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Method for preparing 3-methoxy methyl propionate

A technology of methyl methoxypropionate and methyl acrylate, applied in the field of improvement of the method, can solve the problems of low product yield, large catalyst dosage, complicated refining process, etc., and achieves simple refining process and less catalyst dosage , the effect of improving product yield

Inactive Publication Date: 2005-08-31
CNPC JILIN CHEM GROUP CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The catalyst consumption of the above method is large, the refining process is complicated, and the product yield is low

Method used

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  • Method for preparing 3-methoxy methyl propionate
  • Method for preparing 3-methoxy methyl propionate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Synthesis of methyl 3-methoxypropionate

[0019] Add 32g of sodium methoxide with a concentration of 28% and 57g of methanol to a four-neck flask equipped with a stirrer, thermometer, constant pressure funnel, and reflux condenser, and slowly drip 86g of methyl acrylate over 12 hours under strong stirring. Add it into the said flask (methanol:MA=2.5:1mol), continue to react for 2 hours, and the reaction temperature is 55±2°C.

[0020] (2) Neutralization catalyst

[0021] Slowly add 8.3g of 98% concentrated sulfuric acid into the flask under cooling and stirring, and control the temperature of the system to ≤35°C, and the material in the flask is in a state of suspension.

[0022] (3) Recovery of unreacted materials and refining of products

[0023] The above-mentioned suspension was added to the tower kettle of the glass rectification tower (600mm high φ2×2θ mesh ring packing inside, produced by Tianda Tianjiu Technology Co., Ltd.), and the tower kettle was equipp...

Embodiment 2

[0025] 50.4g concentration is that the methyl alcohol of 28% liquid sodium methylate, 59.6g is added in the four-necked flask that stirrer, thermometer, constant pressure funnel, reflux condenser are equipped with, under vigorous stirring, with 10 hours, 86gMA (methanol: MA =3.0: 1mol), then reacted for 2 hours, and the reaction temperature was 45 ± 2°C, and all the other catalysts were neutralized, the recovery of unreacted materials, and the refining of the product were all the same as (2) and (3) in Example 1, and the product The yield was 86.4%.

Embodiment 3

[0027] The concentrated sulfuric acid that removes catalyst with 28% potassium methylate, neutralization catalyst is 6.4g, and all the other are all relevant parts with embodiment 1. The yield of methyl 3-methoxypropionate is 89.0% (the price of potassium methylate is 5 times higher than that of sodium methylate).

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Abstract

A process for preparing 3-methyl methoxypropionate includes proportionally adding methanol and sodium (or potassium) methoxide as catayst to reactor, stirring while reaction, adding MA, continuous reaction, cooling, stirring while adding concentrated sulfuric acid (or phosphonic acid ) to neutralize catalyst, and refining.

Description

technical field [0001] The present invention relates to a kind of preparation method of methyl 3-methoxy propionate, especially relate to the improvement of this method. Background technique [0002] The boiling point of methyl 3-methoxypropionate is 142-143°C. It is an important organic synthesis intermediate, fine chemical raw material, and organic solvent, and is widely used in the electronics industry, organic synthesis, adhesives and coatings industries, etc. [0003] The main preparation method of this product is methanol-methyl acrylate method. Generally, liquid sodium methoxide and methyl acrylate (MA) with a concentration of 28 to 32% are used as raw materials, and the addition reaction is carried out at 40±2°C; then hydrochloric acid or dilute sulfuric acid is used as a neutralizing agent to neutralize the sodium methoxide catalyst; finally Obtain target product 3-methoxypropionate methyl ester through distillation, yield is 77~88%, and i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/03C07C67/54C07C69/708
Inventor 田振生张吉波崔中文张启忠李志涛宋岩张钰董薇蒋巍刘辉
Owner CNPC JILIN CHEM GROUP CORP
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