Method for synthesizing styrallyl acetate from acetophenone

A technology for styroyl acetate and acetophenone, which is applied in the field of synthesizing styroyl acetate, can solve problems such as inconvenience in large-scale production, easy polymerization of styrene, and potential safety hazards, and achieves the effects of novel synthetic route, good solubility, and easy operation.

Active Publication Date: 2021-03-12
WANHUA CHEM GRP CO LTD
View PDF2 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] This method also uses hydrogen chloride gas, which brings inconvenience to large-scale production, and under strong acid conditions, styrene is easy to polymerize
[0013] In summary, the raw materials of the traditional synthesis process of styroyl acetate in the prior art are highly toxic, the reaction process has a large potential safety hazard, and the yield is low

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 synthesizing styrallyl acetate from acetophenone
  • Method for synthesizing styrallyl acetate from acetophenone
  • Method for synthesizing styrallyl acetate from acetophenone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] Vapor-phase esterification of acetophenone and ketene to styrene acetate:

[0065] Self-made 500mL esterification reaction kettle with stirring, the top of the reaction kettle is equipped with a serpentine condenser tube with a length of 40cm. Kettle, ketene is fed continuously. Add 242.73g of acetophenone and 0.97g of methanesulfonic acid into the esterification reaction kettle. The ketene gas is supplied from a self-made ketene reactor, and the gas outlet is inserted into the bottom of the reaction kettle. The feed rate is 0.60L / min. The stirring speed is 400r / min, and the esterification temperature is controlled at 65°C. The heat preservation reaction was carried out for 3 hours, and the sampling gas phase analysis showed that the conversion rate was 99%, and the selectivity was 99%. Stop feeding ketene, add 50g of saturated sodium bicarbonate aqueous solution to wash three times, add 50g of saturated brine to wash three times, dry at 50°C using anhydrous magnesium...

Embodiment 2

[0071] Vapor-phase esterification of acetophenone and ketene to styrene acetate:

[0072] Self-made 500mL esterification reaction kettle with stirring, the top of the reaction kettle is equipped with a serpentine condenser tube with a length of 40cm. Kettle, ketene is fed continuously. 242.73 g of acetophenone and 1.60 g of benzenesulfonic acid were added to the esterification reactor, and the ketene gas was supplied from a self-made ketene reactor, the gas outlet was inserted into the bottom of the reactor, and the feed rate was 0.60 L / min. The stirring speed is 400r / min, and the esterification temperature is controlled at 65°C. The heat preservation reaction was carried out for 3 hours, and the sampling gas phase analysis showed that the conversion rate was 98%, and the selectivity was 98%. Stop feeding ketene, add 50g of saturated sodium bicarbonate aqueous solution to wash three times, add 50g of saturated brine to wash three times, dry at 50°C using anhydrous magnesium ...

Embodiment 3

[0076] Vapor-phase esterification of acetophenone and ketene to styrene acetate:

[0077] Self-made 500mL esterification reaction kettle with stirring, the top of the reaction kettle is equipped with a serpentine condenser tube with a length of 40cm. Kettle, ketene is fed continuously. 242.73 g of acetophenone and 0.78 g of methanesulfonic acid were added to the esterification reactor, and the ketene gas was supplied from a self-made ketene reactor, the gas outlet was inserted into the bottom of the reactor, and the feed rate was 0.60 L / min. The stirring speed is 400r / min, and the esterification temperature is controlled at 65°C. Insulated reaction for 3 hours, sampling gas phase analysis, the conversion rate was 98%, and the selectivity was 97%. Stop feeding ketene, add 50g of saturated sodium bicarbonate aqueous solution to wash three times, add 50g of saturated brine to wash three times, dry at 50°C using anhydrous magnesium sulfate for 20min, distill under reduced pressu...

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

PropertyMeasurementUnit
boiling pointaaaaaaaaaa
Login to view more

Abstract

The invention provides a method for synthesizing styrallyl acetate from acetophenone, which comprises the following steps: reacting acetophenone with ketene under the catalysis of organic acid to obtain styrene acetate, and hydrogenating styrene acetate to obtain styrallyl acetate. The method is novel in synthetic route, the raw materials acetophenone and ketene are cheap and easy to obtain, the synthetic route is short, the yield is high, no equivalent acetic acid byproduct is produced, and the method has an obvious cost advantage.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and in particular relates to a method for synthesizing styroyl acetate by using vinyl ketone and acetophenone as raw materials. Background technique [0002] Styroyl acetate, also known as gardenia alcohol Ⅱ, scientific name methyl phenylmethanol acetate, transparent colorless to pale yellow viscous liquid, molecular formula: C 10 h 12 o 2 , relative molecular mass: 164.20, boiling point 214°C, belongs to carboxylate synthetic fragrance. Ester flavors are the most widely used in food flavors. Various types of flavors can be obtained through reasonable preparation. They can be used to prepare food flavors such as apples, pineapples, apricots, peaches, pineapples, plums, etc., making many cakes, beverages and other foods fragrant. richer. Styrenyl acetate has a strong diffusivity and can be used as a deodorant for daily chemical essences such as hyacinth, lilac, jasmine, lily of the valley, magnol...

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): C07C67/46C07C67/283C07C69/157
CPCC07C67/46C07C67/283C07C69/157Y02P20/584
Inventor 谢硕王永军黄文学沈稳张永振宋军伟
Owner WANHUA CHEM GRP CO LTD
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