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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  • 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 pollu

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
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Example Embodiment

[0030] Example 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 with a mass ratio of 3:1, turn on high-pressure metering pump 2, and pump at a constant rate of 4g / min Enter the p-hydroxybenzaldehyde toluene solution, set the temperature of the preheater 3 to 260°C, the temperature of the supercritical pipeline reactor 4 to 300°C, and adjust the high-precision reverse pressure controller 6 after the condenser 5, The pressure is controlled at 20±1MPa, and the reaction residence time is 35min. After the completion of the reaction, the reaction liquid was collected and separated by distillation to obtain p-hydroxyphenyl butenone. The calculated yield relative to p-hydroxybenzaldehyde was 96.1%.

Example

[0032] Examples 2~5

[0033] According to Example 1, by changing the flow rate of pump 1 to change the molar ratio of p-hydroxybenzaldehyde, acetone and toluene, keeping pump 2 flow rate, reaction temperature, preheater temperature, reaction pressure and other conditions unchanged, after the reaction is complete The results obtained are as follows (Table 1):

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

[0035]

Example

[0036] Examples 6-9

[0037] According to Example 1, by changing the flow rate of pump 2 to change the molar ratio of p-hydroxybenzaldehyde, acetone and toluene, keeping pump 1 flow rate, reaction temperature, preheater temperature, reaction pressure and other conditions unchanged, the result is obtained after the reaction The results are as follows (Table 2):

[0038] Table 2 The influence of raw material ratio on the 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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