Method for preparating ethyl linoleate by catalysis of composite solid ultra-strong acid

A solid superacid and ethyl linoleate technology, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of high cost, damage, and product quality decline of solid superacids, and achieve Good industrial application prospects, good selectivity and high reactivity

Inactive Publication Date: 2008-03-12
HEILONGJIANG UNIV
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0003] However, the present industrialized method for producing ethyl linoleate is prepared by the esterification reaction of linoleic acid and absolute ethanol under the catalysis of concentrated sulfuric acid. This method has problems such as a large amount of acid waste water discharge and serious corrosion of production equipment. Moreover, due to the strong oxidizing properties of concentrated sulfuric acid, the unsaturated bonds in the linoleic acid molecule will be destroyed during the esterification reaction, resulting in a decrease in the iodine value of the product, a decrease in product quality, and SO 4 2- / TiO 2 Solid superacid catalysts are used as catalysts for the esterification of linoleic acid, and good results have been achieved. However, solid superacids have high cost and short service life, making it difficult to realize industrialization, and their application is limited.

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0016] Composite solid superacid catalyzed method for preparing ethyl linoleate, wherein composite solid superacid SO 4 2- / TiO 2 -SiO 2 The catalyst was prepared as follows, taking 4.88g (0.02mol) Ti(SO 4 ) 2 Dissolve in 20ml of distilled water to make a 1:4 (W / V) solution, add 28% ammonia solution dropwise under stirring, adjust to pH=9 to complete the reaction, and obtain amorphous Ti(OH) 4 Precipitate, then use 2mol / L HNO 3 The solution is adjusted and precipitated to PH = 3, and a certain amount of ethanol aqueous solution of ethyl orthosilicate is added dropwise at 80°C to obtain Ti(OH) with different molar ratios. 4 and Si(OH) 4 After the dropwise addition, continue to stir vigorously at room temperature for 1 hour, dry the obtained sol at 110°C, grind, sieve with a 100-mesh sieve, impregnate with 1mol / l sulfuric acid, suction filter, and dry dry, and finally fired at 450°C for 4 hours to obtain TiO 2 A series of compound SO with different contents 4 2- / TiO ...

Embodiment 2

[0023] The method for the preparation of ethyl linoleate by the composite solid superacid catalysis described in embodiment 1, in the reactor with water separator, condensation pipe, nitrogen protection device, thermometer and magnetic force stirring, add linoleic acid, Dehydrated alcohol and the TiO prepared by the method described in embodiment 1 2 Composite solid superacid SO with a mass percentage of 8.2% and regenerated after 5 uses 4 2- / TiO 2 -SiO 2 Catalyst, the amount of catalyst accounts for 3% of the linoleic acid quality, the mol ratio of linoleic acid and dehydrated alcohol is 1: 4, stirs under the protection of nitrogen, reacts under reflux temperature for 8 hours, isolates the product after cooling to room temperature, uses 0.1 The acid value of the sample was titrated with mol / L KOH standard solution, and the esterification rate of linoleic acid was calculated to be 90.2%.

Embodiment 3

[0025] Prepare SO by the method described in Example 1 4 2- / TiO 2 -SiO 2 Solid superacid catalyst, in which TiO 2 accounting for SO 4 2- / TiO 2 -SiO 2 The mass percentage content is 8.2%, and the Ti(OH) in the control catalyst preparation process4 and Si(OH) 4 The calcination temperature of the mixed sol was 500° C., other conditions for catalyst preparation were the same as those described in Example 1, and the calculated esterification rate of linoleic acid was 88.6%.

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Abstract

The present invention is a method of preparing the linoleic acid ethyl ester with the composite solid superacid catalyst. The production method the of linoleic acid ethyl ester in the existing industrialized production is the esterification reaction between the linoleic acid and the anhydrous ethanol ester with the concentrated sulfuric acid as the catalyst. The method has the problems of the large discharge of the acidic wastewater, the serious corrosion of the production equipment and so on. Therefore, the industrialized production urgently needs an environment-friendly solid acid catalyst. The method of preparing the linoleic acid ethyl ester with the composite solid superacid catalyst of the present invention is that the linoleic acid and the anhydrous ethanol with the molar ratio of 1 to between 1 and 10 are added into the reactor in order; the mixed solution is added with the SO42-/TiO2-SiO2, the composite solid superacid catalyst, whose weight is 1 to 10 percent of the weight of the linoleic acid; the mixed solution is stirred and heated with the protection of the nitrogen; the reaction is done for 2 to 10 hours at the return temperature of 40 DEG C; the solution is delaminated statically after the reaction; the products on the upper layer are decompressed and distilled under the pressure of minus 98.8 to minus 99.3 kPa; the distilled ingredients are collected at the temperature between 162 and 172 DEG C; then the refined inoleic acid ethyl ester can be got. The method of the present invention is suitable for the preparation of the linoleic acid ethyl ester in the industry.

Description

Technical field: [0001] The invention relates to a method for preparing ethyl linoleate, in particular to a method for preparing ethyl linoleate through esterification of linoleate catalyzed by a composite solid superacid. Background technique: [0002] Ethyl linoleate (9,12-octadecadienoic acid ethyl ester) is the main drug raw material for the prevention and treatment of heart and brain thrombosis, arteriosclerosis and other diseases. In the cosmetics industry, this product is used as a nutritional aid to accelerate the renewal of skin cells , whitening skin, and also has moisturizing, anti-allergic, conditioning and other functions, and has been widely used in the pharmaceutical industry, cosmetics industry, and health food industry. [0003] However, the present industrialized method for producing ethyl linoleate is prepared by the esterification reaction of linoleic acid and absolute ethanol under the catalysis of concentrated sulfuric acid. This method has problems suc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/587C07C67/08B01J27/053
Inventor 吴伟马方伟武光李凌飞黄娟
Owner HEILONGJIANG UNIV
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