Supercharge Your Innovation With Domain-Expert AI Agents!

Process for preparing N-acetyl morpholine

The technology of acetylmorpholine and morpholine is applied in the field of preparation of N-acetylmorpholine, can solve the problems of low production intensity of reactor, high production cost, low utilization rate of raw materials, etc., achieves low cost, large production capacity, improved The effect of conversion rate

Inactive Publication Date: 2006-01-18
BC P INC CHINA NAT PETROLEUM CORP +1
View PDF2 Cites 6 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the raw material utilization rate of this synthetic method is too low (the utilization rate of acetic anhydride is only 50%), the production intensity of reactor is little, and production cost is too high

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Process for preparing N-acetyl morpholine
  • Process for preparing N-acetyl morpholine
  • Process for preparing N-acetyl morpholine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046]This embodiment is the specific implementation of the process flow of the present invention. Morpholine (when the recovery liquid is recycled, the amount of morpholine is reduced by 4%), acetic anhydride, toluene (when the recovery liquid is recycled, the amount of toluene is reduced by 95%) are injected into the morpholine metering tank, In the acetic anhydride metering tank and the toluene metering tank (not listed in the figure), put the molecular sieve catalyst (powder) into the stirred tank reactor (1), add morpholine and toluene successively in the reactor, start stirring, heat up. When the temperature in the kettle reaches 110°C, start to add acetic anhydride slowly (the feeding rate is based on the principle that no liquid flooding occurs in the batch reaction rectification tower), and stop heating at the same time. It rises and gasification occurs, and when the acetic anhydride is added, the heating is resumed. The gas phase of the reactor enters the bottom of...

Embodiment 2

[0050] Add 174.2g of morpholine, 8.3g of 98% concentrated sulfuric acid and 41.5g of toluene into a four-neck flask equipped with a stirrer, a thermometer, a constant pressure funnel, a reflux condenser and a water separator, heat until reflux occurs, and stir vigorously and Heat to reflux, under the condition of reflux temperature of 70-74°C, slowly add 102.1g of acetic anhydride dropwise, morpholine: acetic anhydride = 2.1:1, the time of feeding and heating to reflux is 1.5 hours, condense and reflux for 2 hours to divide the water, when the water is divided Stop the reaction when water no longer occurs in the vessel, and the reaction time is 5 hours. Based on morpholine, the conversion rate was 95.1%, and the yield was 91.4%.

example 3

[0052] Add 174.2g morpholine, N-72 strong acid type ion-exchange resin 8.7g and toluene 43.7g in the four-necked flask that is furnished with stirrer, thermometer, constant pressure funnel, reflux condenser and water trap, be heated to reflux occurring, Heat to reflux at slightly boiling or boiling temperature, and slowly add 117.3 g of acetic anhydride dropwise under strong stirring conditions, morpholine: acetic anhydride = 1.8: 1, the time of feeding and heating to reflux is 1.5 hours, condense and reflux for 2 hours to separate water, Stop the reaction when no more water occurs in the water separator, and the reaction time is 5 hours. Based on morpholine, the conversion rate was 98.3%, and the yield was 95.4%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The present invention is preparation process of N-acetyl morpholine as the main material for synthesizing farm germicide dimethomorph and fluoro morpholine, and features that the reaction is completed inside waterborne agent and has acetic anhydride and morpholine in the molar ratio of 1 to 1.8-2.5 as material and strong acid as catalyst to produce N-acetyl morpholine through reaction and rectification, with the waterborne agent amount being 10-50 wt% of the material, reaction time being 3-9 hr and catalyst amount being 1-7 wt% of material. The preparation process also includes heating reflux at boiling temperature, condensing reflux, separating water, deacidifying, dewatering, filtering and vacuum rectifying. The technological process has great production capacity, low cost, less environmental pollution, conversion rate up to 98 % and yield up to 95 %.

Description

Technical field: [0001] The invention relates to a method for preparing main raw materials for synthesizing agricultural fungicides dimethomorph and flumorph and N-acetylmorpholine, an acid gas removing agent for natural gas and synthesis gas. Background technique [0002] N-acetylmorpholine is a very important pharmaceutical and pesticide intermediate, and is the main raw material for the synthesis of agricultural fungicides dimethomorph and flumorph. The mixture of N-acetylmorpholine and N-formylmorpholine is an excellent acid gas removal agent for natural gas and synthesis gas, and it is used in the new Morphysorb process developed abroad in recent years. [0003] The synthesis technique of N-acetylmorpholine mainly contains acetic acid method (Fr1580614), acetyl chloride method (GB2223492), ketene, acetate and acetic anhydride (CN1403449) route. [0004] The conversion rate and yield of the acetic acid route are low, the highest is 85% based on morpholine, the corrosion...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07D295/16
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
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com