A kind of preparation method of o-vanillin spherical crystal

A technology of o-vanillin and spherical crystals is applied in the field of preparation of o-vanillin spherical crystals and achieves the effects of good fluidity, prevention of coalescence and low economic investment

Active Publication Date: 2022-03-29
TIANJIN UNIV
View PDF0 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to overcome the defects of existing o-vanillin products, the invention provides a method for preparing o-vanillin spherulites by liquid-liquid phase separation, and the spherical o-vanillin crystal product is prepared with uniform particles, good dispersibility, and good fluidity. At the same time, the process is green and environmentally friendly

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 o-vanillin spherical crystal
  • A kind of preparation method of o-vanillin spherical crystal
  • A kind of preparation method of o-vanillin spherical crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Prepare 60 mL of a 0.01 g / mL o-vanillin-water mixed solution at 40°C, stir until liquid-liquid phase separation occurs and o-vanillin oil droplets are evenly distributed in the water;

[0031] (2) Cool the solution to 5°C at a cooling rate of 5°C / 1min, maintain a stirring rate of 300rpm until crystallization, and add 0.02% of surfactant sodium stearate (based on the quality of o-vanillin-water mixed solution). Stir continuously for 0.5h to make the crystals coalesce into compact spheres;

[0032] (3) After vacuum filtration, washing with water, and drying at normal pressure at 20° C. for 12 hours, o-vanillin spherical crystals were obtained.

[0033] The XRD pattern of the product is shown in figure 1 , it can be seen that the product is a stable crystal; the average particle size of spherical particles is 300 microns, the angle of repose is 31°, and the tap density is 0.50g / cm 3 .

Embodiment 2

[0035] (1) Prepare 60 mL of a 0.10 g / mL o-vanillin-water mixed solution at 45°C, stir until liquid-liquid phase separation occurs and o-vanillin oil droplets are evenly distributed in the water;

[0036] (2) Cool the solution to 2°C at a cooling rate of 4.5°C / 1min, maintain a stirring rate of 250rpm until crystallization, and add 0.15% of the surfactant sodium hexametaphosphate (based on the quality of the o-vanillin-water mixed solution). Stir continuously for 2.5 hours to make the crystals coalesce into compact spheres;

[0037] (3) After vacuum filtration, washing with water, and drying at 30° C. under normal pressure for 24 hours, o-vanillin spherical crystals were obtained.

[0038] The XRD pattern of the product is shown in figure 1 , it can be seen that the product is a stable crystal; the average particle size of spherical particles is 500 microns, the angle of repose is 31°, and the tap density is 0.58g / cm 3 .

Embodiment 3

[0040] (1) Prepare 60 mL of a 0.15 g / mL o-vanillin-water mixed solution at 50°C, stir until liquid-liquid phase separation occurs and o-vanillin oil droplets are evenly distributed in the water;

[0041] (2) The solution is cooled to 10°C at a cooling rate of 4°C / 1min, and the stirring rate is maintained at 200rpm to crystallization, and 0.30% of the surfactant sodium dodecylbenzenesulfonate (based on o-vanillin-water mixed solution) is added quality). Continue stirring for 3 hours to make the crystals coalesce into compact spheres;

[0042] (3) After vacuum filtration, washing with water, and drying at normal pressure at 35° C. for 36 hours, o-vanillin spherical crystals were obtained.

[0043] The XRD pattern of the product is shown in figure 1 , it can be seen that the product is a stable crystal; the average particle size of spherical particles is 800 microns, the angle of repose is 33°, and the tap density is 0.55g / cm 3 .

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
melting pointaaaaaaaaaa
angle of reposeaaaaaaaaaa
densityaaaaaaaaaa
Login to view more

Abstract

The invention discloses a preparation method of o-vanillin spherical crystals. At 40-50°C, prepare o-vanillin-water mixed suspension with o-vanillin concentration of 0.01-0.20g / mL; keep stirring until liquid-liquid phase separation occurs in the solution; quench the solution to 1-15°C, and continue Stir until the crystals appear; add a surfactant with a mass fraction of 0.02% to 0.40% (based on the mass of the o-vanillin-water mixed solution), and keep stirring for 0.5 to 5 hours to make the crystals coalesce into balls. Filter, wash and dry to obtain o-vanillin spherical crystals. The crystallization process has a single raw material, and the solvent only involves water, which is environmentally friendly and has a simple process. The particle size of spherulite products can be effectively adjusted by the stirring rate. The average particle size of the product is about 300-1200 microns; the crystal particles are round, with high fluidity, the angle of repose is between 30°-33°, and the tap density is 0.50-0.58 g / cm 3 .

Description

technical field [0001] The invention belongs to the technical field of chemical engineering industrial crystallization, and in particular relates to a preparation method of o-vanillin spherical crystals. Background technique [0002] o-vanillin (CAS: 148-53-8), chemical name 2-hydroxy-3-methoxybenzaldehyde, alias o-vanillin, 2-vanillin, etc. The main use of o-vanillin is as a pharmaceutical intermediate, an important starting material for the synthesis of various raw materials and spices, and it is also used in pharmaceutical and electroplating industries. English name ortho-vanillin, molecular formula C 8 h 8 o 3 , molecular weight 152.15, usually pale yellow crystalline solid, melting point 40°C-42°C. Slightly soluble in cold water, soluble in hot water, ethanol, ether, acetone and other solvents. Ortho-vanillin is an organic synthesis intermediate with aromatic odor commonly used in the chemical industry, and has many similar effects to its isomer vanillin. In vitro...

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): C07C45/81C07C47/575
CPCC07C45/81C07C47/575
Inventor 龚俊波刘岩博陈明洋孙萌萌闫辉姚孟惠侯宝红尹秋响
Owner TIANJIN 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