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Method for preparing raspberry ketone under supercritical condition

A raspberry ketone and supercritical technology, which is applied in the preparation of carbon-based compounds, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of high environmental pressure, difficult acid recovery, and easy pollution of the environment. Increased pressure, suitable for industrial production, and high reaction selectivity

Active Publication Date: 2019-04-26
ZHEJIANG NHU CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has many reaction side reactions, complex post-treatment, serious corrosion to equipment, and difficult recovery of acid.
The third is to use anisyl acetone as a raw material to carry out demethylation reaction to synthesize raspberry ketone under acidic (CN104193607B) or alkaline (CN103724173A) system. This method uses hydrobromic acid demethylation, which will produce a large amount of Acidic waste water, and the corrosion and pollution to equipment are serious, cause environmental protection pressure big; The 4th kind is to be raw material with p-hydroxybenzaldehyde and acetone, use a large amount of alkali to make catalyst, synthesize raspberry ketone (CN1036455C by condensation and hydrogenation reaction ), the reaction cost of this method is high, the catalyst is difficult to recycle, and a large amount of salts will be produced, which is easy to pollute the environment

Method used

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  • Method for preparing raspberry ketone under supercritical condition
  • Method for preparing raspberry ketone under supercritical condition
  • Method for preparing raspberry ketone under supercritical condition

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] according to figure 1 As shown in the schematic diagram, turn on high-pressure metering pump 1, and pump acetone at a constant rate of 2g / min; toluene and p-Hydroxybenzaldehyde are prepared into a solution at a mass ratio of 3:1, turn on high-pressure metering pump 2, and pump at a constant rate of 4g / min Enter p-Hydroxybenzaldehyde toluene solution, preheater 3 temperature is set to 260 ℃, the temperature of supercritical pipeline reactor 4 is set to 300 ℃, adjust the high-precision reverse pressure controller 6 behind the condenser 5, The pressure is controlled at 20±1MPa, and the reaction residence time is 35min. After the reaction was completed, the reaction solution was collected and separated by rectification to obtain p-hydroxyphenylbutenone, and the calculated relative yield of p-hydroxybenzaldehyde was 96.1%.

Embodiment 2～5

[0033] According to embodiment 1, by changing the flow rate of pump 1, to change the molar ratio of p-hydroxybenzaldehyde, acetone and toluene, keep the conditions such as the flow rate of pump 2, reaction temperature, preheater temperature, reaction pressure constant, after reaction finishes The results obtained are as follows (Table 1):

[0034] The influence of table 1 raw material ratio on reaction

[0035]

Embodiment 6～9

[0037] According to embodiment 1, by changing the flow rate of pump 2, to change the molar ratio of p-hydroxybenzaldehyde, acetone and toluene, keep conditions such as pump 1 flow rate, reaction temperature, preheater temperature, reaction pressure constant, after the reaction finishes, obtain The results are as follows (Table 2):

[0038] The influence of table 2 raw material ratio on reaction

[0039]

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Abstract

The invention discloses a method for preparing raspberry ketone under a supercritical condition. P-hydroxy benzaldehyde and acetone are used as raw materials, an aromatic solvent is used as a solvent,a condensation reaction is conducted continuously in a pipeline reactor, p-hydroxybenzal vinylmethylketone is obtained in the absence of a catalyst, then, a methanol solution of p-hydroxybenzal vinylmethylketone and hydrogen are subjected to a hydrogenation reduction reaction in a tank reactor under the action of a nickel catalyst to produce raspberry ketone. The preparation method solves the environmental protection problem, has the advantages that the process is simple, acid or base catalysts are not used, few three wastes are produced, the yield is high and enlargement is easy and has higher industrial application values.

Description

technical field [0001] The invention relates to the field of fine chemicals, in particular to a method for preparing raspberry ketone under supercritical conditions. Background technique [0002] Raspberry ketone (p-hydroxybutyrophenone), CAS number: 5471-51-2, chemical name is 4-p-hydroxyphenyl-2-butanone, also known as rubus ketone, insoluble in water and petroleum, soluble in Ethanol, ether and volatile oil are the main aroma components in natural raspberry fruit, and are widely used at home and abroad as a spice with elegant and fruity aroma; it can be used as food additives in beverages, candies, and biscuits; as a modifier, it can be used in In daily spices such as jasmine and tuberose; it can keep the fragrance for a long time, so it is an excellent deodorant, and is widely used in food flavors such as strawberry, raspberry, pineapple and peach. [0003] At present, there are four main chemical synthesis processes for raspberry ketone. The first is to synthesize rasp...

Claims

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Application Information

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IPC IPC(8): C07C45/62C07C49/245
CPCC07C45/62C07C45/74C07C49/245C07C49/248Y02P20/54
Inventor 李观兵王钰毛建拥于明高统海孙群齐雅雅李景波石清爱潘映霞
Owner ZHEJIANG NHU CO LTD
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