermediate, mainly used in pharmaceutical synthesis. [0004] The following descripti...

Claims

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Application Information

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IPC IPC(8): C07D487/18C07C261/04
CPCC07C261/04C07D487/18
Inventor 郭洪臣王旬旬张睿王丽于晓蕾易颜辉
Owner DALIAN UNIV OF TECH
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