A kind of preparation method of proline ionic liquid catalytic synthesis dibutyl carbonate

A technology of dibutyl carbonate and ionic liquids, which is applied in the field of preparation of proline ionic liquids to catalyze the synthesis of dibutyl carbonate, can solve problems such as complex operating procedures, general catalytic effect, and difficulty in large-scale industrial production, and achieve operational The effect of simple process, reduced energy consumption and low cost

Active Publication Date: 2015-09-09
JIANGXI NORMAL UNIV
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the existing Chinese patent CN 102351709 A reports the use of alkaline ionic liquid hydroxide 1-butyl-3-methylimidazolium salt as a catalyst to synthesize dibutyl carbonate by transesterification of dimethyl carbonate and n-butanol, but its The catalytic effect is general, the yield of dibutyl carbonate is only 55%, and the operation procedure of the reaction process is relatively complicated. It is necessary to add dimethyl carbonate dropwise, and the by-product methanol must be continuously distilled out, so it is difficult to large-scale industrialization Production

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
  • A kind of preparation method of proline ionic liquid catalytic synthesis dibutyl carbonate
  • A kind of preparation method of proline ionic liquid catalytic synthesis dibutyl carbonate
  • A kind of preparation method of proline ionic liquid catalytic synthesis dibutyl carbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In a 50 mL reactor, after replacing the air in the reaction vessel with an inert gas, add 5.92 g (80 mmol) of n-butanol, 1.8 g (20 mmol) of dimethyl carbonate and ionic liquid N,N,N,N '-Tetraethylquaternary ammonium L-proline salt 0.15 g (2 wt% of the total mass of raw materials), after stirring and mixing uniformly, heated to a reaction temperature of 110 ° C, carried out transesterification for 4 h, after the reaction was completed, the reaction The feed liquid is cooled in a phase separator, static phase separation, and the separated product and ionic liquid catalyst are poured. The used ionic liquid can be used for the next reaction after vacuum distillation. The product is analyzed by gas chromatography, and dimethyl carbonate The conversion rate of ester is 99.0%, and the selectivity of dibutyl carbonate is 95%.

Embodiment 2

[0028] In a 50 mL reactor, after replacing the air in the reaction vessel with an inert gas, add 5.92 g (80 mmol) of n-butanol, 1.8 g (20 mmol) of dimethyl carbonate and ionic liquid N,N,N,N '-Tetraethylquaternary ammonium L-homoproline salt 0.12 g (1.5 wt% of the total mass of raw materials), after stirring and mixing uniformly, heated to a reaction temperature of 110 ° C, and carried out transesterification for 4 h. The reaction feed liquid is cooled in a phase separator, static phase separation, and the separated product and ionic liquid catalyst are poured. The used ionic liquid can be used for the next reaction after vacuum distillation. The product is analyzed by gas chromatography. The conversion rate of methyl ester is 98.9%, and the selectivity of dibutyl carbonate is 94.8%.

Embodiment 3

[0030] In a 100 mL reactor, after replacing the air in the reaction vessel with an inert gas, add 7.4 g (100 mmol) of n-butanol, 1.8 g (20 mmol) of dimethyl carbonate and ionic liquid N,N,N,N '-Tetraethylquaternary ammonium L-hydroxyproline salt 0.28 g (3 wt% of the total mass of raw materials), after stirring and mixing evenly, heated to a reaction temperature of 110 ° C, and carried out transesterification for 5 h. The reaction feed liquid is cooled in a phase separator, static phase separation, and the separated product and ionic liquid catalyst are poured. The used ionic liquid can be used for the next reaction after vacuum distillation. The product is analyzed by gas chromatography. The conversion rate of methyl ester is 96.9%, and the selectivity of dibutyl carbonate is 92.8%.

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 preparation method of dibutyl carbonate through catalyzed synthesis of a proline ionic liquid. The method comprises the following steps of preparing dibutyl carbonate through ester interexchange reaction of dibutyl carbonate and n-butyl alcohol by taking a proline ionic liquid as a catalyst, wherein a conversion ratio of the dibutyl carbonate under a set catalytic reaction condition is as high as 99%, and selectivity of the dibutyl carbonate can reach over 90%. Compared with the prior art, a green solvent ionic liquid is taken as a catalyst, and therefore, the preparation method disclosed by the invention has a plurality of advantages of being gentle in reaction condition, environment-friendly, high in reaction selectivity, high in product yield, convenient for recycling of the catalyst, and the like, and is an efficient green novel method of synthesizing the dibutyl carbonate.

Description

technical field [0001] The invention relates to a method for preparing dibutyl carbonate catalyzed by a proline-based ionic liquid, which is characterized in that the proline-based ionic liquid is used as a catalyst, and the transesterification reaction between dimethyl carbonate and butanol has high selectivity. synthesis of dibutyl carbonate. Background technique [0002] Dibutyl carbonate is a long carbon chain dialkyl carbonate, which is an important organic intermediate and solvent. Because dibutyl carbonate has good lubricity, wear resistance, corrosion resistance, high thermo-oxidative stability and good biodegradability, it can not only be used as a matrix material for environmentally friendly high-end synthetic lubricants, but also It can be used in a large amount as a solvent for electrolytes in lithium-ion batteries, and can also be used to synthesize diphenyl carbonate, and then produce important engineering plastics such as polycarbonate, which has a wide range...

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 Patents(China)
IPC IPC(8): C07C68/06C07C69/96C07C27/00C07C31/04C07C29/128C07C211/63C07C209/00C07D207/16C07D233/58C07D211/60
CPCB01J31/0277B01J2231/49C07C68/06C07D207/16C07D211/60C07D233/58C07C69/96Y02P20/52Y02P20/54Y02P20/584
Inventor 陶端健杨振欧阳凡许姝李章敏
Owner JIANGXI NORMAL UNIV
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