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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
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  • 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

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  • 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
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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 .

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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

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Application Information

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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
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