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Synthetic method of HDU

A technology of methyl hexamethylene diaminodicarboxylate and synthesis method, which is applied in the preparation of carbamate derivatives, chemical instruments and methods, preparation of organic compounds, etc., to achieve the effect of simple synthesis route

Inactive Publication Date: 2013-01-16
太仓市运通化工厂
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] According to literature reports, zinc acetate has good catalytic properties when used to prepare aromatic carbamates, but it is used to synthesize hexamethylene diaminodicarbamic acid methyl ester (HDU) by DMC aminolysis, but there is no literature report

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] In a three-necked flask equipped with a condenser tube and a thermometer, according to the amount of substances, dimethyl carbonate: 1,6-hexamethylenediamine=2:1, zinc acetate: 1,6-hexamethylenediamine=0.01:1, add 1,6-Hexamethylenediamine, dimethyl carbonate and catalyst zinc acetate were heated and stirred at 332K under reflux for 4 hours, and the low-boiling substance methanol was distilled off under reduced pressure to obtain methyl hexamethylenedicarbamate.

Embodiment 2

[0016] In a three-necked flask equipped with a condenser tube and a thermometer, according to the amount of substances, dimethyl carbonate: 1,6-hexanediamine=7:1, zinc acetate: 1,6-hexanediamine=0.05:1, add 1,6-Hexamethylenediamine, dimethyl carbonate and catalyst zinc acetate were heated and stirred at 364K to reflux for 9 hours, and the low-boiling substance methanol was distilled off under reduced pressure to obtain methyl hexamethylenedicarbamate.

Embodiment 3

[0018] In a three-necked flask equipped with a condenser tube and a thermometer, according to the amount of substances, dimethyl carbonate: 1,6-hexanediamine=4:1, zinc acetate: 1,6-hexanediamine=0.03:1, add 1,6-Hexamethylenediamine, dimethyl carbonate and catalyst zinc acetate were heated, stirred and refluxed at 350K for 6 hours, and the low-boiling substance methanol was distilled off under reduced pressure to obtain methyl hexamethylenedicarbamate.

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PUM

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Abstract

The invention discloses a synthetic method of HDU. The synthetic method comprises the following steps of: adding 1, 6-hexamethylenediamine, dimethyl carbonate and catalyst zinc acetate to a three-necked flask which is provided with a condensing pipe and a thermometer according to weight ratios of materials: the dimethyl carbonate to the 1, 6-hexamethylenediamine is 2 to 7: 1 and the zinc acetate to the 1, 6-hexamethylenediamine is 0.01 to 0.05: 1; heating and agitating and carrying out a reflux reaction for 4 to 9 hours at 332 to 364K; then evaporating a low-boiling point material namely methanol through a pressure reduction way, so as to obtain the HDU. Compared with a traditional synthetic method of the HDU, the synthetic method disclosed by the invention is simple in synthetic route, a transformation rate of the 1, 6-hexamethylenediamine is up to 92%, and yield of the HDU is up to 82%.

Description

technical field [0001] The invention belongs to the field of organic chemical synthesis, in particular to a method for synthesizing methyl hexamethylene diaminodicarboxylate. Background technique [0002] Hexamethylene-1,6-diisocyanate (HDI) belongs to aliphatic diisocyanate (ADI) and is one of the high-grade raw materials for preparing polyurethane. At present, the phosgene method commonly used in industrial production has many shortcomings such as serious environmental pollution, highly toxic raw material phosgene, and difficulty in removing residual chlorine in the product, which affects product performance. Therefore, the HDI non-phosgene clean production process has become a research hotspot at present, among which the dimethyl carbonate (DMC) amination method is currently a more promising HDI green production process. [0003] The process is divided into two processes, the first is DMC aminolysis to synthesize hexamethylene dicarbamate, and then thermal decomposition ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C271/20C07C269/04
Inventor 张卫东
Owner 太仓市运通化工厂