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Method for catalytic synthesis of raspberry ketone in presence of solid acid and alkali

A technology of raspberry ketone and acid-base catalysis, applied in chemical instruments and methods, preparation of organic compounds, carbon-based compounds, etc., can solve the problems of complex post-processing, equipment corrosion, environmental pollution, etc., and achieve simple post-processing, The effect of short reaction time and low equipment investment

Active Publication Date: 2015-04-08
SHANDONG JIUXIN BIOLOGICAL TECH CO LTD
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

This process has many problems such as equipment corrosion, environmental pollution, many side reactions, and complicated post-processing.

Method used

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  • Method for catalytic synthesis of raspberry ketone in presence of solid acid and alkali

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] KF / γ-A1 2 o 3 preparation of

[0034] Put the pretreated carrier into 30% KF aqueous solution, stir and impregnate at 60°C for 2h. Then put it into an oven and dry it at 110°C, grind it and transfer it to a muffle furnace, bake it at 550°C for 6 hours, and cool it for use.

Embodiment 2-4

[0035] Embodiment 2-4 is the synthesis of butanone alcohol

Embodiment 2

[0037] 107g of acetone and 5% catalyst were respectively added to the experimental device equipped with thermocouple and electromagnetic stirring. Heat to 55°C under stirring, start to add 15g of formaldehyde dropwise, and finish dropping within 30min. After 10 minutes of dripping and heat preservation reaction, the catalyst was filtered out and dried for later use. The reaction solution was distilled under reduced pressure at 70°C and 0.1 MPa to recover acetone to obtain the crude product of butanone alcohol, and then rectified, the yield of butanone alcohol was 57.5%.

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Abstract

The invention discloses a method for catalytic synthesis of raspberry ketone in the presence of solid acid and alkali. The method comprises the specific following steps: firstly, catalytically synthesizing butanone alcohol from formaldehyde and acetone which are used as raw materials in the presence of immobilized alkali KF / A12O3 serving as a catalyst; and secondly, catalytically synthesizing raspberry ketone from butanone alcohol and phenol which are used as raw materials in the presence of ion exchange resin D218 serving as a catalyst. The method is characterized in that solid acid and alkali are used for replacing traditional catalysts having strong corrosion, such as NaOH and H2SO4, has the advantages of high yield, low production cost, mild reaction conditions, small corrosion to the device, simple after-treatment, no 'three wastes' pollution and the like and is conductive to industrial production.

Description

technical field [0001] The invention relates to the technical field of organic chemical industry, in particular to a method for synthesizing raspberry ketone by solid acid-base catalysis. Background technique [0002] Raspberry ketone, also known as rubus ketone, chemically named 4-p-hydroxyphenyl-2-butanone, molecular weight: 164.22, melting point: 82-83°C, boiling point: 180°C / 1-2mmHg, insoluble in water, Soluble in ethanol, ether and volatile oil, it is white needle-like crystal or granular solid. It is a kind of spice with elegant and fruity aroma. In addition, it can also be used as an insect attractant in agriculture. Raspberry ketone naturally exists in raspberry fruit. However, the content of raspberry ketone in natural products is extremely low (0.11-0.12mg / kg), and basically has no industrial value. Commercial raspberry ketone is obtained by chemical synthesis. [0003] There are many synthetic methods for raspberry ketone. At present, the most economical route i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/245C07C45/68
Inventor 章晓朱凯张迁
Owner SHANDONG JIUXIN BIOLOGICAL TECH CO LTD
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