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Preparation method of iodinated fatty acid ethyl ester with stable quality

A technology of fatty acid ethyl ester and stable quality, which is applied in the preparation of carboxylate, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of difficult to obtain stable iodinated fatty acid ethyl ester, difficult to remove, difficult to crystallize, etc. , to achieve the effect that the color is not easy to exceed the standard, the quality is improved, and it is not easy to produce

Active Publication Date: 2020-05-22
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, there are plans to freeze vegetable oil first, then iodide (CN201410851605); and further ethyl esterify on the basis of frozen vegetable oil, and then carry out iodination (CN105062693A) schemes, but these schemes use freezing technology to target crystallization Triglycerides, although some triglycerides also contain saturated fatty acids, but because it also includes unsaturated fatty acids, it may be difficult to crystallize and remove, and it is difficult to obtain iodinated fatty acid ethyl esters with high stability

Method used

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  • Preparation method of iodinated fatty acid ethyl ester with stable quality
  • Preparation method of iodinated fatty acid ethyl ester with stable quality

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Take 100g of linseed oil (Yihai Kerry Co., Ltd., the same below) and preheat it to 75°C in a sandwich reactor (Shanghai Shendi Glass Instrument Co., Ltd., the same below); add 35mL of absolute ethanol (Sinopharm Chemical Reagent Co., Ltd. Company, analytically pure, the same below) and 1g sodium methylate (Sinopharm Chemical Reagent Co., Ltd., analytically pure, the same below), reacted for 2h to obtain the reaction solution; the reaction solution was moved to a separatory funnel, and allowed to stand for stratification; take the upper layer Unreacted absolute ethanol was recovered by distillation under reduced pressure, washed with distilled water until neutral and dried to obtain linseed oil fatty acid ethyl ester.

[0040]Mix linseed oil fatty acid ethyl ester and absolute ethanol uniformly at a volume ratio of 1:1, transfer to a low-temperature reaction kettle (German LAUD, the same below), lower the temperature to -25°C at a rate of 1°C per hour, and continue Keep ...

Embodiment 2

[0049] Take 50g perilla oil (Hebei Jiafeng Vegetable Oil Co., Ltd., the same below) and 50g rapeseed oil (Yihai Kerry Co., Ltd., the same below) in a sandwich reactor, preheat to 70°C, add 40mL of absolute ethanol, add 1.5g sodium ethylate (Sinopharm Chemical Reagent Co., Ltd., analytically pure, the same below), reacted for 1.5h to obtain a reaction solution; the reaction solution was moved to a separatory funnel, allowed to stand for stratification, and the upper layer was distilled under reduced pressure to reclaim unreacted absolute ethanol, washed with distilled water until neutral and dried to obtain fatty acid ethyl esters (perilla oil: rapeseed oil = 1:1).

[0050] Mix the above-mentioned fatty acid ethyl ester and absolute ethanol evenly according to the volume ratio of 1:1.5, transfer it to a low-temperature reaction kettle, and lower it to -20°C at a cooling rate of 2°C per hour, and continue to maintain the temperature at -20°C±0.5°C Keep it for 7 days and repeat o...

Embodiment 3

[0058] Take 100g of walnut oil (Hebei Jiafeng Vegetable Oil Co., Ltd., the same below) in a sandwich reactor, preheat to 80°C, add 45mL of absolute ethanol, add 2g of sodium hydroxide (Sinopharm Chemical Reagent Co., Ltd., analytically pure, the same below) ), reacted for 1.5h to obtain a reaction solution; the reaction solution was moved to a separatory funnel, allowed to stand for stratification, and the upper layer was taken for vacuum distillation to reclaim unreacted absolute ethanol, and washed with distilled water to neutrality and dried to obtain walnut oil fatty acid ethyl ester.

[0059] Mix the above-mentioned walnut oil fatty acid ethyl ester and absolute ethanol evenly according to the volume ratio of 1:2, transfer it to a low-temperature reaction kettle, and lower it to -18°C at a cooling rate of 0.5°C per hour, and continue to cool at -18°C±0.5°C Maintain the temperature for 8 days and repeat 3 times; filter with Buchner funnel while it is cold to get walnut oil...

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Abstract

The invention discloses a preparation method of iodinated fatty acid ethyl ester with stable quality, and belongs to the technical field of organic synthesis. The method comprises the following steps:firstly, freezing fatty acid ethyl ester; and iodinating the frozen fatty acid ethyl ester to prepare the iodinated fatty acid ethyl ester with stable quality. After the freezing crystallization process is used, the quality of the prepared iodized fatty acid ethyl ester is greatly improved, the content of saturated fatty acid ethyl ester can be effectively reduced to 5% or below, free iodine is not likely to be separated out, the color is not likely to exceed the standard, and floccules are not likely to be generated.

Description

technical field [0001] The invention relates to a preparation method of iodized fatty acid ethyl ester with stable quality, belonging to the technical field of organic synthesis. Background technique [0002] Iodized fatty acid ethyl ester is obtained by addition of unsaturated fatty acid and iodine. According to the definition of USP30 edition, its iodine content is iodinated fatty acid ethyl ester of 35.2% ~ 38.9%; according to the definition of BP2007 edition, it is iodized fatty acid ethyl ester containing 37% ~ 39% of iodine, mainly used in organ contrast agent, iodine Deficiency, embolic agents, and antitumor drug carriers play an important role in clinical treatment. [0003] Iodized fatty acid ethyl esters can selectively accumulate in the liver cancer tissue area, and at the same time have an embolism effect on blood vessels, so they are often used as suspensions or carriers for liver tumor treatment drugs. At present, in China, the imported ultra-liquid iodinated...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/307C07C69/24
CPCC07C67/307C07C69/24
Inventor 刘元法杜彦鹏李进伟徐勇将翟颖红郑召君
Owner JIANGNAN UNIV
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