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Process for preparing N-formyl morpholine

A technology of formylmorpholine and morpholine, which is applied in the field of solvent extraction in aromatics synthesis equipment, can solve the problems of expensive catalysts, high equipment requirements, and high prices, and achieve low production energy consumption, low equipment investment, and low operating costs Effect

Active Publication Date: 2006-10-04
BC P INC CHINA NAT PETROLEUM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the strong acidity of the reaction system and serious corrosion, it is necessary to use expensive corrosion-resistant equipment. At the same time, waste water is generated during the production process, and formic acid is likely to remain in the product, which is corrosive
[0005] The carbon monoxide carbon-based synthesis method uses CO as an acylating agent, which is rich in raw materials and low in price, but it can only be realized under high temperature and high pressure conditions, and requires the use of expensive catalysts. The process is complicated, the equipment requirements are high, and the investment is large.

Method used

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  • Process for preparing N-formyl morpholine
  • Process for preparing N-formyl morpholine
  • Process for preparing N-formyl morpholine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～5

[0041] like figure 1 As shown, 1 stirring reactor; 2 reaction reflux condenser; 3 catalyst filter; 4 middle tank; 5 batch rectification tower; 6 return condenser; 7 reflux tank; Buffer tank; 11 vacuum pumps. Refer to the schematic diagram of the batch production process of N-formylmorpholine ( figure 1 ), add metered morpholine and transesterification catalyst in stirring reaction kettle 1, under vigorous stirring, slowly add metered methyl formate, control reaction temperature and pressure to reach required requirement, react certain time, obtain crude product .

[0042] The reaction kettle is used as a rectifying kettle at this time, and the heating coil inside the reaction kettle is used for heating, and a batch rectifying tower 5 (theoretical plate number: 35) is used in combination to carry out product separation.

[0043] The operating pressure of the methyl formate separation and recovery process is 0.2Mpa, the temperature of the reactor 1 is 68-82°C, and the methyl ...

Embodiment 6～10

[0048] figure 2 21 static mixer; 22 reactor; 23 flash tank; 24 methyl formate condenser; 25 thin film evaporator; 26 methanol condenser; 27 catalyst settler (or filter); 28 light component tower; 29 light Tower condenser; 210 light tower reboiler; 211 vacuum product tower; 212 product tower condenser; 213 product tower reboiler. Refer to the schematic diagram of the continuous production process of N-formylmorpholine ( figure 2) Methyl formate and morpholine containing a prescribed amount of catalyzer are squeezed into the static mixer 21 with a metering pump respectively, and then enter the tubular reactor 22 (embodiment 6-7) or tower reactor 22 ( Examples 8-10) were reacted to obtain the crude product.

[0049] The crude product flowing out from the reactor enters the flash tank 23 for flash evaporation after the pressure is reduced to 0.15MPa through the throttle valve, and the gas phase part is methyl formate after being condensed, and the liquid phase enters the rotar...

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PUM

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Abstract

The preparation method for N-formyl morpholine comprises: in batch or continual reactor, with 0.5-5wt% ester interchange catalyst, selecting methyl formate and morpholine by mass ratio as 1:1.30~1.74 as material, reacting for 2-6h on condition of normal pressure-0.6Mpa and 30-120Deg; separating and recovering the product. With this invention, the conversion ratio of morpholine can achieve 98%, total yield up to 95%, and purity more than 99.5%.

Description

Technical areas: [0001] The invention relates to a method for preparing an extraction solvent of an aromatic hydrocarbon device, a butene concentration extraction solvent of a methyl ethyl ketone device, and N-formylmorpholine, an acidic gas removal agent for synthesis gas. Background technique [0002] N-formylmorpholine is an excellent extraction solvent for aromatic hydrocarbons units and a solvent for butene concentration in methyl ethyl ketone units. And N-formylmorpholine and its mixture are excellent acid gas removers for natural gas and synthesis gas, and are used in the new Morphysorb process developed abroad in recent years. [0003] The synthesis techniques of N-formylmorpholine mainly include formic acid method (CN1345723, CN1356324 and 1482121), carbon monoxide carbonylation method and methyl formate method. [0004] The formic acid synthesis route uses formic acid as the acylating agent, and synthesizes N-formylmorpholine under the action of an acidic catalyst...

Claims

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Application Information

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IPC IPC(8): C07D295/185
Inventor 张吉波田振生张钰李志涛宋岩崔中文张启忠刘辉
Owner BC P INC CHINA NAT PETROLEUM CORP
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