Preparation method of methyl propionate

A technology of methyl propionate and propionic acid, applied in the field of preparation of methyl propionate, can solve the problems of not achieving ideal results, serious equipment corrosion, great environmental protection pressure, etc. less block effect

Inactive Publication Date: 2012-02-01
BEIJING RISUN TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this synthesis method is that due to the dehydration and strong oxidative properties of sulfuric acid, there are many side reactions in the reaction, serious equipment corrosion, and a large amount of "three wastes" discharge brings great environmental pressure.
Therefore, people have been devoting themselves to finding new catalysts that can replace concentrated sulfuric acid, such as ion exchange resins, Lewis acids, superacids and heteropolyacids, etc., but have not achieved ideal results.

Method used

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  • Preparation method of methyl propionate
  • Preparation method of methyl propionate
  • Preparation method of methyl propionate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] In a 500ml reactor, add 200g of propionic acid and 6g of catalyst a, then start heating, and continuously add a mixture of propionic acid and methanol to the reactor at a speed of 0.8mL / min, wherein the molar ratio of propionic acid to methanol It is 6:5. In this reaction rectification process, the reaction kettle is also a rectification tower tower tank at the same time. Two glass packing rectification columns are used to form a rectification tower. The number of theoretical plates is 16. The reflux ratio controller is used to adjust the reflux ratio R=3. Start the reactive distillation process. During this process, an azeotrope of methanol, water and the product methyl propionate was distilled overhead. The temperature in the kettle is 106-108°C, the temperature at the top of the tower is 71-74°C, and the material is discharged continuously for 120 hours. During the reactive distillation process, the components of the distillate remain stable. Chromatographic analys...

Embodiment 2

[0047] Add 180g propionic acid, 4g catalyst b in the reactor, all the other reaction conditions are with embodiment 1. The temperature in the kettle is 107-109°C, the temperature at the top of the tower is 73-76°C, and the material is discharged continuously for 160 hours. During the reactive distillation process, the components of the distillate remain stable. Chromatographic analysis determined that the content of methyl propionate in the reaction distillate was 90.26wt%, the content of methanol was 3.46wt%, and no propionic acid was detected; the water content was 6.28wt% as detected by coulometric titration. After the reaction finished, according to the weight and concentration of the weight of the reactant and the product, the yield of the available product methyl propionate was calculated to be 97.48%.

Embodiment 3

[0049] Add 150g propionic acid, 18g catalyst b in the reactor, form the rectification column with 3 glass packing rectification columns, the number of theoretical plates is 24, all the other reaction conditions are the same as embodiment 1. The temperature in the kettle is 108-110°C, the temperature at the top of the tower is 74-76°C, and the material is discharged continuously for 240 hours. The distillate components remain stable during the reactive distillation process. Chromatographic analysis determined that the content of methyl propionate in the reaction distillate was 92.38wt%, the content of methanol was 2.92wt%, and no propionic acid was detected; the water content was 4.70wt% as detected by coulometric titration. After the reaction, according to the weight of the reactant and the weight and concentration of the product, the yield of the available product methyl propionate is 99.35%.

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Abstract

The invention discloses a preparation method of methyl propionate. The method is characterized in that: propionic acid and methanol are reacted under the action of an acidic ion liquid catalyst to synthesize the methyl propionate. By the method, equipment corrosion can be reduced, and low-cost and large-scale production of the methyl propionate is realized.

Description

technical field [0001] The invention relates to a method for preparing methyl propionate, in particular to a method for synthesizing methyl propionate from propionic acid and methanol through an acidic ionic liquid catalyst. Background technique [0002] Methyl propionate is an important chemical product, which can be widely used as solvent, preservative, fragrance and organic synthesis intermediate. First of all, methyl propionate is an excellent additive, which is widely used in high-grade food and cosmetic solvents and preservatives; and various propionates can be prepared by saponification reaction, such as calcium propionate, sodium propionate, etc. , widely used as antiseptic additives for food and feed to replace preservatives widely used at present. Secondly, methyl propionate is also an important organic synthesis intermediate, which can be used to synthesize high-grade non-toxic artificial fragrances such as ethyl propionate, benzyl propionate, and isoamyl propion...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/24C07C67/08
Inventor 杨雪岗潘小君张英伟张敏生尹祖建高毅
Owner BEIJING RISUN TECH CO LTD
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