Method for preparing diethoxymethane

A diethoxymethane and integrated technology, applied in the field of diethoxymethane preparation, can solve the problems of long contact time, affecting product quality and yield, affecting conversion rate, etc., to reduce the production of monoethoxymethane , avoid coking inactivation, avoid the effect of secondary reaction

Active Publication Date: 2018-05-18
NANJING NORMAL UNIVERSITY +1
View PDF5 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using organic acid as a catalyst, using kettle reaction to rectify diethoxymethane, the process is simple, easy to operate, and the phenomenon is intuitive, but there are low conversion rate and poor selectivity in the preparation process, and easy to produce monoethoxymethane. The reaction process The product generated in the process cannot be removed in time, and secondary reactions are prone to occur, which brings difficulty to refining and affects product quality and yield.
Diethoxymethane is prepared by reactor reaction distillation using solid acid as a catalyst. There are problems such as uneven distribution of raw materials and catalyst, internal temperature difference and long contact time. The catalyst shows that it is easy to deposit carbon and affect the conversion rate.

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
  • Method for preparing diethoxymethane
  • Method for preparing diethoxymethane
  • Method for preparing diethoxymethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The upper end of the tube bundle reaction device 2 is connected to the rectifying device 1 by a flange, and the temperature of the reaction tube 12 in the tube bundle reaction device 2 is controlled by adding a heating medium from the heating medium feed port 15 to be 101 to 103° C. and the temperature of the preheater 25 The temperature is 102-104°C, while the temperatures of the inner reflux condenser 3 and the outer condenser 16 are controlled by cooling medium, and the temperatures are 65.0-68.0°C and 22.0-28.0°C respectively. The packing in the packing 2 of the rectification section adopts Ring, the packing in the packing 4 of the stripping section adopts ring.

[0020] Mix ethanol and formaldehyde (its mass percentage is 37%) according to the mass ratio of 1.2:1, and control the air speed ratio by valve 26 to be 1.0h -1 , after the mixture is preheated, it is fed into the reaction tube 12 from the second feed port 8 through the distributor 13, and SO is adde...

Embodiment 2

[0022] The basic steps are the same as in Example 1, except that the mass ratio of ethanol and formaldehyde is 1.15:1, SO 4 2- The mass ratio of / Hβ catalyst to formaldehyde is 4.5:100, reacts under the action of catalyst, generates the mixture containing 57.13% diethoxymethane quality, the reflux ratio of the internal reflux condenser 3 of setting is 2, low boiling point The components are refluxed through the condensed part of the internal reflux condenser 3, and the remaining part is condensed through the external condenser 16 to obtain a mixture with a mass content of 91.94%. The yield of diethoxymethane reaches 99.02%, and the material is discharged to the collection tank 17, while Water content of 98.21% and unreacted ethanol flow out from the first outlet 20 at the bottom of the rectification device 1 .

Embodiment 3

[0024] The basic steps are the same as in Example 1, except that the mass ratio of ethanol and formaldehyde is 1.25:1, SO 4 2- The mass ratio of / Hβ catalyst to formaldehyde is 6.5:100, reacts under the action of catalyst, generates the mixture containing 58.31% diethoxymethane mass, the reflux ratio of the set internal reflux condenser 3 is 4, low boiling point The components are refluxed through the condensed part of the internal reflux condenser 3, and the remaining part is condensed through the external condenser 16 to obtain a mixture with a mass content of 92.22%. The yield of diethoxymethane reaches 99.47%, and the material is discharged to the collection tank 17, and Water content of 98.37% and unreacted ethanol flow out from the first outlet 20 at the bottom of the rectification device 1 .

[0025] By adopting the preparation method of the present invention to prepare diethoxymethane, after 700 hours of work, the purity of diethoxymethane only decreases by 0.15%, and...

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 invention discloses a method for preparing diethoxymethane. The method comprises the following steps that an up-down integrated rectification device and a tube bundle reaction device are adopted,ethyl alcohol and formaldehyde are mixed according to the mass ratio of (1.15-1.25):1, the mixture is added into the tube bundle reaction device, a reaction is conducted at 101-103 DEG C, a diethoxymethane mixture is generated, the mixture is lifted to the rectification device to be rectified, and diethoxymethane can be obtained. The method has the advantages that the preparation method can make the generated diethoxymethane mixture continuously and timely guided out of the bottom of the tube bundle reaction device, condensation is not needed, the mixture directly enters the rectification device to be rectified, the phenomenon that a catalyst and the reaction are always in a high-temperature state, and coking deactivation is caused is avoided, a secondary reaction is avoided, producing ofmonoethoxymethane is lowered, the conversion rate of products is increased, the selectivity of the reaction process is improved, and convenience is brought to operation.

Description

technical field [0001] The invention belongs to the field of diethoxymethane preparation. Background technique [0002] Diethoxymethane is regarded as a diether of the same carbon dihydric alcohol, which is quite stable to alkalis and oxidants, and has unique properties. It can not only be used as a solvent in organic synthesis, a solvent in batteries, and a fuel additive. It can also be used as a reagent for organic reactions, such as formaldehyde equivalents, substrates for carbonylation, etc. [0003] At present, the preparation of diethoxymethane uses inorganic acids, heteropoly acids or solid organic acids (such as: acidic molecular sieves, carbon-supported acids, etc.) as catalysts, and is prepared by kettle reaction or reactive distillation. The use of inorganic acid catalyzed reaction is easy to produce acidic wastewater, which is gradually eliminated by organic acid catalyzed reaction. Using organic acid as a catalyst, using kettle reaction to rectify diethoxymeth...

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
Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/30C07C41/50C07C41/58
CPCC07C41/50C07C41/58C07C43/30
Inventor 顾正桂曹晓艳沈林虎冯志群李硕凌鸿钰
Owner NANJING NORMAL UNIVERSITY
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap