Method for recycling by-product 2-ethylacraldehyde from reaction process of preparing trimethylolpropane by condensing and hydrogenating method

A technology of trimethylolpropane and ethylacrolein, which is applied in the field of recovery and utilization of the by-product 2-ethylacrolein in the reaction process of preparing trimethylolpropane by condensation hydrogenation, can solve the problem of low selectivity, Affecting TMP yield and other issues, achieving high economic utilization and reducing reaction costs

Inactive Publication Date: 2012-01-04
SHANGHAI HUAYI GRP CO
View PDF6 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The presence of EA makes the selectivity of DMB in the aldol condensation step not high, which will eventually affect the yield of TMP, so its utilization is of great economic significance

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] According to the molar ratio of triethylamine to formaldehyde of 0.020, add 37wt% formaldehyde aqueous solution and triethylamine into the three-necked flask successively, stir and mix evenly, heat the water bath to 30°C, and then mix to the above-mentioned Add n-butyraldehyde (the molar ratio of formaldehyde to n-butyraldehyde is 2.2) dropwise into the solution, and the dropwise addition is completed within 1 hour. After the dropwise addition, continue to react at 30° C. for 2 hours, and stand to separate layers. The lower water phase is DMB, and the upper oil phase is mainly EA and butyraldehyde.

[0018] Subsequently, the upper oil phase was separated, and it was measured that the content of EA in the upper oil phase was 70%, and the content of butyraldehyde was 25%. After adding formaldehyde with 2 times the molar amount of EA therein, the pH value was adjusted to 10.0 with triethylamine, and the temperature was raised to 50° C. to continue the reaction for 5 hours....

Embodiment 2

[0020] According to the molar ratio of triethylamine to formaldehyde of 0.020, add 37wt% formaldehyde aqueous solution and triethylamine into the three-necked flask successively, stir and mix evenly, heat the water bath to 40°C, and then mix to the above-mentioned Add n-butyraldehyde (the molar ratio of formaldehyde to n-butyraldehyde is 2.2) dropwise into the solution, and the dropwise addition is completed within 1 hour. After the dropwise addition, continue to react at 30° C. for 2 hours, and stand to separate layers.

[0021] Subsequently, the upper oil phase was separated, and the content of EA and butyraldehyde was measured to be 82% and 11% respectively. After adding formaldehyde with 3 times the molar amount of EA therein, the pH value was adjusted to 10.5 with triethylamine, and the temperature was raised to 50° C. to continue the reaction for 5 hours. The selectivity is 90%.

Embodiment 3

[0023] According to the molar ratio of triethylamine to formaldehyde of 0.020, add 37wt% formaldehyde aqueous solution and triethylamine into the three-necked flask successively, stir and mix evenly, heat the water bath to 50°C, and then, under the condition of stirring, mix to the above-mentioned Add n-butyraldehyde (the molar ratio of formaldehyde to n-butyraldehyde is 3.0) dropwise to the solution, and the dropwise addition is completed within 1 hour. After the dropwise addition, continue to react at 50° C. for 2 hours, and stand to separate layers.

[0024] Subsequently, the upper oil phase was separated, and the content of EA and butyraldehyde was determined to be 90% and 6%, respectively. After adding formaldehyde with 4 times the molar amount of EA therein, adjust the pH value to 11 with triethylamine, and react at 50° C. for 5 h at the same time. After the reaction, the conversion rate of EA is measured to be 95%, and the selectivity of TMP generated is 93%.

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 recycling a by-product 2-ethylacraldehyde from a reaction process of preparing trimethylolpropane by a condensing and hydrogenating method. The method comprises the following steps of: taking the main by-product 2-ethylacraldehyde (EA) generated at a condensation stage of aldol in trimethylolpropane prepared by condensing and hydrogenating method as the raw material; separating and reacting the raw material with formaldehyde under the alkaline condition; and finally, obtaining trimethylolpropane (TMP). According to the invention, more than 90% of the EA can be basically transformed and the selectivity of the generated TMP is more than 90%; the method improves the economic utilization of the raw material and the reaction cost is reduced as well. The method provided by the invention also can directly utilize the commercial grade EA and formaldehyde to react under the alkaline condition so that the EA can be transformed into TMP.

Description

technical field [0001] The present invention relates to a recovery and utilization method of by-product 2-ethylacrolein in the reaction process of preparing trimethylolpropane by condensation hydrogenation method, in particular to a method for the recovery and utilization of by-product 2-ethylacrolein in the reaction process of preparation of trimethylolpropane by condensation hydrogenation method The by-product 2-ethylacrolein is recovered for use in the process for the preparation of trimethylolpropane. Background technique [0002] Trimethylolpropane (TMP) is an important fine chemical product with a low melting point (58.8°C) and three methylol groups in its molecular structure, which can react with organic acids to form monoesters or polyesters , react with aldehydes and ketones to form acetals and ketals, and react with diisocyanates to form carbamates, etc. It is widely used in the production of aviation lubricants, plasticizers, surfactants, alkyd resins, polyuretha...

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): C07C31/22C07C29/38
Inventor 杨旭石冯汝明廖本仁揭元萍张春雷
Owner SHANGHAI HUAYI GRP CO
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