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Preparation method of meta-alkyl urea series compounds

A compound, alkyl urea technology, applied in the field of synthesis of organic compounds, can solve problems such as low product yield and purity, difficult steps to remove solvents, serious side reactions, etc., to reduce reaction costs, reduce risks, simplify the process The effect of the processing step

Inactive Publication Date: 2009-12-23
BEIJING INST OF CLOTHING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] In order to solve the serious side reactions existing in the prior art, and the low yield and purity of the product due to the extremely difficult step of removing the solvent in the post-treatment process, and the need for high-temperature and high-pressure reaction conditions, the present invention provides an economical And the method that is very easy to implement has produced high-purity partially substituted alkylurea series compounds with high yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Synthesis of N,N-diethylurea

[0045] Add 175g of urea, 250mL of diethylamine in a 1000mL four-necked bottle equipped with a stirrer, a thermometer and a reflux device, and the mol ratio of urea and amine is 1.2: 1.0; The volume ratio is 1:1. The preparation method of this water-based reaction medium is as follows: add 10g of zinc-zinc oxide complex, 8g of lead oxide-lead nitrate complex, and 2.5g of diethylammonium chloride into 250mL of pure water successively, stir to form a suspension, and The pH value is between 6 and 7.

[0046] The reaction system is stirred and heated to 60°C, and the overflowing ammonia gas is absorbed by the acid through the tail gas absorption device. After 60h, the reaction ended.

[0047] After the reaction was completed, the reactor was cooled to room temperature, and the crude product was fully dried and filtered to separate the insoluble matter. The resulting filtrate was recrystallized to obtain the pure product as white needle-like...

Embodiment 2

[0049] N,N-Dipropylurea Synthesis

[0050] Add 165g of urea, 250mL of dipropylamine in a 1000mL four-necked flask equipped with a stirrer, a thermometer and a reflux device, the molar ratio of urea and amine is 1.5:1.0; 125mL of water-based reaction medium, the volume of amine and water-based reaction medium The ratio is 2:1. The preparation method of the water-based reaction medium is as follows: add 10g of zinc-zinc oxide complex, 10g of ferric oxide-ferric chloride complex, and 1.5g of dipropylammonium chloride into 125mL of pure water in sequence, and stir to form a suspension solution with a pH between 6 and 7.

[0051] The reaction system is stirred and heated to 90°C, and the overflowing ammonia gas is absorbed by the acid through the tail gas absorption device. After 35h, the reaction ended.

[0052] After the reaction was completed, the reactor was cooled to room temperature, and the crude product was fully dried and filtered to separate the insoluble matter. The ...

Embodiment 3

[0054] Synthesis of N,N-Dibutylurea

[0055] Add 135g of urea, 250mL of dibutylamine in a 1000mL four-necked flask equipped with a stirrer, a thermometer and a reflux device, and the molar ratio of urea and amine is 1.5:1.0; 100mL of water-based reaction medium, amine and water-based reaction medium The volume ratio is 2.5:1. The preparation method of the water-based reaction medium is as follows: add 17g of zinc-zinc oxide-zinc acetate complex, 15g of stannous chloride, and 1g of dibutylammonium chloride into 100mL of pure water in turn, stir to form a suspension, and its pH The value is between 6 and 7.

[0056] The reaction system is stirred and heated to 120°C, and the overflowing ammonia gas is absorbed by the acid through the tail gas absorption device. After 24h, the reaction ended.

[0057] After the reaction was completed, the reactor was cooled to room temperature, and the crude product was fully dried and filtered to separate the insoluble matter. The resulting ...

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Abstract

The invention relates to a preparation method of meta-alkyl urea series compounds. The meta-alkyl urea series compounds is prepared by adopting urea and primary amine or secondary amine of aliphatic or alicyclic in a synthesis reactor with a water-based reaction medium at 60-180 DEG C; wherein, the water-based reaction medium comprises a liquid which can provide protons, a metal which can perform complexation with amine and strengthen the nucleophilic attack of amine or a ion of the metal, and a nonionic surfactant or a quaternary ammonium salt surfactant; the pH value of the water-based reaction medium is 5-7; the metal or the ion thereof is at least one of Zn, Sc, Ti, Zr, V, Sn, Pb and Fe and the selected ion also comprises at least one of the following negative ions: OH, Cl, SO4, NO3, CO3, HCO3, CH3COO and C2H5COO which can combine with the metal or the ion thereof. The method solves the problems of high demands for equipments, expensive raw material price, low synthesis yield and extremely expensive product price in the prior art, thus eliminating the obstruction in the industrial application of the product of the invention.

Description

technical field [0001] The invention relates to a method for synthesizing organic compounds, in particular to a method for catalytically preparing partially substituted alkylurea series compounds in a water-based system by reacting aliphatic amines with urea. Background technique [0002] Traditional nonionic surfactants have excellent equilibrium surface tension properties, but poor dynamic surface tension properties; commonly used anionic surfactants have good dynamic surface tension properties, but are prone to foaming. [0003] Partially substituted alkylurea series compounds are a new class of nonionic surfactants. Since the 1990s, the excellent effects of partially substituted alkylurea series compounds on reducing the equilibrium and dynamic surface tension have attracted widespread attention. A large number of studies have shown that partially substituted alkylurea series compounds can not only provide excellent balance and dynamic surface tension properties, but al...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C273/18C07C275/06C07C275/26
Inventor 廖青张鸣雯
Owner BEIJING INST OF CLOTHING TECH
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