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A technology of methyl methoxypropionate and methyl acrylate, which is applied in the field of improvement of the method, can solve problems such as complex refining process, low product yield, large catalyst consumption, etc., and achieve simple refining process, less consumption, Effect of Product Yield Improvement
Inactive Publication Date: 2006-06-07
CNPC JILIN CHEM GROUP CORP +1
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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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Embodiment 1
[0018] (1) Synthesis of methyl 3-methoxypropionate
[0019] Add 32 g of sodium methoxide with a concentration of 28% and 57 g of methanol to a four-necked flask equipped with a stirrer, thermometer, constant pressure funnel, and reflux condenser. Under vigorous stirring, slowly drop 86 g of methyl acrylate over 12 hours. Add to the flask (methanol: MA=2.5:1 mol), continue the reaction for 2 hours, and the reaction temperature is 55±2°C.
[0020] (2) Neutralization catalyst
[0021] 8.3g of 98% concentrated sulfuric acid is slowly added into the flask under cooling and stirring, and the temperature of the system is controlled to be ≤35°C, and the materials in the flask are in a state of suspension.
[0022] (3) Recovery of unreacted materials and refining of products
[0023] The above-mentioned suspension is added to the tower kettle of a glass distillation tower (filled with 600mm high Φ2×2θ mesh ring packing, produced by Tianda Tianjiu Technology Co., Ltd.), which is equipped wi...
Embodiment 2
[0025] Add 50.4g of 28% liquid sodium methoxide and 59.6g of methanol to a four-necked flask equipped with a stirrer, thermometer, constant pressure funnel, and reflux condenser. Under vigorous stirring, 86gMA (methanol:MA) =3.0:1mol), react for another 2 hours, the reaction temperature is 45±2℃, the rest of the catalyst is neutralized, the unreacted material is recovered, and the product is refined. All are the same as (2) and (3) in Example 1. The product The yield was 86.4%.
Embodiment 3
[0027] Except for the 28% potassium methoxide used for the catalyst and 6.4 g of concentrated sulfuric acid to neutralize the catalyst, the rest is the same as that of Example 1. The yield of methyl 3-methoxypropionate is 89.0% (the price of potassium methoxide is 5 times higher than that of sodium methoxide).
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Abstract
The invention relates to a method for preparing methyl 3-methoxypropionate. The molar ratio of raw material methanol to MA is 2.0 to 3.0:1, and sodium methoxide or potassium methoxide is used as a catalyst. 5.3~14.3%; first add the required amount of catalyst and methanol into the reactor, add the required MA into it for at least 10 hours under strong stirring, continue the reaction for 2~6 hours, and the reaction temperature is 45~60°C; the reaction is over Finally, under cooling and stirring, to the above reaction product, add concentrated sulfuric acid or 85% phosphoric acid to neutralize the catalyst in an amount of 1 / 2 or 1 / 3 of the molar amount of the catalyst, and maintain the temperature ≤ 35°C; Purified to obtain the target product. The mol ratio of this preparation method methyl alcohol and MA is 2.4-2.6: 1, and sodium methylate consumption is 10-11% (wt) of methanol amount, and reaction temperature is 54-56 ℃, and the reaction time is 14 hours, and wherein MA feed time is After 12 hours, the recovered product front fraction can be recycled, which has the advantages of high yield, simple refining and less catalyst consumption.
Description
Technical field [0001] The invention relates to a method for preparing methyl 3-methoxypropionate, in particular to the improvement of the 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, organic solvent, and is widely used in the electronics industry, organic synthesis, adhesives and coating industries. [0003] The main preparation method of this product is the methanol-methyl acrylate method. Generally, liquid sodium methoxide and methyl acrylate (MA) with a concentration of 28-32% are used as raw materials, and the addition reaction is carried out at 40±2℃; then, the sodium methoxide catalyst is neutralized with hydrochloric acid or dilute sulfuric acid as a neutralizer; and finally The target product, methyl 3-methoxypropionate, is obtained by distillation, with a yield of 77-88%. The chemical reaction formula is: [0004]...
Claims
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