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Method for preparing p-hydroxybenzaldehyde and m-hydroxybenzaldehyde from mixed cresol

A technology of p-hydroxybenzaldehyde and m-hydroxybenzaldehyde, which is applied in the field of preparing p-hydroxybenzaldehyde and m-hydroxybenzaldehyde from mixed phenols, can solve the problems of low efficiency and cumbersome methods, and achieve the goal of expanding the selection range and reducing production costs Effect

Inactive Publication Date: 2013-08-28
东营海源化工股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, all methods of separating the mixture of the two are extremely tedious and inefficient

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Oxidation:

[0026] Add mixed phenol into a high-pressure reactor equipped with a stirrer, a thermometer and an air duct, start stirring, and keep stirring during the reaction; add methanol, catalyst, sodium hydroxide, and calcium oxide in sequence, close the reaction system, and react Heat the kettle jacket with hot water to a temperature of 70°C in the kettle, and keep it warm for 1 hour to completely dissolve the solid NaOH; feed air to react, and control the pressure in the kettle to 0.5 MPa, and react at a temperature of 70°C for 6 hours. After the reaction is over, the water in the jacket of the reaction kettle is lowered to normal temperature, and the exhaust valve is opened to discharge the residual gas in the kettle.

[0027] Copper chloride and cobalt chloride are used as catalysts, and the ratio of the two is copper chloride:cobalt chloride=1.00:0.90.

[0028] The amount of catalyst added is 5% of the mixed phenol.

[0029] Mixed phenol:methanol:sodium hydr...

Embodiment 2

[0036] Oxidation:

[0037] Add mixed phenol into a high-pressure reactor equipped with a stirrer, a thermometer and an air duct, start stirring, and keep stirring during the reaction; add methanol, catalyst, sodium hydroxide, and calcium oxide in sequence, close the reaction system, and react Heat the kettle jacket with hot water to a temperature of 70°C, and keep it warm for 1 hour to completely dissolve the solid NaOH; feed air to react, and control the pressure inside the kettle to 0.2 MPa MPa, and react at a temperature of 80°C for 10 hours. After the reaction is over, the water in the jacket of the reaction kettle is lowered to normal temperature, and the exhaust valve is opened to discharge the residual gas in the kettle.

[0038] Copper chloride and cobalt chloride are used as catalysts, and the ratio of the two is copper chloride: cobalt chloride=1.00:1.10.

[0039] The amount of catalyst added is 2% of the mixed phenol.

[0040] Mixed phenol:methanol:sodium hydroxid...

Embodiment 3

[0047] Oxidation:

[0048] Add mixed phenol into a high-pressure reactor equipped with a stirrer, a thermometer and an air duct, start stirring, and keep stirring during the reaction; add methanol, catalyst, sodium hydroxide, and calcium oxide in sequence, close the reaction system, and react Heat the kettle jacket with hot water to a temperature of 70°C in the kettle, and keep it warm for 1 hour to completely dissolve the solid NaOH; feed air to react, and control the pressure in the kettle to 0.5 MPa, and react at a temperature of 70°C for 6 hours. After the reaction is over, the water in the jacket of the reaction kettle is lowered to normal temperature, and the exhaust valve is opened to discharge the residual gas in the kettle.

[0049] Copper chloride and cobalt chloride are used as catalysts, and the ratio of the two is copper chloride:cobalt chloride=1.00:0.90.

[0050] The amount of catalyst added is 5% of the mixed phenol.

[0051] Mixed phenol:methanol:sodium hydr...

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PUM

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Abstract

The invention discloses a method for preparing p-hydroxybenzaldehyde and m-hydroxybenzaldehyde from mixed cresol. The method comprises the following steps of: 1, oxidization: adding sodium hydroxide, calcium oxide and a catalyst to mixed cresol and methanol which are used as raw materials for reacting under the conditions of heating and pressurizing, thus obtaining a mixture of p-hydroxybenzaldehyde and m-hydroxybenzaldehyde; and separating the mixture to obtain the crude product of the mixture of p-hydroxybenzaldehyde and m-hydroxybenzaldehyde; 2, refining: refining the crude product of the mixture of p-hydroxybenzaldehyde and m-hydroxybenzaldehyde to obtain the mixture of p-hydroxybenzaldehyde and m-hydroxybenzaldehyde; and 3, separation: sublimating the mixture of p-hydroxybenzaldehyde and m-hydroxybenzaldehyde by virtue of the property of the p-hydroxybenzaldehyde easy to sublimate under heating, and condensing the sublimate, thus obtaining the p-hydroxybenzaldehyde in a condensation tank and keeping the m-hydroxybenzaldehyde in a sublimation tank; and finally, separating out the p-hydroxybenzaldehyde and the m-hydroxybenzaldehyde from each other.

Description

technical field [0001] The invention relates to a method for preparing p-hydroxybenzaldehyde and m-hydroxybenzaldehyde, especially suitable for preparing p-hydroxybenzaldehyde and m-hydroxybenzaldehyde with mixed phenol. Background technique [0002] Both p-hydroxybenzaldehyde and m-hydroxybenzaldehyde are important chemical raw materials. There are many methods for producing p-hydroxybenzaldehyde and m-hydroxybenzaldehyde, and these methods are complex in operation and serious in pollution. Now the common method for industrial production of p-hydroxybenzaldehyde and m-hydroxybenzaldehyde is to use p-cresol as raw material, and selectively oxidize the methyl group on the benzene ring of p-cresol to obtain p-hydroxybenzaldehyde; use m-cresol as raw material for the same process m-Hydroxybenzaldehyde can be obtained. The supply of raw materials p-cresol and m-cresol is small and the price is high, so the price of p-hydroxybenzaldehyde and m-hydroxybenzaldehyde has been high ...

Claims

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Application Information

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IPC IPC(8): C07C45/36C07C47/542C07C45/81
Inventor 刘彦丰刘锋李崇赵秋云王芳张力擎张大治张曾
Owner 东营海源化工股份有限公司
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