Method for preparing alpha-oxocarboxylate through selective oxidation of alpha-hydroxy carboxylate

A technology of hydroxycarboxylate and oxocarboxylate, which is applied in the field of preparation of α-oxocarboxylate, can solve the problems of high reaction temperature, high cost, explosion, etc., and achieve the effect of high yield and low cost

Inactive Publication Date: 2021-03-12
XIAMEN UNIV
View PDF7 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the gas-phase oxidation method has high reaction temperature, harsh reaction conditions, and high requirements for equipment; while in the liquid-phase oxidation system, the oxidants are mainly hydrogen peroxide and molecular oxygen. Compared with molecular oxygen, the cost of using hydrogen peroxide as an oxidant is relatively high. , there is also a risk of explosion in the actual production process

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 alpha-oxocarboxylate through selective oxidation of alpha-hydroxy carboxylate
  • Method for preparing alpha-oxocarboxylate through selective oxidation of alpha-hydroxy carboxylate
  • Method for preparing alpha-oxocarboxylate through selective oxidation of alpha-hydroxy carboxylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1. The preparation method of VPO catalyst is as follows:

[0025] 1) Weigh 0.92g V 2 o 5 Place in a mixed solvent of isobutanol-benzyl alcohol (20ml-20ml), and heat to reflux at 140°C for 5h; after cooling the above reaction solution, add 1.42g of 85wt% phosphoric acid, raise the temperature to 140°C and continue to reflux for 5h; The solution was cooled to room temperature and then filtered, and the obtained solid was washed twice with acetone, and placed in a vacuum drying oven to heat up to 100°C and dried for 6 hours to obtain the catalyst precursor vanadium hydrogen oxyphosphate (VOHPO 4 0.5H 2 O).

[0026] 2) Put the catalyst precursor prepared in step 1) in a muffle furnace, raise the temperature to 420° C. at a rate of 3° C. / min, and then calcinate it for 16 hours to obtain VPO.

[0027] 2. Using the above-mentioned VPO catalyst, prepare α-oxocarboxylate by selective oxidation of α-hydroxycarboxylate:

[0028] Add 5.9g of ethyl lactate, 10ml of diethyl succ...

Embodiment 2

[0032] 1. Supported VPO catalyst, the carrier is strong hydrophobic SiO 2 , the preparation method is as follows:

[0033] 1) Weigh 0.92g V 2 o 5 Place in a mixed solvent of isobutanol-benzyl alcohol (20ml-20ml), heat to reflux at 140°C for 5h; add 1.0g of strongly hydrophobic SiO 2 , continue to reflux for 2h; after cooling the above reaction solution, add 1.42g of 85wt% phosphoric acid, heat up to 140°C and continue to reflux for 5h; filter the reaction solution after cooling to room temperature, wash the obtained solid twice with acetone, and place in a vacuum oven The temperature was raised to 100°C and dried for 6 hours to obtain the supported catalyst precursor vanadium hydrogen oxyphosphate (VOHPO 4 0.5H 2 O).

[0034] 2) Place the catalyst precursor prepared in step 1) in a muffle furnace, raise the temperature to 420°C at a rate of 3°C / min, and then calcinate for 16 hours to obtain VPO / SiO 2 (hydrophobic).

[0035] 2. Using the above VPO / SiO 2 (Hydrophobic) Ca...

Embodiment 3

[0040] 1. The preparation method of VPO catalyst is as follows:

[0041] 1) Weigh 0.92g V 2 o 5 Place in a mixed solvent of sec-butanol-phenylethyl alcohol (15ml-15ml), heat and reflux at 130°C for 4h; after cooling the above reaction solution, add 1.20g of 85wt% phosphoric acid, heat up to 130°C and continue to reflux for 4h; The solution was cooled to room temperature and then filtered, and the obtained solid was washed twice with acetone, and placed in a vacuum drying oven to heat up to 100°C and dried for 6 hours to obtain the catalyst precursor vanadium hydrogen oxyphosphate (VOHPO 4 0.5H 2 O).

[0042] 2) The catalyst precursor prepared in step 1) was placed in a muffle furnace, and the temperature was raised to 360° C. at a rate of 3° C. / min, and then calcined for 12 hours to obtain VPO.

[0043] 2. Using the above-mentioned VPO catalyst, prepare α-oxocarboxylate by selective oxidation of α-hydroxycarboxylate:

[0044] Add 5.9g of methyl lactate, 8ml of dimethylforma...

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 alpha-oxocarboxylate through selective oxidation of alpha-hydroxy carboxylate, and relates to the field of preparation of alpha-oxocarboxylate, in a liquid phase solvent, molecular oxygen is used as an oxygen source, vanadium phosphorus oxide (VPO) compounded by + 4 valence V and + 5 valence V is used as a catalyst, and alpha-hydroxy carboxylate is reacted with molecular oxygen to be selectively oxidized to prepare alpha-oxocarboxylate; wherein the vanadium phosphorus oxide (VPO) catalyst is a vanadium phosphorus oxide (VPO) catalyst compounded byvanadyl phosphate (VOPO4) (VV) and vanadyl pyrophosphate ((VO) 2P2O7) (VIV). The vanadium phosphorus oxide (VPO) catalyst is a cheap non-noble metal catalyst and is relatively low in cost; the reaction can be carried out under normal pressure, and the requirement on equipment is low; according to the invention, high yield (90%) of alpha-oxocarboxylate is realized; and the catalyst can be repeatedly used after being reactivated.

Description

technical field [0001] The invention relates to the field of preparation of alpha-oxocarboxylates, in particular to a method for preparing alpha-oxocarboxylates by selective oxidation of alpha-hydroxycarboxylates. Background technique [0002] α-Oxocarboxylate contains both carbonyl and ester functional groups, and is an important class of organic intermediates with high added value. Due to its special structure, α-oxocarboxylates are widely used in the fields of medicine, spices, food and cosmetics. [0003] At present, the main method for preparing α-oxocarboxylates is through the catalytic oxidation of α-hydroxycarboxylates. The raw material α-hydroxycarboxylate of this method is cheap and easy to obtain, and the α-oxocarboxylate can be prepared only by oxidizing the alcohol hydroxyl on the α-hydroxycarboxylate into a ketone group, which has high atom economic efficiency . The method is mainly divided into gas phase oxidation method and liquid phase oxidation method. ...

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): C07C67/313C07C69/716B01J27/198
CPCB01J27/198C07C67/313C07C69/716Y02P20/584
Inventor 李军李卓昱王杨志王宏涛王焱良
Owner XIAMEN 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