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Preparation method of isoamyl laurate

A technology of isoamyl laurate and lauric acid, which is applied in the preparation of carboxylate, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of peculiar smell, high acid value and high manufacturing cost of isoamyl laurate , to achieve the effect of low cost, low acid value and avoiding re-rectification

Inactive Publication Date: 2019-04-19
广州星业科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention provides a preparation method of isoamyl laurate, so as to at least solve the problems of high production cost, high acid value and peculiar smell of isoamyl laurate in the prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The preparation method of the embodiment of the present invention 1 isoamyl laurate is as follows:

[0024] Add lauric acid (400g, 2mol) and isoamyl alcohol (440g, 5mol) successively in the reaction flask with water separator, reflux condensing device and thermometer, heat and stir until lauric acid melts, add 5g of zinc methanesulfonate, three Zinc fluoroacetate 12.6g (mass ratio of zinc methanesulfonate:zinc trifluoroacetate=1:2.5, a total of 17.6g, 2%), after stirring at 125°C for 6 hours, no water came out. Distillation, keeping the system at -0.097mpa vacuum degree, the fraction distilled at 148-150°C is isoamyl laurate (acid value 0.02), and the yield is 99.5% (calculated by the molar amount of lauric acid).

[0025] Add lauric acid (400 g, 2 mol) and isoamyl alcohol (176 g, 2 mol) to the remaining liquid in the reaction flask, repeat the above process again, heat and stir until the lauric acid melts, and stir at 125°C for 6 h, no more water will come out. Distil...

Embodiment 2

[0028] The preparation method of the embodiment of the present invention 2 isoamyl laurate is as follows:

[0029] Add lauric acid (400g, 2mol) and isoamyl alcohol (220g, 2.5mol) successively in a reaction flask with a water separator, reflux condensing device, and thermometer, heat and stir until the lauric acid melts, and add 0.22g of copper methanesulfonate , copper trifluoroacetate 1.02g (mass ratio copper methanesulfonate: copper trifluoroacetate = 1:4.6, a total of 1.24g, 0.2%), after stirring at 130°C for 14h, no water came out. Distillation, keeping the system at -0.097mpa vacuum degree, the fraction distilled at 148-150°C is isoamyl laurate (acid value 0.04), and the yield is 99.2% (calculated by the molar amount of lauric acid).

[0030] Add lauric acid (400g, 2mol) and isoamyl alcohol (176g, 2mol) to the remaining liquid in the reaction flask, repeat the above process again, heat and stir until the lauric acid melts, and stir at 130°C for 14h and no water will come ...

Embodiment 3

[0033] The preparation method of the embodiment of the present invention 3 isoamyl laurate is as follows:

[0034] Add lauric acid (400g, 2mol) and isoamyl alcohol (352g, 4mol) successively in the reaction flask with water separator, reflux condensing device and thermometer, heat and stir until lauric acid melts, add manganese methanesulfonate 2g, three 5.52 g of copper fluoroacetate (manganese methanesulfonate: copper trifluoroacetate = 1:2.76, a total of 7.52 g, 1%), after stirring at 110°C for 10 hours, no water came out. Distillation, keeping the system at -0.097mpa vacuum degree, the distilled fraction at 148-150°C is isoamyl laurate (acid value 0.07), and the yield is 99.9% (in the chemical reaction, it can be considered that the yield reaches 100 %).

[0035] Add lauric acid (400g, 2mol) and isoamyl alcohol (176g, 2mol) to the remaining liquid in the reaction flask, repeat the above process again, heat and stir until the lauric acid melts, and stir at 110°C for 10h and...

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Abstract

The invention provides a preparation method of isoamyl laurate. The preparation method includes the following steps: S1, mixing lauric acid and isoamyl alcohol according to a molar ratio of 1:1.05-6,and heating and stirring the mixture until the lauric acid melts; S2, adding a catalyst which accounts for 0.1%-5% of the weight of the mixed solution, and performing a reaction under the condition ofmaintained 110-140 DEG C for 5-14 h; and S3, starting a vacuum pump, carrying out vacuum distillation by keeping the system under vacuum at -0.090--0.100 mpa, and collecting fraction of 140-150 DEG Cwhich is the isoamyl laurate, wherein the catalyst is a mixture of methanesulfonate and trifluoroacetate. The yield of the isoamyl laurate obtained by the synthetic method can be up to 100%. The preparation method of isoamyl laurate has the advantages of reasonable process, low cost, easy industrial production, no pollution and environmental protection, and is a simple, economical and environmentally friendly method for preparing isoamyl laurate. The provided isoamyl laurate has a wide range of applications in the cosmetics, food and wine industries and is an important fine chemical.

Description

technical field [0001] The invention relates to a method for preparing isoamyl laurate, in particular to a method for preparing isoamyl laurate with high yield and low acid value, belonging to the field of fine chemicals. Background technique [0002] Isoamyl laurate is one of the commonly used and important laurate esters. Isoamyl laurate is a colorless oily liquid with a faint ester, oily, woody, and yeasty aroma. It is used in the field of cosmetics as emollient oil. Natural products exist in beer, brandy, rum, whiskey, white wine, etc., and are allowed to be used as food spices. [0003] In the preparation process of existing isoamyl laurate, strong acid is commonly used to catalyze the preparation, but the acidity value in the isoamyl laurate obtained by distillation is higher (due to steaming out of unreacted lauric acid and strong acid) and there is peculiar smell (caused by strong acid). Organic raw material coking), need repeatedly rectifying, cause the isoamyl la...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08B01J31/04C07C69/24
CPCC07C67/08B01J31/0225B01J31/04B01J2231/49B01J35/19C07C69/24
Inventor 李方孟巨光李建莫林峰
Owner 广州星业科技股份有限公司
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