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Method for efficiently recovering low-content benzoic acid through melt crystallization

A melting crystallization, benzoic acid technology, applied in the separation/purification of carboxylic acid compounds, organic chemistry and other directions, can solve the problems of using many equipment, limited solvent dissolution, cumbersome process, etc., and achieve the effect of simplifying operation and reducing operation cost.

Pending Publication Date: 2021-11-30
TIANJIN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method does not indicate the purity of raw materials, and the amount of solvent dissolved is limited, and the process is more cumbersome and requires more equipment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment example 1

[0023] In the 500ml layer type melting crystallizer, drop into 260.29g content and be the crude product of benzoic acid of 67.15%, be heated up to 115 ℃ to material all melt into liquid state, carry out cooling according to the cooling rate of 20K / h, the final temperature of cooling is 73 ℃; discharge Mother liquor, and then raise the material to 122°C at a heating rate of 15K / h to sweat; discharge the sweating liquid; heat and melt to discharge. The obtained product has a purity of 94.91%. The one-way yield is 36.46%.

Embodiment example 2

[0025] In a 500ml layered melting crystallizer, put 388.8g of benzoic acid crude product with a content of 51.57% into it, heat up to 110°C until the material is completely melted into a liquid state, and cool down at a cooling rate of 22K / h, and the final temperature of cooling is 75°C; discharge Mother liquor, and then raise the material to 109°C at a heating rate of 16K / h to sweat; discharge the sweating liquid; heat and melt to discharge. The obtained product has a purity of 93.11%. The single-pass yield is 37.37%. If the mother liquor and sweating liquid are applied mechanically, the total yield can reach 97.3%.

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PUM

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Abstract

The invention belongs to the field of chemical purification, and particularly relates to a method for efficiently recovering low-content benzoic acid through melt crystallization. The method comprises the following steps: (1), performing liquid-phase feeding: adding a solid benzoic acid coarse material with the mass percentage of 40-85% into a layered melt crystallizer, and performing melting at a melting temperature until the solid benzoic acid coarse material is molten into a liquid state; (2), performing cooling and crystallizing: cooling the liquid benzoic acid coarse material with the mass percentage content of more than or equal to 40% at the cooling rate of 1-30K / h, the final cooling temperature being 70-80 DEG C; and keeping the temperature constant for 0.5 h; (3), performing heating and sweating: after the uncrystallized mother liquor is discharged, sweating the crystal at the heating rate of 1-20 K / h, performing eating to 110-125 DEG C, keeping the temperature for 0.5 h, and discharging the sweating liquid; and (4), melting the materials. The method provided by the invention is suitable for the benzoic acid crude product with the mass percentage content of more than or equal to 40%, preferably more than or equal to 50%, is free of additional solvents, reduces the operation cost, simplifies the operation, is environment-friendly, does not produce three wastes, and can obtain benzoic acid with the purity of more than 93%.

Description

technical field [0001] The invention belongs to the field of chemical purification, and relates to a method for efficiently recovering low-content benzoic acid through melt crystallization. Background technique [0002] Benzoic acid is an aromatic acid organic compound and the simplest aromatic acid. It appears as white needle-like or scale-like crystals. It exists widely in nature in the form of free acid, ester or its derivatives. It is mainly used in the preparation of sodium benzoate preservatives, and in the synthesis of drugs and dyes; it is also used in the production of plasticizers, mordants, fungicides and spices. Therefore, the commercial value of benzoic acid is huge, so if it is possible to recover low-content benzoic acid, it is of great value to obtain a high-purity product. [0003] Initially, benzoic acid was obtained by dry distillation of benzoin gum or hydrolysis of alkaline water, and also by hydrolysis of hippuric acid. In industry, toluene, o-xylene ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/43C07C63/06
CPCC07C51/43C07C63/06
Inventor 王彦飞杨鹏辉许史杰张凯丽朱亮杨立斌赵晓昱赵文立韩梅贾原媛杨静赵子健
Owner TIANJIN UNIV OF SCI & TECH
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