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Prepn process of iodized plant ethyl oleate

A technology of vegetable oil and oil ethyl ester, which is applied in the field of preparation of iodized vegetable oil ethyl ester, can solve the problems of poor thermal stability, low conversion rate of short-chain fatty alcohol, increased product cost, etc., and achieves mild reaction conditions and product stability Good, the effect of increasing the conversion rate

Active Publication Date: 2007-08-22
季珉
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 1. Lipase, but lipase is effective for the esterification or transesterification of long-chain fatty alcohols, and has a low conversion rate for short-chain fatty alcohols (such as methanol or ethanol, etc.), and methanol, ethanol and by-product glycerol are harmful to the enzyme Certain toxicity can easily inactivate the enzyme. Furthermore, because the lipase is expensive, the cost of the product will be increased [Yang Jiguo, Lin Weitie, Wu Junlin, Research Progress in Enzymatic Synthesis of Biodiesel, Chemical Environmental Protection, 2004, 24 (2) :6-120]
[0006] 2. Acid, the use of acid-catalyzed transesterification requires higher reaction temperature and longer reaction time, but iodized vegetable oil and iodized vegetable oil ethyl ester are iodides, which are relatively poor in thermal stability; and the method catalyst consumption Large, high alcohol-oil ratio will lead to higher production and recycling costs [Gao Yinyu, Chen Wenwei, Ruan Rongsheng, Lin Xiangyang, Chen Caiyong, Biodiesel Research Progress, Renewable Energy, 2004, (3) (Total No. 115): 6 -10】
[0008] The dynamic viscosity of iodinated vegetable oil for clinical injection is low, generally 34-70mPa·s, which requires a higher conversion rate of the transesterification reaction of iodinated vegetable oil. transesterification reaction to achieve this purpose, this process has not been reported in the literature at home and abroad

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1 (synthesis of iodized poppy seed oil ethyl ester):

[0023] 1. Synthesis of Iodized Poppy Seed Oil,

[0024] Raw material and source:

[0025] Poppy Seed Oil【Gansu Nongken Medicine and Medicinal Materials Station Vegetable Oil Factory】

[0026] Iodine Tablets 【Imported from Japan and repackaged by Wuhan Jiangbei Chemical Reagent Co., Ltd. Analytical Pure】

[0027] Red phosphorus [analytical pure from Tianda Chemical Reagent Factory, Dongli District, Tianjin]

[0028] Distilled water [self-made double distillation]

[0029] At 25°C, add 100g of iodine tablets and 15g of red phosphorus into the reactor, and slowly drop into 20mL (ie 20g) of distilled water. During this process, hydrogen iodide gas is generated, and the generated hydrogen iodide gas is passed into a device. Have in the reactor of 100g poppy seed oil, reaction time is 36 hours, obtains crude iodized poppy seed oil, washes 6 times with the ethanol that is equivalent to crude iodized poppy se...

Embodiment 2

[0037] Embodiment 2 (synthesis of iodized walnut kernel oil ethyl ester):

[0038] 1. Synthesis of iodized walnut kernel oil,

[0039] Raw material and source:

[0040]Walnut kernel oil【Dalian Ruifang Biochemical Products Co., Ltd.】

[0041] Iodine Tablets 【Imported from Japan Jiangbei Reagent Co., Ltd.】

[0042] Red phosphorus [analytical pure from Tianda Chemical Reagent Factory, Dongli District, Tianjin]

[0043] Distilled water [self-made double distillation]

[0044] At 0°C, add 100g of iodine tablets into the reactor, then slowly drop into a suspension containing 15g of red phosphorus and 20mL (ie 20g) of water, during which hydrogen iodide gas is generated, and the generated hydrogen iodide gas Pass in a reactor that 100g walnut kernel oil is housed, and the reaction time is 16 hours, obtains crude iodinated walnut kernel oil, washes 10 times with the ethanol that is equivalent to phase preparation iodized walnut kernel oil 1 / 8 volume, removes Free iodine, then was...

Embodiment 3

[0051] Embodiment 3 (synthesis of iodized peanut oil ethyl ester):

[0052] 1. Synthesis of iodized peanut oil,

[0053] Raw material and source:

[0054] Peanut oil 【Luhua Peanut Oil Co., Ltd.】

[0055] Iodine Tablets 【Imported from Japan and repackaged by Wuhan Jiangbei Chemical Reagent Co., Ltd. Analytical Pure】

[0056] Red phosphorus [analytical pure from Tianda Chemical Reagent Factory, Dongli District, Tianjin]

[0057] Distilled water [self-made double distillation]

[0058] At 40°C, add 100g of iodine tablets and 15g of red phosphorus into the reactor, slowly drop into 20mL (that is, 20g) of distilled water, during which hydrogen iodide gas is generated, and the generated hydrogen iodide gas is passed into a device In the reactor with 100g of peanut oil, the reaction time is 96 hours to obtain crude iodized peanut oil, wash 3 times with ethanol equivalent to 3 / 2 volume of crude iodized peanut oil, remove free iodine, and then use a concentration of 0.2mol / L sodi...

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Abstract

The present invention relates to preparation process of iodized vegetable oil ethyl ester. Iodized vegetable oil is first produced with vegetable oil and hydrogen iodide gas through addition reaction, and iodized vegetable oil and ethanol then produce ester exchange reaction under the action of alkali catalyst to produce iodized vegetable oil ethyl ester, with the hydrogen iodide gas being produced through reaction of iodine, red phosphorus and water. The present invention has facile cheap materials and high conversion rate of ester exchange reaction, and the product has low viscosity.

Description

technical field [0001] The invention relates to a preparation method of iodized vegetable oil ethyl ester. Background technique [0002] Contrast medium, also known as contrast medium, is one of the most commonly used diagnostic reagents in interventional radiology operations, mainly used for the display of blood vessels and body cavities. There are various types of contrast agents, and most of the contrast agents currently used in X-ray diagnostics are iodine-containing preparations, that is, the main component is iodine. The characteristic of iodine is that it is opaque to X-rays. Therefore, when taking X-ray films, the distribution of iodine in the body can be used to generate contrast; or to make blood vessels and soft tissues that are usually invisible on X-ray films clear, so as to assist doctors to make reliable decisions. diagnosis. Iodized vegetable oil ethyl ester is clinically called iodized oil ethyl ester, which is mainly used to diagnose liver diseases and tr...

Claims

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Application Information

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IPC IPC(8): C07C67/307C07C69/62
Inventor 奚江波柏正武尹传奇李世荣
Owner 季珉
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