Maltol Grignard section intermediate purification method

A purification method and intermediate technology, which are applied in the field of maltol Grignard section intermediate purification, can solve the problems affecting the yield and output of maltol, low quality, and low furfuryl alcohol yield, etc., so as to facilitate production control, increase yield and improve production efficiency. Effect of quality, solvent consumption reduction

Inactive Publication Date: 2021-02-26
ANHUI JINGHE IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The yield of furfuryl alcohol is low and the quality is not high
Seriously affect the yield and yield of maltol

Method used

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  • Maltol Grignard section intermediate purification method

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Effect test

Embodiment 1

[0020]A method for purifying maltol Grignard process intermediates, which is characterized in that it comprises the following steps:

[0021](1) Intermediate press 2m3The flow rate of / h enters the rectification tower for rough separation of furfuryl alcohol and solvent. The bottom temperature of the rectification tower is 60℃, and the top temperature is 40℃;

[0022](2) Then it is extracted from the bottom of the rectification tower into the first-level flash distillation kettle, and the extraction flow is 1.5m3 / h, the temperature of the first-level flash vaporizer is 85℃, the gas phase of the first-level flash vaporizer enters the second-level flash vaporizer after condensing, the temperature of the second-level flash vaporizer is 65℃, and the gaseous phase of the second-level flash vaporizer enters the third after condensing The temperature of the three-stage flash tank is 60℃. The temperature of the three-stage flash tank is collected after the gas phase condensation. The temperature ...

Embodiment 2

[0026]A method for purifying maltol Grignard process intermediates, which is characterized in that it comprises the following steps:

[0027](1) Intermediate press 2m3The flow rate of / h enters the rectification tower for rough separation of furfuryl alcohol and solvent. The bottom temperature of the rectification tower is 60℃, and the top temperature is 40℃;

[0028](2) Then it is extracted from the bottom of the rectification tower into the first-level flash distillation kettle, and the extraction flow is 1.5m3 / h, the temperature of the first-level flash vaporizer is 85℃, the gas phase of the first-level flash vaporizer enters the second-level flash vaporizer after condensing, the temperature of the second-level flash vaporizer is 65℃, and the gaseous phase of the second-level flash vaporizer enters the third after condensing The temperature of the three-stage flash distillation kettle is 60℃. The temperature of the three-stage flash distillation reactor is collected after gas phase con...

Embodiment 3

[0032]A method for purifying maltol Grignard process intermediates, which is characterized in that it comprises the following steps:

[0033](1) Intermediate press 2m3The flow rate of / h enters the rectification tower for rough separation of furfuryl alcohol and solvent. The bottom temperature of the rectification tower is 60℃, and the top temperature is 40℃;

[0034](2) Then it is extracted from the bottom of the rectification tower into the first-level flash distillation kettle, and the extraction flow is 1.5m3 / h, the temperature of the first-level flash vaporizer is 85℃, the gas phase of the first-level flash vaporizer enters the second-level flash vaporizer after condensing, the temperature of the second-level flash vaporizer is 65℃, and the gaseous phase of the second-level flash vaporizer enters the third after condensing The temperature of the three-stage flash tank is 60℃. The temperature of the three-stage flash tank is collected after gas phase condensation. The temperature of t...

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Abstract

The invention provides a maltol Grignard section intermediate purification method which comprises the following steps that an intermediate enters a rectifying tower according to the flow of 2 m < 3 >/h, the tower bottom temperature of the rectifying tower is 60 DEG C, and the tower top temperature of the rectifying tower is 40 DEG C; then the intermediate enters a primary flash kettle, wherein theextraction flow is 1.5 m < 3 >/h, the temperature of the first-stage flash evaporation kettle is 85 DEG C, the gas phase of the first-stage flash evaporation kettle is condensed and then enters a second-stage flash evaporation kettle, the temperature of the second-stage flash evaporation kettle is 65 DEG C, the gas phase of the second-stage flash evaporation kettle is condensed and then enters athird-stage flash evaporation kettle, and the temperature of the third-stage flash evaporation kettle is 60 DEG C, the condensed gas phase of the three-stage flash kettle is collected, and the flash kettle is distilled under reduced pressure, wherein the vacuum degree is -0.08 MPa; the materials in the second-stage flash evaporation kettle and the third-stage flash evaporation kettle are returnedto the first-stage flash evaporation kettle every 3 hours; and qualified furfuryl alcohol is extracted from the bottom of the first-stage flash evaporation kettle according to the flow of 0.5 m < 3 >/h. According to the method, the furfuryl alcohol content and yield can be improved, meanwhile, intermittent repeated operation is achieved, and the labor intensity of personnel is relieved.

Description

Technical field[0001]The invention relates to a method for purifying a maltol Grignard process intermediate.Background technique[0002]In the production process of maltol, the traditional furfural method is used. Grignard reagent reacts with furfural in toluene and tetrahydrofuran solvents to form furfuryl alcohol intermediates, and then the solvent is separated and purified by vacuum distillation in the steam reduction kettle. Furfuryl alcohol is used in the chlorination section. However, this separation and purification method is a batch-type single-tank operation, which is complicated in operation, low in production capacity, and high in energy consumption, and the content of furfuryl alcohol after purification is not high and there are many impurities. Furfuryl alcohol is also contained in the recovered solvent. The production of furfuryl alcohol is low and the quality is not high. Seriously affect the yield and output of maltol.Summary of the invention[0003]The technical problem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/44
CPCC07D307/44Y02P20/10
Inventor 詹见陈金林谢国柱
Owner ANHUI JINGHE IND
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