Process for preparing plant sterol ester

A technology for phytosterol esters and phytosterols, which is applied in the green field of chemical synthesis of phytosterol esters, can solve the problems of low catalyst activity and large dosage, and achieves the effect of easy preparation and green synthesis route

Inactive Publication Date: 2011-11-23
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problem that exists is that catalyst activity is low, and consumption is big (up to 10%), will realize 95% esterification rate, and required time is as long as 18 hours
However, the strong corrosiveness of sodium methoxide and the by-product methanol are undesirable in food production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～9

[0027] Embodiment 1~9 prepares fatty acid with soybean oil

[0028] Soybean oil is stored in a high-pressure reactor, add different volumes of distilled water, different types and qualities of antioxidants, nitrogen gas at the bottom for 10 minutes, and nitrogen gas at different temperatures to the desired pressure, heat preservation and pressure holding for 2 to 4 hours, Cool down, reduce temperature and reduce pressure. The product is separated by centrifugation, the water phase is removed, and the oil phase is dried with molecular sieves to obtain free mixed fatty acids. The degree of hydrolysis of oil was monitored by TLC method, and the final fatty acid was determined by gas chromatography. The data are shown in Table 1:

[0029] Reality

[0030] It can be seen from Table 1 that the degree of hydrolysis increases with the increase of temperature and pressure, but the high pressure increases the equipment cost significantly, and there is a safety problem, so i...

Embodiment 10～39

[0031] The synthesis of embodiment 10~39 sterol ester

[0032] Before the experiment, the sterol raw material was placed in an oven and dried overnight at 60 °C. Fatty acid raw materials are adsorbed and dehydrated by molecular sieve 3A. Weigh a certain mass of mixed phytosterol PS, add a predetermined mass of fatty acid into a 500mL beaker, blow nitrogen, heat the oil bath to melt the sample, then raise the temperature to the desired temperature, and keep it warm. Then, add an appropriate amount of catalyst, stir, and react for 3 to 12 hours. The intermediate process adopts TLC to monitor the esterification process, and the final product adopts GC to measure the degree of esterification. The amount of each reactant described and sterol esterification condition and esterification rate are as shown in table 2~3:

[0033] Table 2. Effect of catalyst and its dosage on the esterification of oleic acid and sterol

[0034] Reality

Shi

example

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Embodiment 40

[0041]According to the esterification operation in Example 33, about 350 grams of the reaction solution were obtained. After the reaction was terminated, heat filtered, and the filtrate was transferred to a molecular still, and the vacuum pressure was 3 mmHg. Distilled at 120 ° C, and 65 grams of the light phase and 280 grams of the heavy phase were recovered. Brown, add 2.8 g of activated carbon to the heavy phase, stir at 90° C. and 100 r / min for 2 hr, and heat filter to obtain 275 g of light yellow, clear and transparent sterol ester product.

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PUM

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Abstract

The invention relates to a preparation method of plant sterol ester, which comprises heating fatty acid and phytosterol to 120 to 180DEG C, dissolving, adding catalyst, controlling temperature at 120 to 180DEG C to process esterification for 5-12h, separating and purifying reaction solution to obtain plant sterol ester, wherein the weight ratio of the fatty acid and the phytosterol is 1-5;1, the catalyst is calcium oxide, magnesia or lanthanum oxide or relative mixture, the catalyst is 0.2-3% of the total phytosterol and fatty acid. The preparation method of plant sterol ester uses solvent-free system, while the synthesis route is environment-friendly, effective, simple and suitable for large-scale preparation and separation.

Description

technical field [0001] The invention relates to a preparation method of phytosterol esters, in particular to a green method for chemically synthesizing phytosterol esters in a solvent-free system. Background technique [0002] As we all know, cardiovascular and cerebrovascular diseases are the number one killer of human health, and high blood cholesterol is the most important risk factor for cardiovascular and cerebrovascular diseases. Therefore, blocking or reducing the absorption of cholesterol has become an effective way to prevent and treat cardiovascular and cerebrovascular diseases. Numerous clinical experiments have proved that phytosterols can significantly reduce the absorption of cholesterol and play a role in lowering blood cholesterol. Because it is derived from natural vegetable oil by-products, it has high safety (approved by the FDA as a GRAS substance in 1998), and is especially suitable for patients with mild hypercholesterolemia or added to food as a funct...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J9/00C07J75/00
Inventor 孟祥河潘秋月邵平孙培龙
Owner ZHEJIANG UNIV OF TECH
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