Novel laurolactam preparation method and synthesis apparatus

A technology of laurolactam and synthesis equipment, which is applied in the preparation of lactam, oxime and heterocyclic compounds, etc., to achieve the effects of high purity, high conversion rate, high selectivity and high yield

Pending Publication Date: 2021-08-06
HANWHA SOLUTIONS CORP
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  • Abstract
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Problems solved by technology

However, these various synthetic methods require a multi-step process, so when constructing an overall process system, it is necessary to study a more efficient method

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  • Novel laurolactam preparation method and synthesis apparatus

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[0035] The present invention provides a method for preparing laurolactam, a synthesis device thereof, and a system for preparing laurolactam including one or more of them. When performing each process step of the present invention, the following effects can be achieved, that is, There is no need to separate the obtained product including the target substance synthesized in each step without reacting and remaining substances, etc. in a separate process, and the above obtained product can be directly used as a reactant in the subsequent step, and the conversion rate and selectivity can reach significantly higher until the final step of the synthesis of laurolactam.

[0036] The preparation method of laurolactam of the present invention comprises: step a), utilizes catalyst to epoxidize cyclododecene to synthesize epoxidized cyclododecane; Step b), by making above-mentioned epoxidized cyclododecane performing a catalytic reaction to synthesize cyclododecanone; and step c), synthe...

Embodiment 1

[0080] Cyclododecene Synthesis Process

[0081] Utilize high-speed stirring batch type (Batch) reactor (500ml, 800rpm), the cyclododecatriene of 200g, the RuCl of 40mg 3 , 5.56g of triphenylphosphine (110:1=triphenylphosphine:Ru), 3.44g of 35% formalin (triphenylphosphine:formalin=1:2), 0.5g of acetic acid (Acetic acid), 10.54 g of ethanol were added to the reactor, and the reactor was connected. After that, use 5kg / cm 2 Nitrogen (N 2 ) purging (purge) 3 times, using hydrogen (H 2 ) after purging 3 times, the reactor pressure was increased to 10 barg. Next, increase the reactor temperature from 25°C to 145°C in about 40 minutes, if the pressure of the reactor starts to drop, raise the reactor pressure to 20bar, raise the temperature to 160°C in about 10 minutes, and carry out the reaction Keep it in the process. The reaction was carried out for a total of 6 hours, during which time hydrogen was continuously supplied in order to continue to maintain the pressure. After...

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Abstract

The present invention relates to a laurolactam preparation method and a synthesis apparatus, and epoxidation and a rearrangement reaction are carried out in the conversion of cyclododecene into cyclododecanone so that the preparation method can synthesize laurolactam having a higher purity with a higher selectivity and in a higher yield than a conventional preparation method.

Description

technical field [0001] The invention relates to a novel method and device for preparing laurolactam. Background technique [0002] Generally, the industrial method for preparing amide compounds is to transform the corresponding oxime compounds through Beckmann rearrangement reactions. For example, laurolactam can be synthesized to cyclododecanone oxime via a Beckmann rearrangement reaction. However, the process of the Beckmann rearrangement reaction is a rather complicated process, using concentrated sulfuric acid and oleum as catalysts, they are strong acids, because of the need for high content, when neutralized, a large amount of by-products of ammonium sulfate are produced, which has Limitations need to be set on the equipment used to process it. Moreover, the Beckmann rearrangement reaction is carried out in a solvent, which needs to have high solubility to cyclododecanone oxime, and does not react with the concentrated sulfuric acid and oleum as the catalyst, so its ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D201/04C07D225/02C07C5/03C07C13/273C07C45/58C07C49/307C07C249/04C07C251/44
CPCC07C249/04C07C45/58C07D225/02C07C2601/20C07C251/44C07C49/413C07D201/04C07C5/03C07C13/273C07C49/307
Inventor 金芝娟金荣镇朴正锡朴真虎徐玄邢成勋宋圭镐
Owner HANWHA SOLUTIONS CORP
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