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Method for reducing waste residues of N,N'-dicyclohexylcarbodiimide product

A technology for dicyclohexylcarbodiimide and products is applied in the field of reducing N,N'-dicyclohexylcarbodiimide product waste residue, which can solve problems such as difficult desulfurization, achieve simple and reliable control, improve appearance, and reduce production cost effect

Inactive Publication Date: 2020-03-24
SHANDONG HUIHAI PHARMA & CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] It is difficult to completely desulfurize by traditional process methods, and obtain high-purity N, N'-dicyclohexylcarbodiimide products

Method used

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  • Method for reducing waste residues of N,N'-dicyclohexylcarbodiimide product
  • Method for reducing waste residues of N,N'-dicyclohexylcarbodiimide product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add potassium carbonate accounting for 1.5% of the total material mass to the crude DCC without solvent, control the temperature at 110° C., stir for 1 h, then reduce the pressure to below -0.09 MPa, and distill under reduced pressure to obtain DCC. The purity is more than 99.63%, the yield is more than 96.5%, and the amount of waste residue is 0.7% of the mass of DCC crude product. The wastewater produced by oxidation is used as cooling circulating water after passing the MVR distillation test.

Embodiment 2

[0020] Add 1% sodium carbonate to the crude DCC without solvent, control the temperature at 100° C., stir for 1 h, then reduce the pressure to below -0.09 MPa, and distill under reduced pressure to obtain DCC. The purity is more than 99.60%, the yield is more than 95.9%, and the amount of waste residue is 0.9% of the mass of DCC crude product. The wastewater produced by oxidation is used as cooling circulating water after passing the MVR distillation test.

Embodiment 3

[0022] Add potassium carbonate accounting for 2% of the total material mass to the crude DCC without solvent, control the temperature at 120° C., stir for 1 h, then reduce the pressure to below -0.09 MPa, and distill under reduced pressure to obtain DCC. The purity is more than 99.58%, the yield is more than 96.1%, and the amount of waste residue is 1% of the mass of DCC crude product. The wastewater produced by oxidation is used as cooling circulating water after passing the MVR distillation test.

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Abstract

The invention discloses a method for reducing waste residues of an N,N'-dicyclohexylcarbodiimide product. The method comprises the following steps: adding potassium carbonate or sodium carbonate intoa crude DCC product in a solvent-free state, controlling a temperature to be 100-120 DEG C, carrying out stirring for 1 hour, controlling a pressure to be less than -0.09 MPa, and performing distilling to obtain qualified DCC. Potassium carbonate or sodium carbonate is added to increase the pH value of a reaction system, and potassium carbonate and sodium carbonate do not react with the product, so the stability of N,N'-dicyclohexylcarbodiimide is facilitated, and the N,N'-dicyclohexylcarbodiimide is prevented from being decomposed at a high temperature; the amount of waste residues produced after DCC distillation can be reduced by 50% and is 1% or less of the mass of the crude DCC product, so environmental protection investment is greatly reduced; the method is simple and reliable to control, and production cost is reduced; and meanwhile, aspotassium carbonate or sodium carbonate is used as a catalyst, the product becomes transparent and colorless from light yellow, so the appearanceof the product is improved.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a method for reducing waste residue of N,N'-dicyclohexylcarbodiimide products. Background technique [0002] N, N'-Dicyclohexylcarbodiimide, referred to as DCC, the molecular formula is: C 13 h 22 N 2 , the structural formula is: [0003] [0004] Relative molecular mass: 206.33, white to pale yellow crystalline solid or transparent liquid, melting point 33-35°C, boiling point 154-156°C (1.47KPa), insoluble in water, soluble in benzene, ethanol, ether. N,N'-Dicyclohexylcarbodiimide is mostly used in the synthesis of peptide drugs as a dehydration condensation agent, and the product purity is very high, which is difficult to meet by traditional techniques. [0005] The traditional production process of N,N'-dicyclohexylcarbodiimide is roughly as follows: [0006] The reaction of cyclohexylamine and carbon disulfide generates dicyclohexyl thiourea, and ox...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C267/00
CPCC07C267/00C07C2601/14
Inventor 付德修王磊李保铃张国辉侯绪会刘志威张忠政
Owner SHANDONG HUIHAI PHARMA & CHEM
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