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Method for recovering cyclohexylamine by decomposing DCU

A technology of cyclohexylamine and sulfuric acid, applied in chemical instruments and methods, preparation of organic compounds, preparation of amino compounds, etc., can solve the problems of high production cost, poor safety, low yield, etc., and achieve low cost and easy separation. Effect

Inactive Publication Date: 2019-09-10
SHANDONG HUIHAI PHARMA & CHEM
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  • Description
  • Claims
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Problems solved by technology

[0006] The purpose of the present invention is to provide a method for decomposing and reclaiming cyclohexylamine by overcoming the problems of poor safety, low yield and high production cost that are ubiquitous in the prior art

Method used

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  • Method for recovering cyclohexylamine by decomposing DCU

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Effect test

Embodiment 1

[0018] Add 200kg of DCU, 4000L of water, and 40kg of concentrated sulfuric acid into the reaction kettle, start stirring, raise the temperature to 80°C and keep it warm for 6 hours. 175kg of cyclohexylamine products were distilled, with a yield of 99.15%, a purity of 99.77%, and a moisture content of 3.2%.

Embodiment 2

[0020] Add 200kg of DCU, 1000L of water, and 80kg of concentrated sulfuric acid into the reaction kettle, start stirring, raise the temperature to 120°C and keep it warm for 2 hours. 175.8 kg of cyclohexylamine products were distilled, with a yield of 99.25%, a purity of 99.53%, and a moisture content of 3.0%.

Embodiment 3

[0022] Add 200kg of DCU, 3500L of water, and 100kg of concentrated sulfuric acid into the reaction kettle, start stirring, raise the temperature to 90°C and keep it warm for 4 hours. 175.4kg of cyclohexylamine products were distilled, with a yield of 99.385%, a purity of 99.59%, and a moisture content of 3.2%.

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Abstract

The invention relates to a method for recovering cyclohexylamine by decomposing DCU. The method comprises the following steps: adding DCU, water and sulfuric acid to a reaction bottle, starting stirring, raising the temperature to 80-120 DEG C and carrying out a reaction for 2-6 h, transferring the material into a distillation flask for distillation after the reaction is completed, and collectinga distilled product, namely cyclohexylamine. A biological polypeptide condensing agent by-product DCU is subjected to recycling and waste resource utilization, the problem that industrialization treatment of DCU is difficult is solved, and regeneration of DCU to cyclohexylamine and then to DCC is realized; no solvent is used, shortcomings that an organic solvent is inflammable and explosive, and the cost is high are avoided, the yield of cyclohexylamine is 99.10% or more, and the purity is 99.50% or more; and the raw materials are only DCU, water and sulfuric acid, and products are only cyclohexylamine and carbon dioxide, so that separation is easy, the method is safe and environment-friendly, low in cost, and suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of treatment of by-products of biological polypeptide condensing agents, and in particular relates to a method for decomposing and recovering cyclohexylamine from DCU. Background technique [0002] DCU (dicyclohexyl urea) is a white powdery solid, mainly used as a by-product of biological peptide condensation agent DCC (N,N'-dicyclohexylcarbodiimide). [0003] At present, there are Stevens CL, Singhal G A, Ash AB.Carbodiimides dehydration of ureas.The Journal of Organic Chemistry.1967,32:2895 and Chen Fen'er. Improvement of the preparation method of dicyclohexyl carbodiimide at home and abroad. .Chemical Reagents, 1992,14 (1): disclosed in 54 with p-toluenesulfonyl chloride / pyridine, phosphorus pentoxide / pyridine, benzenesulfonyl chloride / triethylamine, etc., in addition to using phosphorus oxychloride / liquid caustic soda method to convert DCU to DCC. [0004] The above several methods utilizing DCU to synthesize DC...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/62C07C211/35
CPCC07C209/62C07C2601/14C07C211/35
Inventor 张国辉赵攀峰李保铃黄明路张路军付德修
Owner SHANDONG HUIHAI PHARMA & CHEM
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