Method for recycling recycled N,N'-dicyclohexylurea

A technology of dicyclohexylurea and cyclohexylamine, which is applied in chemical instruments and methods, preparation of amino compounds, preparation of organic compounds, etc., can solve the problems of high production cost, poor safety, low yield and the like, and achieves easy separation, low cost effect

Active Publication Date: 2016-03-30
SHANDONG HUIHAI PHARMA & CHEM
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  • Claims
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Problems solved by technology

[0005] The purpose of the present invention is to provide a method for recycling N,N'-dicyclohexyl urea by ...

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  • Method for recycling recycled N,N'-dicyclohexylurea

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Embodiment 1

[0018] Add 2000kg of N,N'-dicyclohexylurea and 800kg of sodium hydroxide to the reaction kettle, start stirring, raise the temperature to 230°C, and control the temperature at 230-240°C, and keep it warm for 6h. 1750kg of cyclohexylamine products were distilled, with a yield of 99.15% and a purity of 99.77%.

Embodiment 2

[0020] Add 2000kg of N,N'-dicyclohexylurea and 1000kg of sodium hydroxide to the reaction kettle, start stirring, raise the temperature to 270°C, and control the temperature at 270-280°C, and keep it warm for 5h. 1758kg of cyclohexylamine products were distilled, with a yield of 99.25% and a purity of 99.53%.

Embodiment 3

[0022] Add 2000kg of N,N'-dicyclohexylurea and 1200kg of sodium hydroxide to the reaction kettle, start stirring, raise the temperature to 340°C, and control the temperature at 340-350°C, and keep it warm for 3h. 1754kg of cyclohexylamine products were distilled, with a yield of 99.385% and a purity of 99.59%.

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Abstract

The invention relates to a method for recycling recycled N,N'-dicyclohexylurea. The method comprises the steps of adding N,N'-dicyclohexylurea and sodium hydroxide into a reaction still, starting stirring, raising temperature to 80-450 DEG C and reacting for 2-8 hours to steam out yielded fluid of cyclohexane in a reaction process. The method has the advantages that the N,N'-dicyclohexylurea of a bio-polypeptide condensing agent by-product is recycled to achieve reclamation of wastes, the problem that the industrialization of the N,N'-dicyclohexylurea is hard to be processed is solved, and the regeneration from the N,N'-dicyclohexylurea to cyclohexylamine to N,N'-dicyclohexylcarbodiimide is achieved, a solvent is not used, and the shortcomings that an organic solvent is flammable and combustible and high in cost are overcome, the yield of the cyclohexylamine is larger than 99%, the purity is larger than 99.3%, raw materials only have the N,N'-dicyclohexylurea and the sodium hydroxide, the products are only cyclohexylamine and sodium carbonate, and the cyclohexylamine and the sodium carbonate can be separated easily. The method is safe and environmentally friendly, low in cost and suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of treatment of biological polypeptide condensing agent by-products, and in particular relates to a method for reusing recovered N,N'-dicyclohexylurea. Background technique [0002] N,N'-dicyclohexyl urea is a white powdery solid, mainly used as a by-product of biological polypeptide condensing agent DCC. At present, there are StevensCL, SinghalGA, AshAB.Carbodiimidesdehydrationofureas.TheJournalofOrganicChemistry.1967,32:2895 and Chen Fener. Improvement of the preparation method of hexylcarbodiimide. Chemical reagents, 1992,14 (1): disclosed in 54 with p-toluenesulfonyl chloride / pyridine, phosphorus pentoxide / pyridine, benzenesulfonyl chloride / triethylamine etc., in addition Use the method of phosphorus oxychloride / liquid caustic soda to convert N,N'-dicyclohexylurea into N,N'-dicyclohexylcarbodiimide. [0003] The above several methods utilizing N,N'-dicyclohexyl urea to synthesize N,N'-dicyclohexylcarbodiimide, t...

Claims

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Application Information

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IPC IPC(8): C07C209/62C07C211/35
CPCC07C209/62C07C211/35
Inventor 张国辉张忠政殷福东李华振张世凤
Owner SHANDONG HUIHAI PHARMA & CHEM
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