Method for purifying resorcinol by means of continuous crystallization

A technology for resorcinol and crystallization, which is applied in the field of separation and purification of resorcinol, can solve the problems of reduced energy consumption for recovery and large energy consumption for solvent recovery, and achieves reduced operating costs, high purity and yield, and guaranteed stability. sexual effect

Inactive Publication Date: 2012-08-22
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above research is for the purification of resorcinol by direct cooling crystallization. Compared with one-step crystallization, the crystal purity and yield obtained by multi-stage continuous crystallization are higher. At the same time, the mixed solvent used has the disadvantages of high energy consumption for solvent recovery. Compared with the mixed solvent, toluene is used as Reduced energy consumption for solvent recovery

Method used

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  • Method for purifying resorcinol by means of continuous crystallization

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Add resorcinol crude product and toluene in dissolving device 1, wherein toluene and resorcinol crude product mass ratio are 6.05: 1, and resorcinol crude product purity is 97.79%, and temperature rises to 110 ℃, treats resorcinol After complete dissolution, the solution enters the crystallizer 3 through the pump 2, the temperature of the crystallizer 3 is 85°C, the stirring speed is 300r / min, and the residence time is 1h; then the crystal slurry enters the crystallizer 5 through the pump 4, and the temperature of the crystallizer 5 is 65°C , the stirring speed is 250r / min, the residence time is 1h; then the magma enters the crystallizer 7 through the pump 6, the temperature of the crystallizer 7 is 45°C, the stirring speed is 200r / min, and the residence time is 0.5h. Finally, the crystal slurry enters the solid-liquid separation device 9 through the pump 8 to complete the solid-liquid separation operation. The resulting mother liquor is analyzed by gas chromatography, a...

Embodiment 2

[0019] Add resorcinol crude product and toluene in dissolving device 1, wherein toluene and resorcinol crude product mass ratio are 6.05: 1, and resorcinol crude product purity is 97.79%, and temperature rises to 110 ℃, treats resorcinol After complete dissolution, the solution enters the crystallizer 3 through the pump 2, the temperature of the crystallizer 3 is 80°C, the stirring speed is 350r / min, and the residence time is 1.25h; then the crystal slurry enters the crystallizer 5 through the pump 4, and the temperature of the crystallizer 5 is 65 °C, the stirring speed is 300r / min, and the residence time is 0.75h; then the magma enters the crystallizer 7 through the pump 6, the temperature of the crystallizer 7 is 45°C, the stirring speed is 300r / min, and the residence time is 0.75h. Finally, the crystal slurry enters the solid-liquid separation device 9 through the pump 8 to complete the solid-liquid separation operation. The resulting mother liquor is analyzed by gas chroma...

Embodiment 3

[0021] The experimental device and operation are the same as in Example (1), except that the crystallization temperature of the crystallizer 7 is 40° C., the stirring speed is 250 r / min, and the residence time is 0.5 h. The experimental results are shown in Table 1.

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Abstract

A method for purifying resorcinol by means of continuous crystallization belongs to the technical field of separation and purification of resorcinol, and includes: dissolving the resorcinol into methylbenzene in weight ratio of (6.0-6.1):1, and enabling solution to enter a primary crystallizer to crystallize with the temperature and stirring speed of the primary crystallizer constant; enabling magma to enter a secondary crystallizer, and crystallizing at a certain crystallizing temperature, at a certain stirring speed and by means of equal stop; enabling magma to enter a tertiary crystallizer, and crystallizing at a certain crystallizing temperature, at a certain stirring speed and by means of equal stop, wherein the temperature of the primary crystallizer, the temperature of the secondary crystallizer and the temperature of the tertiary crystallizer are sequentially decreased; and subjecting the magma to solid-liquid separation, and then scrubbing and drying obtained crystals by the methylbenzene. The method realizes continuous operation of crystallization and purification, operating cost is reduced, production capacity is improved, and stability of operating parameters is guaranteed.

Description

technical field [0001] The invention belongs to the technical field of separation and purification of resorcinol, and relates to a method for continuous crystallization and purification of resorcinol. Background technique [0002] Resorcinol is an important fine organic intermediate, which is widely used in rubber, medicine, agriculture, fuel, coating and other fields. In recent years, the demand for resorcinol in the domestic market has increased significantly, and a considerable amount needs to be imported every year to meet the domestic market demand. At present, there are two main processes for producing resorcinol in the world: sulfonation alkali fusion method and m-dicumene oxidation method. The sulfonated alkali fusion process is lengthy, has many three wastes, and the yield is low; while the m-dicumene oxidation method has high yield, good automatic control degree, and easy continuous large-scale production, especially the three wastes discharged by this method rar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/08C07C37/84
Inventor 黄崇品王海萍张傑陈标华
Owner BEIJING UNIV OF CHEM TECH
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