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Preparation method and application for heterogeneous phase catalyst

A heterogeneous catalyst and solvent technology, applied in catalyst activation/preparation, preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of complex process, environmental pollution, expensive raw materials, etc., and achieve the effect of high yield

Active Publication Date: 2013-03-27
昆明理工大学设计研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to solve the problems of complex process, environmental pollution, expensive raw materials, and difficult recycling of catalysts in the prior art, the present invention provides a simple method for preparing recyclable heterogeneous catalysts

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 0.5g of MnO 2 Add 50ml of methanol into a 100ml hydrothermal kettle, treat in an oil bath at 100°C for 10 hours, cool the hydrothermal kettle to room temperature naturally, filter the solid after opening the kettle, wash with methanol, and dry at 60°C to obtain a heterogeneous catalyst. spare.

[0023] Accurately weigh 1.125g of methyl carbamate, 0.291g of 1,6-hexanediamine, 4.8g of methanol, and add 0.03g of the catalyst prepared above into a 100ml batch reactor, and react at 190°C for 8h; after the reaction, cool naturally After reaching room temperature, open a kettle to filter off the catalyst, distill off the solvent under reduced pressure, and crystallize the solid to obtain methyl 1,6-hexamethylenedicarbamate with a yield of 43%.

Embodiment 2

[0025] 1g of Fe 2 o 3 Add 100ml of methanol into a 200ml hydrothermal kettle, treat in an oil bath at 220°C for 1 hour, cool the hydrothermal kettle to room temperature naturally, filter the solid after opening the kettle, wash with methanol, and dry at 60°C to obtain a heterogeneous catalyst, which is ready for use .

[0026] Accurately weigh 1.5g of methyl carbamate, 0.291g of 1,6-hexamethylenediamine, 4.8g of methanol, add 0.03g of the catalyst prepared above into a 100ml batch reactor, and react at 190°C for 6h; after the reaction, cool naturally After reaching room temperature, open a kettle to filter off the catalyst, distill off the solvent under reduced pressure, and crystallize the solid as methyl 1,6-hexamethylenedicarbamate, with a yield of 52%.

Embodiment 3

[0028] 1g of Co 2 o 3 Add 100ml of methanol into a 200ml hydrothermal kettle, treat in an oil bath at 190°C for 6 hours, cool the hydrothermal kettle to room temperature naturally, filter the solid after opening the kettle, wash with methanol, and dry at 60°C to obtain a heterogeneous catalyst, which is ready for use .

[0029] Accurately weigh 2.25g of methyl carbamate, 0.582g of 1,6-hexanediamine, 9.6g of methanol, and add 0.06g of the catalyst prepared above into a 200ml batch reactor, and react at 100°C for 10h; after the reaction, cool naturally After reaching room temperature, open a kettle to filter off the catalyst, distill off the solvent under reduced pressure, and crystallize the solid as methyl 1,6-hexamethylenedicarbamate with a yield of 57%.

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PUM

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Abstract

The invention discloses a preparation method for a heterogeneous phase catalyst. The method comprises the steps of treating a mixture of one or more selected from MnO2, Fe2O3, Co2O3, NiO, CuO, ZnO, PbO and PbO2 for some time at a high temperature with a solvent, cooling the mixture, taking the mixture out, filtering, washing and drying the mixture to obtain the catalyst. The prepared catalyst can be used in synthesis of 1,6-hexamethylene-dimethylurethane, 1,6-hexamethylene-diethylurethane and 1,6-hexamethylene-dibutylurethane. In a batch reactor, 1,6-hexamethylene-dimethylurethane, 1,6-hexamethylene-diethylurethane and 1,6-hexamethylene-dibutylurethane are synthesized by using1,6-hexamethylene diamine (HDA), methyl carbamate, ethyl carbamate, butyl carbamate and a solvent such as methanol, ethanol and butanol in the presence of the catalyst. The process for preparing the catalyst is simple; the operations of the reaction are safe and simple; and yield and selectivity can reach higher than 96%.

Description

technical field [0001] The invention relates to a preparation method of a heterogeneous catalyst and applies the catalyst to the synthesis of 1,6-hexamethylene dicarbamate, belonging to the field of catalyst preparation and application. Background technique [0002] 1,6-Hexamethylenedicarbamate is an important chemical intermediate, mainly used in the synthesis of 1,6-Hexamethylenediaminoisocyanate (HDI). HDI is an important aliphatic isocyanate for the synthesis of high-grade polyurethane (PU). Compared with aromatic isocyanate, because it does not contain carbon-carbon double bonds, the polyurethane coating prepared has no yellowing, color and gloss retention, and chalking resistance. It is currently the most demanded aliphatic isocyanate, and its derived polyurethane also has the characteristics of low density, high strength, non-toxic and harmless, and heat resistance. It is widely used in aviation, textile, plastic, coating and rubber industries. [0003] The tradition...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J37/08B01J23/34B01J23/745B01J23/75B01J23/755B01J23/06B01J23/14B01J23/835C07C271/20C07C269/04
CPCY02P20/584
Inventor 赵文波韩冰李艳红刘艳娜孙彦琳覃显业
Owner 昆明理工大学设计研究院有限公司
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