Process for preparing natural benzaldehyde

A benzaldehyde, natural technology, applied in the field of benzaldehyde, can solve the problems of difficult selection of a non-toxic phase transfer catalyst, lower naturalness of product benzaldehyde, immature industrialization conditions, etc., to avoid emulsification and increase reaction rate , The effect of reducing side effects

Inactive Publication Date: 2005-07-06
XIAMEN UNIV +1
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Problems solved by technology

But because the strong oxidizing property of ozone can make the natural degree of product benzaldehyde reduce (the price of natural benzaldehyde is 25-30 times of unnatural product), the productive rate of this method is not high in addition, and there is certain environmental protection problem, therefore There is no industrialization report in China
[0006] In the presence of a phase transfer catalyst, although the process for preparing benzaldehyde by alkaline hydrolysis of cinnamon oil has the advantages of shortening the reaction time, mild reaction conditions, and low production costs, it also has the disadvantages of low yield and difficult selection of a non-toxic Phase transfer catalysts and post-treatment of toxic phase transfer catalysts, etc., therefore, the industrialization conditions of this method are not yet mature

Method used

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  • Process for preparing natural benzaldehyde
  • Process for preparing natural benzaldehyde

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Experimental program
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Embodiment 1

[0025] Example 1: Take by weighing 1.2g of NaOH, 0.3g of Tween-40, and 210g of water, add to a four-necked flask and stir evenly, then add 40g of Guangxi cinnamon oil (containing cinnamaldehyde 80%) under stirring, and stir at a slow speed The temperature of the system was raised to 98° C., and the reaction was continuously stirred for 24 hours under reflux. Finally, the water phase and the oil phase were separated, and the content of benzaldehyde and cinnamaldehyde in the oil phase was analyzed by gas chromatography, and the yield of benzaldehyde was calculated to be 44%.

[0026] Adopt the technique of the present invention below, so that contrast with above-mentioned result.

[0027] Weigh ethanolamine 100g, Na 2 CO 3 100g (for analytically pure anhydrous matter), 5g of dodecyltrimethylammonium bromide, add in 10Kg water phase and mix uniformly; The above mixed aqueous solution; add 1.85 kg of cinnamon oil containing cinnamaldehyde 80% to the dropping funnel, and cover a...

Embodiment 2

[0029] Embodiment 2: with 2.5gNa 2 CO 3 Replace the 1.2gNaOH in the embodiment 1, all the other are the same as the embodiment 1, finally the yield of benzaldehyde is 48.3%.

[0030] Likewise, the process of the present invention was adopted in order to compare with the above-mentioned results.

[0031] Similar to Example 1, the difference is that the organic base adopts diethanolamine 100g, Na 2 CO 3120g, cationic surfactant adopts tetradecyltrimethylammonium bromide 2g and octadecyltrimethylammonium bromide 2g, water is 10.5kg, cinnamon oil is 1.2kg, reaction temperature is 102 ℃, cinnamon oil The instillation time was controlled at 8 hours. The yield of benzaldehyde was 57.5%.

Embodiment 3

[0032] Embodiment 3: similar to Example 1, the difference is that each 0.08g of dodecyltrimethylammonium bromide, tetradecyltrimethylammonium bromide, cetyltrimethylammonium bromide Replace the Tween-40 in embodiment 1, all the other are with embodiment 1, the yield that finally gets benzaldehyde is 49.0% (dodecyl trimethyl ammonium bromide), 49.2% (tetradecyl trimethyl ammonium bromide) ammonium bromide), 49.5% (hexadecyltrimethylammonium bromide).

[0033] Likewise, the process of the present invention was adopted in order to compare with the above-mentioned results.

[0034] Similar to Example 1, the difference is that the organic base adopts diethanolamine 60g, triethanolamine 40g, Na 2 CO 3 150g, the cationic surfactant adopts 1g of dodecyltrimethylammonium bromide, 16kg of water, 1kg of cinnamon oil, the reaction temperature is 105°C, and the dripping time of cinnamon oil is controlled at 6 hours. The yield of benzaldehyde was 56.4%. When the organic base adopts etha...

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Abstract

The preparation method of natural benzaldehyde relates to a kind of benzaldehyde, and provides a new method for preparing natural benzaldehyde by hydrolyzing cinnamon oil under alkaline conditions. Add water to organic base, Na2CO3, and cationic surfactant; heat the mixed aqueous solution, drop in cinnamon oil; condense and collect the product; when the amount of the collected oil phase is only 8% to 12% of the initial amount, stop adding water, when the benzaldehyde When the content is reduced to less than 10% and the cinnamaldehyde content is greater than 60%, the reaction is stopped. Avoid the polymerization and disproportionation reaction of products under strong alkaline conditions, and reduce the amount of benzene and toluene generated due to the existence of small molecule OH-. The use of cationic surfactant instead of nonionic surfactant avoids saponification and emulsification of the product, and the reaction rate is greatly improved. The side reactions such as polymerization and disproportionation of the product are directly reduced. The reaction time of the process is shortened; the yield of the main product of the reaction is increased.

Description

technical field [0001] The invention relates to a kind of benzaldehyde, in particular to a method for preparing natural benzaldehyde by hydrolyzing natural cinnamon oil under alkaline conditions. Background technique [0002] With the development of food and beverage industry, food additives have become an indispensable substance in people's daily life. The need for safety and deliciousness is the development direction of food additives. Therefore, natural benzaldehyde, which is the main raw material of food and beverage spices, is being widely used in industries such as food, beverage, health care products, and pharmaceuticals. According to incomplete statistics, one The annual natural benzaldehyde used in food flavors and flavors has reached as much as 500 tons. [0003] The traditional production method of natural benzaldehyde is to use nuts containing amygdalin as raw materials, and use special treatments such as steam distillation and alkaline washing to remove hydrocy...

Claims

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Application Information

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IPC IPC(8): C07C45/42C07C47/54
Inventor 陈良坦黄泰山朱建清赖桂勇
Owner XIAMEN UNIV
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