A process for pressurized catalytic synthesis of high-purity dodecylnitrile

A high-purity technology of dodecyl nitrile, which is applied in the field of pressurized catalytic synthesis of high-purity dodecyl nitrile, can solve the problems of many intermediate products, low product purity, and high cost, and achieve the value of large-scale industrialization promotion, high product purity, and low cost. low effect

Active Publication Date: 2020-06-05
WUXI YINDA NYLON
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the shortcomings of this method are also very obvious: ①The product purity is not high, the finished product often contains crystals, and the total yield is low
② This method uses some conventional catalysts for dehydration, such as silica gel, γ-Al 2 o 3 etc., relatively more by-products, poor product color
[0008] (2) It is prepared by dehydration of lauric acid and ammonia or reacting with urea. Because this method does not use a catalyst, the reaction temperature is relatively high, there are more by-products, the total yield is low, and there are more intermediate products.
The products produced by this method have residual chemical solvents to varying degrees, and the relative cost is relatively high.

Method used

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  • A process for pressurized catalytic synthesis of high-purity dodecylnitrile
  • A process for pressurized catalytic synthesis of high-purity dodecylnitrile
  • A process for pressurized catalytic synthesis of high-purity dodecylnitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Put the raw material 1kg of lauric acid and 0.5% catalyst into the ammoniation reactor, heat up and melt at 170°C to pass through the ammonia: when starting to pass through the ammonia, pay attention to the flux of ammonia gas, probably controlled at about 35L / min, operate according to the time course, and control the temperature at 170°C in the early stage -190℃, pressure 1kg / cm 2 , time 1.5 hours; later stage temperature control 270-280 ℃, pressure 2kg / cm 2 , time 3 hours, 4.5 hours after the end of the reaction, sampling analysis (product purity detection adopts gas chromatography).

[0032] Catalysts are metal salts of zinc and molybdenum. The metal salt is sulfate, wherein the molar ratio of the metal salt of zinc to the metal salt of molybdenum is 1:1.

Embodiment 2

[0034] Put the raw material 1kg of lauric acid and 0.5% catalyst into the ammoniation reactor, heat up and melt at 170°C for ammonia flow: pay attention to the ammonia flux when starting the ammonia flow, and control it at about 40L / min, operate according to the time course, and control the temperature at 180°C in the early stage -190℃, pressure 1kg / cm 2 , time 1.5 hours; later stage temperature control 270-280 ℃, pressure 1.5kg / cm 2 , time 2.5 hours, 4.5 hours reaction finishes, sampling analysis (product purity detection adopts gas chromatography).

[0035] Catalysts are metal salts of zinc and molybdenum. The metal salt is phosphate, wherein the molar ratio of the metal salt of zinc to the metal salt of molybdenum is 1:3.

Embodiment 3

[0037] Put the raw material 1kg of lauric acid and 1% catalyst into the ammoniation reactor, heat up and melt at 170°C for ammonia flow: pay attention to the ammonia flux when starting the ammonia flow, control it at about 35L / min, operate according to the time course, and control the temperature at 180°C in the early stage -190℃, pressure 1kg / cm 2 , time 1 hour; later stage temperature control 270-280 ℃, pressure 2kg / cm 2 , time 2.5 hours, 3.5 hours after the end of the reaction, sampling analysis (product purity detection adopts gas chromatography).

[0038] Catalysts are metal salts of zinc and molybdenum. The metal salt is sulfate, wherein the molar ratio of the metal salt of zinc to the metal salt of molybdenum is 1:2.

[0039] The specific performance test is shown in Table 2.

[0040] Table 2

[0041] Example 1 Example 2 Example 3 melting point 3.7℃ 3.6℃ 3.8℃ content 98.5％ 99.2％ 98.5％

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Abstract

The invention relates to a process for synthesizing high-purity lauronitrile through pressurized catalysis, and belongs to the technical field of spice synthesis. According to the process, raw materials of lauric acid and catalysts are fed into an ammoniation reactor; temperature rise is performed for melting; nitrogen introduction starts; the pressure rise is controlled according to the time program; the temperature is controlled; after reaction, the final product of lauronitrile is obtained. The process has the advantages that the novel catalysts are used, pressurization, ammoniation and dehydration are performed by using the lauric acid as raw materials; the lauronitrile is produced by a one-step method; the product purity is high; the byproducts are few; the cost is low; great industrial popularization values are realized.

Description

technical field [0001] The invention relates to a process for pressurized catalytic synthesis of high-purity dodecyl nitrile, which belongs to the technical field of perfume synthesis. Background technique [0002] Lauryl nitrile, also known as lauryl nitrile, is a new type of fragrance that can replace lauric aldehyde, etc. It has the fruity aroma of citrus, grape, pomelo and lemon, and can be used as a raw material for soap, detergent and cosmetic essence. It is very stable within the range of neutral pH value and is widely used abroad. [0003] As far as prior art is concerned, dodecyl nitrile production method has following several kinds: [0004] (1) Using Litsea cubeba nucleolus oil as raw material, it is obtained through catalytic ammoniation dehydration, and its reaction formula is as follows: [0005] [0006] In this process, under the condition of normal pressure and 180-290°C, ammonia bubbling reaction is used to catalyze dehydration, and one-step method to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C253/20C07C255/03
CPCC07C253/20C07C255/03
Inventor 陈尚标沈俊毅胡瑞莉殷炼伟
Owner WUXI YINDA NYLON
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