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Method for producing hexa-methylene diamino-methyl formate with catalysis

A technology for methyl hexamethylene dicarbamate and catalytic preparation, which is applied in the preparation of carbamate, preparation of carbamate derivatives, chemical instruments and methods, etc., can solve the problem of high cost of ionic liquid, corrosion of reaction equipment, mechanical Low strength and other problems, to achieve the effect of wide and convenient source of materials, low corrosion and high mechanical strength

Inactive Publication Date: 2010-02-17
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Many catalysts have been developed in the process of synthesizing urethane from amine and dimethyl carbonate: zinc acetate powder, zirconia powder, zinc oxide powder, lead acetate powder, zinc chloride, lead chloride, ionic liquid etc., the common disadvantages of these catalysts are separation difficulties; chloride catalysts have corrosion problems to reaction equipment, and ionic liquids have disadvantages such as high cost; in addition, other supported catalysts have low mechanical strength

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In a 0.5-liter autoclave, add 50 grams of 1,6-hexanediamine (HDA), 180 grams of dimethyl carbonate (DMC), and 0.3 grams of catalyst 1Cr18Ni9Ti powder, at a temperature of 70 ° C and a pressure of 0.5 MPa And rotating speed is under 600 rev / min conditions, keep temperature, pressure and rotating speed reaction after 18 hours, obtain a mixture by hexamethylene one isocyanate one carbamate methyl ester, hexamethylene dicarbamate methyl ester and a small amount Alkylation by-product composition, chromatographic analysis hexamethylene dicarbamate methyl ester yield is 96%, separation yield is 94%, hexamethylene-isocyanate-methyl carbamate chromatographic content is 3.5% , The chromatographic content of alkylated by-products is 0.5%.

Embodiment 2

[0020] In a 0.5 liter autoclave, add 100 grams of 1,6-hexanediamine (HDA), 300 grams of dimethyl carbonate (DMC), and 1.5 grams of catalyst 1Cr18Ni9 powder, at a temperature of 70 ° C and a pressure of 0.5 MPa And rotating speed is under 600 rev / min conditions, keep temperature, pressure and rotating speed reaction after 18 hours, obtain a mixture by hexamethylene one isocyanate one carbamate methyl ester, hexamethylene dicarbamate methyl ester and a small amount Alkylation by-product composition, chromatographic analysis hexamethylene dicarbamate methyl ester yield is 96%, separation yield is 94%, hexamethylene-isocyanate-methyl carbamate chromatographic content is 3.5% , The chromatographic content of alkylated by-products is 0.5%.

Embodiment 3

[0022] In a 0.5 liter autoclave, add 100 grams of 1,6-hexanediamine (HDA), 280 grams of dimethyl carbonate (DMC), 0.9 grams of catalyst 0Cr18Ni9Ti powder, at a temperature of 70 ° C and a pressure of 0.5 MPa And rotating speed is under 600 rev / min conditions, keep temperature, pressure and rotating speed reaction after 18 hours, obtain a mixture by hexamethylene one isocyanate one carbamate methyl ester, hexamethylene dicarbamate methyl ester and a small amount Alkylation by-product composition, chromatographic analysis hexamethylene dicarbamate methyl ester yield is 96%, separation yield is 94%, hexamethylene-isocyanate-methyl carbamate chromatographic content is 3.5% , The chromatographic content of alkylated by-products is 0.5%.

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PUM

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Abstract

The invention relates to a method for catalyzing and preparing hexamethylene aminomethyl formate, which adopts 1, 6-hexamethylene diamine and dimethyl carbonate as reactant to catalyze and prepare hexamethylene aminomethyl formate by using alloy catalyst under suitable hardeness condition. The method is mild in reaction condition, easy in catalyst recycling, high in purity of the separated and obtained product and relatively less in by-product.

Description

technical field [0001] The invention relates to a method for catalytically preparing methyl hexamethylene dicarbamate. Background technique [0002] As a class of important organic reaction intermediates, isocyanates are widely used in industry, agriculture, medicine and health. These compounds are widely used in the synthesis of polyisocyanates, polyurethanes, polyureas, polymer adhesives, insecticides, herbicides, etc. Among them, 1,6-hexamethylene diisocyanate (HDI) belongs to non-yellowing aliphatic diisocyanate, which is mainly used in automotive OEM coatings and repair paints, aircraft OEM paints and repair paints, anti-corrosion coatings, wooden furniture paints, wire enamelled paints, Train refinish paint, polyurethane adhesive with good light stability and rocket propellant, etc. [0003] At present, isocyanates are mainly prepared by reacting corresponding amine compounds with phosgene. Phosgene is a highly toxic compound, and a large amount of highly corrosive ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C271/10C07C269/04C07C263/04C07C265/04
CPCY02P20/584
Inventor 邓友全石峰郭晓光田雄马祥元王利国
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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