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Method for preparing benzalacetone under supercritical condition

A benzylidene acetone, supercritical technology, applied in the field of synthesis of benzylidene acetone, can solve the problems of long reaction time, low empty yield, low yield, etc., achieve shortened reaction time, increase reaction temperature and pressure, and high selectivity Effect

Active Publication Date: 2014-05-14
ZHEJIANG NHU CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the deficiency of this method is: the reaction time is long, and the yield of reaction is too low, only has 46.2%; Use a large amount of deionized water in the reaction, acetone and water miscible, and benzaldehyde is also soluble in water, exists very much in the separation process. Difficulty; at the same time, the reaction is realized through an autoclave, which is a batch reaction with low space-time yield and high energy consumption
If the reaction is amplified, there will be a huge problem in the equipment

Method used

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  • Method for preparing benzalacetone under supercritical condition
  • Method for preparing benzalacetone under supercritical condition

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Example 1 (eg figure 1 ): Turn on high-pressure metering pump 1, pump acetone A at a constant rate of 7ml / min, turn on high-pressure metering pump 2, pump benzaldehyde B at a constant rate of 1ml / min, set the temperature of preheater 3 at 250°C, and exceed The temperature of the critical pipeline reactor 4 is set at 350°C, the high-precision reverse pressure controller 6 behind the condenser 5 is adjusted, the pressure is controlled at 25±1MPa, and the reaction residence time is 20min. After the reaction was completed, the reaction solution was collected and analyzed by gas chromatography. With ethyl benzoate as the internal standard, the content of the calibrated benzylidene acetone was 20.3%, and the calculated selectivity of the benzylidene acetone was 96.3%.

Embodiment 2-6

[0019] According to embodiment 1, by changing the flow rate of pump 1, to change the molar ratio of benzaldehyde and acetone, keeping the conditions such as reaction temperature, preheater temperature, reverse pressure constant, the following results are obtained after the reaction (Table 1):

[0020] Table 1, the influence of raw material ratio on reaction

[0021]

Embodiment 7-12

[0023] According to Example 1, only the temperature of the pipeline reactor was changed, and the conditions such as pump flow rate, preheater temperature and reverse pressure were kept constant, and the following results were obtained after the reaction (Table 1):

[0024] Table 2. Effect of temperature on reaction

[0025] Example temperature Benzylidene acetone selectivity 7 300℃ 92.2% 8 320℃ 93.8% 9 340℃ 95.7% 10 360℃ 96.4% 11 390℃ 96.0% 12 420℃ 94.7% 13 450℃ 93.4%

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Abstract

The invention discloses a method for preparing benzalacetone under the supercritical condition. According to the conventional synthetic method, reaction is realized by an autoclave, and is intermittent, low in space time yield of the reaction and high in energy consumption. According to the method, the benzalacetone is prepared by performing the one-step condensation reaction of benzaldehyde and acetone which serve as raw materials under the supercritical condition, wherein the conversion rate of the benzaldehyde is over 99 percent, and the reaction yield of the benzaldehyde is over 92 percent. According to method, other solvents and acid or base catalysts are not needed to be added, the residual acetone can be recycled directly, so the method has the advantages of environment friendliness, no pollution, high selectivity and the like.

Description

technical field [0001] The invention relates to a method for synthesizing benzylidene acetone under supercritical conditions. Background technique [0002] Benzylideneacetone, white or light yellow crystal, flammable, easily soluble in sulfuric acid, ethanol, ether, benzene and chloroform, slightly soluble in water and petroleum ether. It has the smell of coumarin, the color becomes darker when exposed to light, and it is easy to decompose when heated for a long time. In nature, it mainly exists in hydrolyzed soybean or hydrogenated soybean protein. The United States "Food and Pharmacological Administration (FDA)" has awarded the chemical GAPS title and approved it as an edible spice. The chemical properties of the product are relatively stable, and it is an organic compound with a wide range of uses. It has a strong sweet pea-like aroma. In the spice industry, as a raw material for synthetic spices, benzylidene acetone is used to blend sweet pea series flavors and fruity...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/217C07C45/74
CPCY02P20/54
Inventor 毛建拥邓德福李浩然陈志荣
Owner ZHEJIANG NHU CO LTD
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