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Synthesis proces sof N-methyl morpholine

A technology of methyl morpholine and a synthesis method is applied in the field of synthesis of organic compounds, can solve problems such as being not very suitable, and achieve the effects of easy operation, good equipment continuity and mild reaction conditions

Inactive Publication Date: 2007-11-07
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is not very suitable for fluidized bed production of small batch products such as N-methylmorpholine

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1, a kind of synthetic method of N-methylmorpholine, carries out following steps successively:

[0023] 1), preparation of supported catalyst:

[0024] a), the commercially available γ-Al 2 o 3 With a concentration of 10% H 3 PO 4 The solution was treated and soaked at 40°C-60°C for 30 minutes, then filtered out and dried, then roasted at 450°C for 3.5 hours, and at 700°C for 5 hours before use.

[0025] b) Dissolving 79.0 g of cobalt nitrate and 26.4 g of solid nickel nitrate (excluding crystal water) in 50 mL of distilled water to prepare 50 mL of metal salt solution for later use. With the ratio of 1.2mL metal salt solution / 1.0gγ-Al2O3 carrier, the above treated γ-Al2O3 was immersed in the prepared solution for 36 hours; filtered to obtain the filtrate and catalyst.

[0026] c) Dry the catalyst obtained after the above-mentioned filtration at 60°C for 2 hours under stirring, put it into a muffle furnace and bake it at 80°C, 150°C, and 280°C for 3 hour...

Embodiment 2

[0032] Embodiment 2, a kind of synthetic method of N-methylmorpholine:

[0033] In step 2), the mol ratio of morpholine and methanol is changed to 1: 6, the reaction temperature is controlled at 140°C, the hydrogen pressure is adjusted so that the reactor pressure remains at 0.5Mpa, and the raw material is used at a space velocity of 0.3g / h / mL catalyst Enter the catalyst bed layer reaction. All the other are the same as in Example 1.

[0034] The gas chromatography analysis content of the obtained product is 95%, and the product yield after recycling a batch of raw materials is 97%.

Embodiment 3

[0035] Embodiment 3, a kind of synthetic method of N-methylmorpholine:

[0036] In step 2), the mol ratio of morpholine and methanol is changed to 1: 1, the reaction temperature is controlled at 200°C, the hydrogen pressure is adjusted so that the reactor pressure remains at 0.2Mpa, and the raw material is 0.1g / h / mL catalyst space velocity Enter the catalyst bed layer reaction. All the other are the same as in Example 1.

[0037] The gas chromatography analysis content of the obtained product is 95%, and the product yield after recycling a batch of raw materials is 90%.

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Abstract

The present invention discloses synthesis process of N-methyl morpholine. The mixture of morpholine and methanol as the material after being gasified is made to pass through fixed bed containing supported catalyst to produce amination reaction under hydrogen condition; and the resultant is condensed, collected, dewatered and rectified to obtain N-methyl morpholine. The supported catalyst is prepared with metal salt solution of at least two of copper salt, nickel salt, cobalt salt, palladium salt and platinum salt and carrier and has metal accounting for 33-41 wt%. The synthesis process of the present invention can produce N-methyl morpholine of high purity in the yield up to 85 %.

Description

technical field [0001] The invention relates to a method for synthesizing organic compounds, in particular to a method for synthesizing an organic chemical intermediate - N-methylmorpholine. Background technique [0002] N-methylmorpholine is an important organic chemical intermediate, which is an excellent solvent, emulsifier, corrosion inhibitor, polyurethane foam catalyst, and can also be used as a pesticide intermediate. The synthesis methods mainly include N-methylation method using morpholine as raw material, cyclization method using diethanolamine as raw material, cyclization method using diethanolamine as raw material, and synthesis method using dichloroethane as raw material. These methods are generally catalyzed by metal catalysts and carried out at higher temperatures and pressures. The most convenient method is to use morpholine as a raw material and directly select different methylating reagents for N-methylation reaction. At present, the method for synthesizi...

Claims

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Application Information

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IPC IPC(8): C07D295/03B01J23/75B01J23/755
Inventor 陈新志张涛钱超
Owner ZHEJIANG UNIV
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