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Method for preparing lemonile by using citral and device of preparation method

A production method and technology of citral, which are applied in the production method and device field of citral for preparing citric nitrile, can solve the problems of citral double bond oxidation side reaction, high energy consumption of repeated condensation, high ammoniation reaction temperature, etc., and achieve product The effect of good quality, low production cost and low reaction temperature

Inactive Publication Date: 2012-09-19
CENTRAL SOUTH UNIVERSITY OF FORESTRY AND TECHNOLOGY
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  • Abstract
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  • Application Information

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Problems solved by technology

The raw materials hydroxylamine hydrochloride and hydroxylamine sulfate used in this synthesis process have the disadvantages of strong corrosiveness, high toxicity, and expensive reagents, and a large amount of waste water is generated during the production process, causing serious environmental pollution.
[0004] Another method introduced by Zheng Hailin et al. (One-step catalytic ammoniation method for the synthesis of new international spices-lemon eyes, Journal of Guangxi University 1996, (21) 4:383-386) is a method for the synthesis of lemon eyes by gas phase ammoniation. This method requires lemon Repeated gasification of aldehydes and repeated condensation of reaction products consumes a lot of energy, and the ammoniation reaction temperature is high, and citral is prone to double bond oxidation side reactions

Method used

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  • Method for preparing lemonile by using citral and device of preparation method
  • Method for preparing lemonile by using citral and device of preparation method
  • Method for preparing lemonile by using citral and device of preparation method

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Embodiment 1

[0021] Embodiment 1: the production device embodiment of citral preparation citric nitrile

[0022] refer to figure 1 , the production plant embodiment that citral of the present invention prepares citric nitrile mainly consists of isopropanol storage tank 1, citral storage tank 2, ammonia water storage tank 3, hydrogen peroxide storage tank 4, ethyl acetate storage tank 5, oxygen storage tank 6, Ammonia storage tank 7, air pump 8. Air pump 9. Reaction tank 10. Conveyor pump 11. Extraction tank 12, oil-water separator 13, intermediate storage tank 14, feeding pump 15. Distillation tower 16. Condensation cooler 17. Ethyl acetate recovery tank 18. Condensation cooler 19. Composition of product storage tank 20, heating, cooling and vacuum systems. The outlets of isopropanol storage tank 1, citral storage tank 2, ammonia water storage tank 3, and hydrogen peroxide storage tank 4 are respectively connected to the top inlet of reaction tank 10, and the bottom outlet of r...

Embodiment 2

[0027] The present embodiment provides a kind of production method that citral prepares citric nitrile, comprises the following steps:

[0028] (1) Ammonification reaction: Add 30 kg of activated CuCl catalyst in the reaction tank 10, open the discharge valve at the lower part of the citral storage tank 2, add 1000 kg of citral to the reaction tank 10, and start the reaction tank 10 agitator, open the discharge valve at the lower part of the isopropanol storage tank 1 at the same time, add 4000 kg of isopropanol to the reaction tank 10 to dissolve citral; , slowly add ammonia water with a mass fraction of 20%, and control the amount of ammonia water added to be the number of moles of ammonia: the number of moles of citral is 1.1. After the addition is completed, react for 30 minutes to end the ammoniation reaction.

[0029] (2) Oxidation reaction: Adjust the temperature of the material in the reaction tank 10 to -10°C, open the lower valve of the hydrogen peroxide storage tank...

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Abstract

The invention relates to a method for preparing lemonile by using citral and a device of preparation method. The citral serves as a raw material and is subjected to ammoniation reaction and oxidation reaction to produce the lemonile under the action of catalysts. The invention also discloses the device of the method which prepares the lemonile by using the citral. A plurality of raw material tanks are connected in the device so as to achieve continuous production, and simultaneously reaction tanks and extraction tanks are arranged and provide further preferred conditions for related reaction. By the aid of the method, the produced lemonile is low in cost, little in waste gas, waste water and waste residues, high in purity and the like. The process is simple in operation, easy to control and convenient for production scale enlargement.

Description

technical field [0001] The invention relates to the preparation of citric nitrile, in particular to a production method and a device for preparing citric nitrile from citral. Background technique [0002] Citrinitrile fragrance has the advantages of specific fragrance, strong and long-lasting, stable chemical properties, etc. It is especially suitable for adding fragrance to alkaline media such as shampoo soaps and detergents. It is non-toxic and non-irritating to the human body, and can be used as a chemically unstable Inexpensive and high-quality alternatives to aldehyde fragrances. Citrilonitrile is also a synthetic 2,6-dimethyl-7-cyano-3,6-dieneheptanol-2 acetate and 2-methyl-6-formyl-1,5-dieneheptanol Acetate of -3 is the raw material of two spices, and the raw material of synthetic drugs vitamin A and vitamin E, which has a broad market. [0003] At present, the process of synthesizing citric nitrile from citral mainly adopts hydroxamin oximination method: such as ci...

Claims

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Application Information

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IPC IPC(8): C07C255/07C07C253/26
Inventor 黎继烈
Owner CENTRAL SOUTH UNIVERSITY OF FORESTRY AND TECHNOLOGY
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