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M-aminobenzoic acid spherical crystal and preparation method thereof

A technology of aminobenzoic acid and spherical crystals, which is applied in the preparation of cyanide reaction, chemical instruments and methods, and the preparation of organic compounds. Utilization, low cost effect

Active Publication Date: 2021-02-12
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The cooling crystallization process of m-aminobenzoic acid in this method is carried out in a water-p-chlorotoluene system. Experiments are carried out according to the disclosed method of the invention. The prepared m-aminobenzoic acid crystals are needle-shaped and are crystal form I, with a particle size of about 20 μm. , small particle size acicular crystal habit will lead to easy agglomeration of the product, poor chemical stability, small particle size acicular metastable crystal form I has hidden dangers of crystal transformation due to the aforementioned reasons, and the crystallization process needs to add alkali to adjust pH, complex operation, and requires equipment Corrosion resistance, high production cost

Method used

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  • M-aminobenzoic acid spherical crystal and preparation method thereof
  • M-aminobenzoic acid spherical crystal and preparation method thereof
  • M-aminobenzoic acid spherical crystal and preparation method thereof

Examples

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Effect test

Embodiment 1

[0064] Dissolve 10g of m-aminobenzoic acid I crystal form raw material in 100g of isopropanol at 60°C and 250r / min stirring speed to prepare a m-aminobenzoic acid solution, the solution concentration is 0.091g / g solution, at 3°C / 10min Cooling rate Cool the solution to 10°C, continue to stir at 250r / min until the crystals appear, and continue to stir at a constant temperature for 40 minutes to coalesce the crystals into balls. At this time, the density of the crystal slurry is 0.078g / g solution, then filter the crystal slurry, wash with water, Air-dried at 50°C for 12 hours to obtain spherical crystals of m-aminobenzoic acid. The purity of the spherical crystals of m-aminobenzoic acid obtained after testing is 98.1%, and the volume average particle size is 1.22mm, as attached figure 2 As shown, the angle of repose is 25.8°, the fluidity of the product is greatly improved, and it has a significant improvement effect on the post-treatment of the product such as filtration, washi...

Embodiment 2

[0066] Dissolve 13g of m-aminobenzoic acid I crystal form raw material in 100g of ethylene glycol at 65°C and a stirring rate of 300r / min to prepare a m-aminobenzoic acid solution, the solution concentration is 0.115g / g solution, at 5°C / 10min Lower the temperature of the solution to 5°C, continue to stir at 300r / min until the crystals appear, and continue to stir at a constant temperature for 60 minutes to make the crystals coalesce into balls. At this time, the density of the crystal slurry is 0.080g / g solution, then filter the crystal slurry and wash with water , Blast drying at 50°C for 12 hours to obtain spherical crystals of m-aminobenzoic acid. The purity of the spherical crystals of m-aminobenzoic acid obtained through testing is 98.0%, the volume average particle size is 0.63mm, and the angle of repose is 24.4°. treatment, there is a significant improvement; the agglomeration rate of spherical crystals is 6.0%, which is far less than 58-64% of needle crystals; the tap ...

Embodiment 3

[0068] Dissolve 11g of m-aminobenzoic acid I crystal form raw material in 100g of ethanol at 50°C and a stirring rate of 200r / min to prepare a m-aminobenzoic acid solution. Cool the solution to 10°C at a high speed, continue to stir at 200r / min until the crystals appear, and continue to stir at a constant temperature for 50 minutes to coalesce the crystals into balls. At this time, the density of the crystal slurry is 0.080g / g solution, then filter the crystal slurry, wash with water, °C blast drying for 10 hours to obtain spherical crystals of m-aminobenzoic acid. The purity of the spherical crystals of m-aminobenzoic acid obtained through testing is 98.2%, the volume average particle size is 0.55mm, and the angle of repose is 27.7°. treatment, there is a significant improvement; the agglomeration rate of spherical crystals is 6.5%, which is far less than 58-64% of needle-shaped crystals; the tap density of spherical crystals is 0.35g / cm 3 , which improves the storage and tr...

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Abstract

The invention relates to an m-aminobenzoic acid spherical crystal and a preparation method thereof. The method comprises the following steps: dissolving m-aminobenzoic acid I crystal form raw materials in an organic solvent at 45-65 DEG C under the stirring action to prepare an m-aminobenzoic acid solution, cooling the solution to 5-20 DEG C, continuously stirring until crystals emerge, continuously stirring for 30-60 minutes to coalesce the crystals into balls, separating solid and liquid crystal slurry, filtering, washing and drying a wet solid product to obtain m-aminobenzoic acid sphericalcrystals. The spherical crystal prepared by the invention can effectively improve the chemical stability and the crystal form stability of the m-aminobenzoic acid I crystal form. The purity of the spherical crystals is greater than 98%, the volume average particle size is 0.55-1.50 mm, the crystal particles are round, the fluidity is high, the repose angle is 24.3-27.7 degrees, the caking rate is3.0-6.5%, the tap density is 0.28-0.35 g / cm<3>, and the specific surface area is 0.14-0.23 m<2> / g.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering industrial crystallization, and in particular relates to a spherical m-aminobenzoic acid crystal and a preparation method thereof. Background technique [0002] Aminobenzoic acid (CAS: 99-05-8), alias 3-aminobenzoic acid, English name is 3-Aminobenzoic acid, molecular formula C 7 h 7 NO 2 , the molecular weight is 137.1360, and the structural formula is as follows: [0003] [0004] M-aminobenzoic acid is usually white or light yellow needle-like crystals with a melting point of 173-174°C. Slightly soluble in water, easily soluble in methanol, ethanol, acetone, ether and other solvents. M-aminobenzoic acid is an important fine organic chemical product and organic intermediate. It has a wide range of uses including the synthesis of new organic light-emitting materials, azo dyes, new plant growth regulators, and the preparation of new pharmaceutical intermediates. With the conti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/42C07C229/60
CPCC07C227/42C07C229/60
Inventor 鲍颖肖一婷周丽娜拓振光高宇锋侯宝红滕汝刚
Owner TIANJIN UNIV
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