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Method for synthesis of N-substituted dicarbamate with urea as carbonyl source

A diurethane and nitrogen-substituted technology, which is applied in the field of polyurea degradation and synthesis of nitrogen-substituted diurethanes, can solve the problems of catalyst deactivation, loss, and poor reusability, and achieve high atom utilization and low Effect of deactivation and reduction of operating costs

Inactive Publication Date: 2017-02-15
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

However, in this process, the catalyst is easily deactivated, the loss is serious, and the reusability is poor.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0020] 1) Preparation of copper-zinc composite oxide catalyst—co-precipitation method

[0021] Copper nitrate and zinc nitrate were used as precursors, 1.5 mol / L sodium carbonate precipitant was titrated to pH = 9-11, the precipitate was aged at 70 °C for 12 hours, the obtained precipitate was washed with distilled water several times until neutral, and dried at 80 °C for 12 hours. Hours, 300-700 ℃ roasting, powdery solids are obtained, marked as xCuO-yZnO-Z, where x ranges from 0.5 to 2, y ranges from 0.5 to 2, and Z represents the roasting temperature.

Embodiment 1

[0023] Add 114 g of butanediamine polyurea, 90 g of industrial grade urea, 8.2 g of the above-mentioned CuO-ZnO-500 catalyst, and 1750 mL of ethanol into a 5L stainless steel reaction kettle, close the reactor, purging with nitrogen, and raise the temperature to 200 °C for 20 h , purging with nitrogen during, control the nitrogen flow rate 20 L / h, after the reaction solution is cooled, the catalyst is recovered by filtration, the resulting product is added to the internal standard biphenyl, quantitatively analyzed by the internal standard method, the conversion rate of the obtained polyurea is 93 %, the selectivity of N-substituted diurethane is 98%.

Embodiment 2

[0025] 142g of hexamethylenediamine polyurea, 90g of industrial grade urea, 8.2g of the above-mentioned CuO-ZnO-500 catalyst, 1750mL of ethanol were added to a 5L stainless steel reactor, and the reactor was sealed. After the reaction solution was cooled, nitrogen was purged during the period, and the nitrogen flow rate was controlled to 20 L / h. The catalyst was recovered by filtration, and the resulting product was added to the internal standard biphenyl. Quantitative analysis by the internal standard method showed that the conversion rate of the polyurea obtained was 92%. , The selectivity of N-substituted diurethane is 96%.

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Abstract

The invention discloses a method for synthesis of N-substituted dicarbamate with urea as a carbonyl source; the method comprises the steps of taking a non precious metal composite oxide as a catalyst, taking polyurea, urea and alcohol as raw materials, and carrying out a reaction at the temperature of 180-220 DEG C for 10-22 hours to obtain N-substituted dicarbamate; an active component of the catalyst is a complex of two non precious metal oxides of zinc, copper, titanium and niobium. The method has the advantages of high conversion rate, high yield, high catalyst activity and good stability, and can be reused.

Description

technical field [0001] The invention relates to a method for synthesizing nitrogen-substituted diurethane by degrading polyurea with urea as a carbonyl source under the action of a non-noble metal composite oxide catalyst. Background technique [0002] Urethane is an important class of fine chemicals, which can be used as intermediates in organic synthesis, and react with functional groups such as unsaturated hydrocarbons, aldehydes, ketones, polyols and aromatic rings to generate derivatives for various purposes, such as isocyanate, polyurethane, Dialkyl carbonate, melamine derivatives and various heterocyclic compounds. At the same time, such compounds can also be used as intermediates for modification of pesticides, medicines and synthetic resins, such as antibacterial drugs, anticancer drugs, insecticides, herbicides, etc. In addition, in the field of peptide and combinatorial chemistry, carbamate is also an effective amine protecting group and functional group linker. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C269/00C07C271/20C07C271/24C07C271/28B01J23/80B01J23/20
CPCC07C269/00B01J23/20B01J23/80C07C271/20C07C271/24C07C271/28
Inventor 邓友全李庆贺王培学刘士民费玉清马祥元何昱德卢六斤
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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