Synthetic process for N,N'-bi(3-dimethylaminopropyl)urea

A technology of dimethylaminopropyl and synthesis process, applied in the N field, can solve the problems of expensive ethylene carbonate, harsh operating conditions, high raw material cost, and achieve the effects of simple operation, less three wastes, and high product yield

Active Publication Date: 2018-07-20
ANHUI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This route can avoid the generation of ammonia, but the reaction also needs high temperature (120~140 ℃) and feeds nitrogen, and the operating conditions are harsh; and ethylene carbonate is more expensive than urea, and the cost of raw materials is high; the product also contains N-(3- Impurities such as dimethylaminopropyl) monourea and by-product ethylene glycol are difficult to remove, resulting in low product purity

Method used

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  • Synthetic process for N,N'-bi(3-dimethylaminopropyl)urea

Examples

Experimental program
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Effect test

Embodiment 1

[0028] In the present embodiment, the synthesis process of N, N'-bis(3-dimethylaminopropyl)urea is as follows:

[0029] Add 3 mol of N,N-dimethyl-1,3-propanediamine and solvent toluene to the reaction bottle, stir under cooling, control the temperature of the reaction solution below 10°C, add bis(trichloromethyl ) Carbonate 0.5mol toluene solution, drop it for 1 hour, continue to stir and react for 2 hours after dropping; then add 3mol saturated aqueous solution of potassium carbonate to neutralize, install the water separator, raise the temperature and separate the water, observe the water separator until no water comes out Cooled to room temperature, filtered, the filtrate was distilled off toluene under reduced pressure to obtain the target product N, N'-bis(3-dimethylaminopropyl)urea, the yield was 91%, and the gas chromatography analysis purity was greater than 98%. IR (cm -1 ):761,1038,1267,1636,1941,3325 have absorption peaks;

[0030] 1 H-NMR (D 2 O, ppm): 1.45-1.5...

Embodiment 2

[0032] In the present embodiment, the synthesis process of N, N'-bis(3-dimethylaminopropyl)urea is as follows:

[0033] Add 3 mol of N,N-dimethyl-1,3-propanediamine and solvent benzene into the reaction bottle, stir under cooling, control the temperature of the reaction solution below 10°C, add bis(trichloromethyl ) Carbonate 0.5mol benzene solution, drop it for 1h, continue to stir and react for 2h after dripping; then add 3mol saturated aqueous solution of potassium carbonate to neutralize, install the water separator, raise the temperature and divide the water, observe the water separator until no water comes out Cooled to room temperature, filtered, and the filtrate was distilled off under reduced pressure to remove benzene to obtain the target product N, N'-bis(3-dimethylaminopropyl) urea with a yield of 92% and a gas chromatographic analysis purity greater than 98%.

Embodiment 3

[0035] In the present embodiment, the synthesis process of N, N'-bis(3-dimethylaminopropyl)urea is as follows:

[0036] Add 3 mol of N,N-dimethyl-1,3-propanediamine and solvent toluene to the reaction bottle, stir under cooling, control the temperature of the reaction solution below 10°C, add bis(trichloromethyl ) Carbonate 0.5mol toluene solution, drop it for 1 hour, continue to stir for 2 hours after dropping; then add 3mol saturated aqueous solution of sodium carbonate to neutralize, install the water separator, raise the temperature and separate the water, observe the water separator until no water comes out Cooled to room temperature, filtered, the filtrate was distilled off toluene under reduced pressure to obtain the target product N,N'-bis(3-dimethylaminopropyl)urea, the yield was 90%, and the gas chromatography analysis purity was greater than 98%.

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Abstract

The invention discloses a synthetic process for N,N'-bi(3-dimethylaminopropyl)urea. The synthetic process comprises the following steps: firstly dissolving N,N'-dimethyl-1,3-diaminopropane in an organic solvent, reacting with bi(trichloromethyl)carbonate to obtain hydrochloride of the N,N'-bi(3-dimethylaminopropyl)urea; and adding alkaline liquor for neutralizing, so as to obtain an N,N'-bi(3-dimethylaminopropyl)urea water solution, and removing the solvent through azeotropic water separation, filtration desalination and distillation, so as to obtain a target product of the N,N'-bi(3-dimethylaminopropyl)urea. The synthetic process is high in product yield, high in purity, simple and convenient in operation, and less in three wastes, and suitable for industrial application.

Description

technical field [0001] The invention relates to a synthesis process of N,N'-bis(3-dimethylaminopropyl)urea, belonging to the technical field of organic synthesis. Background technique [0002] N, N'-bis(3-dimethylaminopropyl) urea (DPU) is a fine chemical with a wide range of uses, which can be used as a foaming agent for the synthesis of polyurethane foam plastics, and can also be used for the synthesis of diaminocarbamide Polymer (PUB), and PUB is used in the alkaline galvanizing process to improve the deposition performance of the metal. [0003] At present, the synthetic processes disclosed at home and abroad can be classified into two types: [0004] The first route is to use urea to react with N,N-dimethyl-1,3-propanediamine. The process requires high temperature (120-140°C) and nitrogen gas, which will increase energy consumption and cost, and the reaction will Ammonia gas with a pungent odor is released and there is a risk of polluting the environment. If the crud...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C273/18C07C275/14
CPCC07C273/1809C07C273/1863C07C273/189C07C275/14
Inventor 潘忠稳张庭兰李阳阳
Owner ANHUI UNIVERSITY
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