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Anisaldehyde preparation method

A technology for anisaldehyde and p-hydroxybenzaldehyde, which is applied in the field of preparation of anisaldehyde, can solve the problems of high cost, great harm to people and the environment, and difficulty in treating dimethyl sulfate-containing waste water, and achieves low production cost and improved reaction performance. Conversion rate, easy-to-handle effects

Inactive Publication Date: 2019-12-20
HUAIAN WAN BANG SPICE IND CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with other methods such as anethole oxidation, anisole chloromethylation, and p-cresol synthesis, this method has the advantages of short production cycle, high yield (91%), and low cost. However, dimethyl sulfate Ester is a highly toxic drug, which is extremely harmful to people and the environment. The whole process of transportation, storage, and use is controlled. It is difficult and costly to treat wastewater containing dimethyl sulfate.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Put 122g of p-hydroxybenzaldehyde, 48g of sodium hydroxide, and 192g of water into the autoclave, close the autoclave, start stirring, replace the air in the autoclave with nitrogen, control the temperature at 70°C to 80°C, and perform a salt-forming reaction for 3 hours.

[0022] Methane chloride is preheated and vaporized at 30°C to 50°C, and the vaporization pressure is 0.5Mpa to 0.6Mpa.

[0023] Slowly feed gasified and preheated methyl chloride into the autoclave for alkylation reaction, control the reaction temperature at 70°C to 80°C, and the pressure at 0.5Mpa to 0.6Mpa. When the pressure in the autoclave no longer drops, the reaction ends. When the sample is detected, the content of p-hydroxybenzaldehyde in the raw material is less than 0.1%, the temperature is lowered, the pressure is released, nitrogen is replaced, and the nitrogen environment is left to stand for stratification, and the separated organic phase is washed with 8% to 12% sodium sulfate solution ...

Embodiment 2

[0026] Put 122g of p-hydroxybenzaldehyde, 52g of sodium hydroxide, and 208g of water into the autoclave, seal the autoclave, start stirring, replace the air in the autoclave with nitrogen, control the temperature at 70°C to 80°C, and perform a salt-forming reaction for 2 hours.

[0027] Methane chloride is preheated and vaporized at 30°C to 50°C, and the vaporization pressure is 0.5Mpa to 0.6Mpa.

[0028] Slowly feed gasified and preheated methyl chloride into the autoclave for alkylation reaction, control the reaction temperature at 70°C to 80°C, and the pressure at 0.5Mpa to 0.6Mpa. When the pressure in the autoclave no longer drops, the reaction ends. When the sample is detected, the content of p-hydroxybenzaldehyde in the raw material is less than 0.1%, the temperature is lowered, the pressure is released, nitrogen is replaced, and the nitrogen environment is left to stand for stratification, and the separated organic phase is washed with 8% to 12% sodium sulfate solution u...

Embodiment 3

[0031] Put 122g of p-hydroxybenzaldehyde, 60g of sodium hydroxide, and 240g of water into the autoclave, seal the autoclave, start stirring, replace the air in the autoclave with nitrogen, control the temperature at 70°C to 80°C, and perform a salt-forming reaction for 5 hours.

[0032] Methane chloride is preheated and vaporized at 30°C to 50°C, and the vaporization pressure is 0.5Mpa to 0.6Mpa.

[0033] Slowly feed gasified and preheated methyl chloride into the autoclave for alkylation reaction, control the reaction temperature at 70°C to 80°C, and the pressure at 0.5Mpa to 0.6Mpa. When the pressure in the autoclave no longer drops, the reaction ends. When the sample is detected, the content of p-hydroxybenzaldehyde in the raw material is less than 0.1%, the temperature is lowered, the pressure is released, nitrogen is replaced, and the nitrogen environment is left to stand for stratification, and the separated organic phase is washed with 8% to 12% sodium sulfate solution u...

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PUM

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Abstract

The invention discloses an anisaldehyde preparation method, which comprises: (1) stirring and mixing p-hydroxybenzaldehyde, sodium hydroxide and water, and carrying out a salifying reaction in a nitrogen environment; (2) after the salifying reaction is finished, continuously introducing preheated and gasified chloromethane into the reaction system in the step (1), carrying out an alkylation reaction, finishing the reaction when the chloromethane is continuously introduced and the pressure of the system is not reduced any more in the reaction process, cooling, releasing the pressure, carrying out standing layering in a nitrogen environment, and washing the organic phase with a sodium sulfate solution until achieving a weakly alkaline state to obtain crude anisaldehyde; and (3) carrying outpressure reducing rectification on the crude anisaldehyde obtained in the step (2) to obtain finished anisaldehyde. According to the invention, methyl chloride is adopted to replace dimethyl sulfate so as to substantially reduce the harm to the human body and the environment, achieve high yield and low cost and easily treat wastewater.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a preparation method of anisaldehyde. Background technique [0002] Anisaldehyde, also known as anisaldehyde, p-methoxybenzaldehyde. Appearance is colorless to pale yellow liquid with sweet, powdery, spicy, creamy, vanilla aroma and taste. Molecular formula is C 8 h 8 o 2 , the molecular weight is 136.15, the melting point is 2.5°C, the boiling point is 249.5°C, almost insoluble in water, easily soluble in organic solvents such as ethanol, ether, acetone, chloroform, etc., and can volatilize with water vapor. Mainly used for blending acacia, lilac, sunflower, osmanthus, lily of the valley and other daily flavors as well as vanilla, spices, almonds, butter, anise, caramel, cherry, chocolate, walnut, raspberry, strawberry, mint, nuts, etc. Food flavor. [0003] At present, the industrial production mainly adopts the p-hydroxybenzaldehyde method to prepare a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/64C07C47/575
CPCC07C45/64C07C47/575
Inventor 陈文抗龙晋辉杨丽谢雨
Owner HUAIAN WAN BANG SPICE IND CO LTD