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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  • Claims
  • Application Information

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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 p

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0025] Example 1: Weigh 1.2g of NaOH, 0.3g of Tween-40, and 210g of water, add them to a four-neck flask and stir evenly, then add 40g of Guangxi cinnamon oil (containing 80% cinnamaldehyde) 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 are separated, and the content of benzaldehyde and cinnamaldehyde in the oil phase is analyzed by a gas chromatograph. The yield of benzaldehyde is 44% by calculation.

[0026] The process of the present invention is used below in order to compare with the above results.

[0027] Weigh ethanolamine 100g, Na 2 CO 3 100g (analytical pure anhydrous), 5g of dodecyltrimethylammonium bromide, add 10Kg of water and mix evenly; add to the reaction vessel equipped with agitator, thermometer, condenser and dropping funnel The above mixed aqueous solution; add 1.85kg of cinnamon oil containing 80% cinnama...

Example Embodiment

[0029] Example 2: Using 2.5gNa 2 CO 3 Instead of 1.2 g of NaOH in Example 1, the rest is the same as in Example 1. The final yield of benzaldehyde is 48.3%.

[0030] Similarly, the process of the present invention is used to compare with the above results.

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

Example Embodiment

[0032] Example 3: Similar to Example 1, the difference is that dodecyltrimethylammonium bromide, tetradecyltrimethylammonium bromide, and cetyltrimethylammonium bromide are each 0.08g Instead of Tween-40 in Example 1, the rest is the same as in Example 1. The final yield of benzaldehyde is 49.0% (dodecyltrimethylammonium bromide), 49.2% (tetradecyltrimethyl Ammonium bromide), 49.5% (hexadecyltrimethylammonium bromide).

[0033] Similarly, the process of the present invention is used to compare with the above results.

[0034] Similar to Example 1, the difference is that the organic base is 60g diethanolamine, 40g triethanolamine, Na 2 CO 3 150g, 1g dodecyltrimethylammonium bromide is used as cationic surfactant, 16kg of water, 1kg of cinnamon oil, reaction temperature of 105°C, and cinnamon oil dripping time is controlled at 6 hours. The yield of benzaldehyde was 56.4%. When the organic base is 60g ethanolamine, 40g diethanolamine, Na 2 CO 3 80g, 3g tetradecyltrimethylammonium bro...

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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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