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Method for synthesizing N-methylpiperazine

A technology of methylpiperazine and a synthesis method, which is applied in the field of chemical synthesis of chemical products, can solve the problems that the production cost is difficult to reduce, can only reach 50%, and the replacement cost is high, and achieves obvious technological advancement, reduced energy consumption, and reduced production costs. The effect of cost reduction

Active Publication Date: 2008-08-13
安徽长华化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The reaction temperature of this method is as high as 300°C, the energy consumption is large, and the single-pass conversion rate can only reach 50%, there are many by-products, and the product purity is low; It is getting lower and lower, and the energy consumption is getting higher and higher. At a certain time, it can only be completely replaced. The replacement cost is very high, and the production cost is difficult to reduce.

Method used

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  • Method for synthesizing N-methylpiperazine

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Add 86 grams of piperazine (1mol) and 800 grams of methanol to a capacity of 2 liters of autoclave, start the stirrer, add 81 grams of formaldehyde (1mol) with a concentration of 37% in batches from the feeding hole, and then add 4 grams of Raney Nickel catalyst, closed autoclave.

[0018] After replacement with nitrogen and hydrogen successively, then, raise the hydrogen pressure in the kettle to 2.0Mpa, close the hydrogenation valve, keep stirring, and slowly raise the temperature of the material to 70-80°C, maintain the temperature, and keep the kettle pressure at 2.0Mpa. Mpa, carry out the hydrogenation reaction until the hydrogenation reaction is completed (without absorbing hydrogen). Cool down the reaction kettle, release the pressure, and take out the reactants.

[0019] Filter and remove the catalyst Raney nickel for the next batch of reactions. Take the filtrate, distill and recover the solvent methanol and unreacted piperazine, collect the fraction at 137°C...

Embodiment 2

[0021] Add 97.3 grams of 37% formaldehyde (1.2mol) in batches, and all the other conditions are the same as in Example 1.

Embodiment 3

[0023] Add 113.5 grams of 37% formaldehyde (1.6mol) in batches, and all the other conditions are the same as in Example 1.

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Abstract

The invention relates to a synthesis method of N-methylpiperazine and chemical synthesis methods of chemical products, particularly to a synthesis process of N-methylpiperazine using vermex, formaldehyde and hydrogen as materials. Vermex is reacted with formaldehyde under atmosphere pressure to generate a condensate, and then the condensate is reacted with hydrogen in a same reaction container and under catalysis of Raney nickel catalyst to obtain N-methylpiperazine, wherein, the hydrogenation pressure is 1.0-6.0 MPa, the hydrogenation temperature is 70-100 DEG C, the catalyst dosage is 4%-12% of vermex dosage, the reaction solvent is methanol. The method has advantages of short process, low investment, high efficiency, etc.

Description

technical field [0001] The invention relates to a chemical synthesis method of chemical products, in particular to a synthesis process of N-methylpiperazine using piperazine, formaldehyde and hydrogen as raw materials. Background technique [0002] N-Methylpiperazine is one of the derivatives of piperazine and is an important fine chemical product. It can be used in medicine to synthesize ofloxacin, levofloxacin, fleroxacin and other antibacterial drugs It is also widely used in rubber, plastic and other polymer chemical industries. [0003] At present, the product is still in the development stage in China, and there are two main synthetic methods of domestic development recorded in the literature: [0004] Method 1: first react piperazine and hydrochloric acid in absolute ethanol to generate piperazine hydrochloride, evaporate the ethanol to separate piperazine hydrochloride, then react with formaldehyde and formic acid to obtain N-methylpiperazine hydrochloride, Then ne...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/03
CPCY02P20/584
Inventor 仲高华
Owner 安徽长华化工有限公司
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