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Preparation method of 3-ethoxyl ethyl propionate

A technology of ethyl ethoxy propionate and ethyl acrylate, applied in the field of preparation of ethyl 3-ethoxy propionate, can solve problems such as affecting production efficiency, increasing difficulty in processing, solvent recovery, etc., and improving production efficiency , The effect of reducing solvent recovery and consumption, and reducing by-products

Active Publication Date: 2012-06-27
LINHAI LIANSHENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] This scheme 3-ethoxy ethyl propionate yield reaches 90%, but because the acetonitrile used is made solvent, causes a large amount of solvents to need reclaiming, and catalyst is the potassium fluoride that is carrier with aluminum oxide, after reaction finishes Increased difficulty in postprocessing
The reaction time is as long as more than 20 hours, which will affect the production efficiency to a certain extent in the industrialization process, and the yield is low

Method used

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  • Preparation method of 3-ethoxyl ethyl propionate
  • Preparation method of 3-ethoxyl ethyl propionate
  • Preparation method of 3-ethoxyl ethyl propionate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Synthesis of 3-ethoxy ethyl propionate

[0031] Add 1.6g of sodium metal and 160g of ethanol to a four-necked flask equipped with an electric stirring device, a thermometer, a constant pressure dropping funnel and a reflux condenser, and slowly add 290g of ethyl acrylate dropwise under strong stirring for 1 hour. In the flask, the reaction was continued for 2 hours at a reaction temperature of 45±2°C.

[0032] (2) Neutralizer

[0033] Slowly add 7g of 98% concentrated sulfuric acid into the flask under cooling and stirring, and control the temperature of the system to ≤20°C, and the material in the flask is in a state of suspension.

[0034] (3) Recovery of unreacted materials and refining of products

[0035] The above-mentioned suspension is added in the tower still of glass rectification tower, open vacuum and carry out underpressure distillation (20mmHg), and agitator is housed in this tower still. Raise the temperature and heat until reflux appears at the to...

Embodiment 2

[0041] Add 1.5g of sodium metal and 175g of ethanol to a four-necked flask equipped with an electric stirring device, a thermometer, a constant pressure dropping funnel and a reflux condenser, and slowly add 290g of ethyl acrylate dropwise for 1 hour under strong stirring. In described flask, continue to react with 2 hours, and reaction temperature is 45 ± 2 ℃, all the other catalysts are neutralized, the recovery of unreacted material, the refinement of product are all the same as (2), (3) in embodiment 1 , The finished product yield is 89%, and the content is greater than 99%.

Embodiment 3

[0043] Reclaim product front cut 46g among the embodiment 1, wherein ethanol accounts for 61%, ethyl acrylate accounts for 7%, and product 3-ethoxy ethyl propionate accounts for 32%; Metal sodium 0.5g is first added to the four-necked flask described in Example 1, and the ethyl acrylate recovered and 145g of added fresh ethyl acrylate are slowly added dropwise to the flask under vigorous stirring for 1 hour, and continue Reaction with 2 hours, reaction temperature is 45 ± 2 ℃, and all the other catalysts are neutralized, the recovery of unreacted material, the refinement of product are all the same as (2) and (3) in embodiment 1, product 3-ethoxypropane Acetate ethyl ester yield is 92%, and total yield is 96.3% [(total yield %=the newly added 3-ethoxy ethyl propionate in the reaction generation 3-ethoxy ethyl propionate / raw material ) moles × 100%].

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Abstract

The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for preparing 3-ethoxy ethyl propionate. The method comprises a synthesizing step and a refining step, wherein the synthesizing step adopts ethanol and ethyl acrylate as raw materials to carry out addition under the action of a catalyst, and the catalyst adopts alkali metal or alkali alcoholate. The method has the following advantages: 1, the method adopts one of the raw materials as solvent to react, so as to reduce solvent recovery and consumption in the production process; 2, the reaction catalyst uses basic catalyst such as sodium metal and the like, so as to improve reaction yield greatly; 3, the dosage of the reaction catalyst is reduced to about 2 percent, so as to lower amountof salt greatly after the reaction is finished, and reduce byproducts; 4, the reaction time can be shortened to 3 hours, so as to improve production efficiency; and 5, fore zeolite obtained in distillation can be used for next reaction, so as to achieve circular application, so that the proposal reaches green chemical requirement.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a preparation method of ethyl 3-ethoxypropionate. Background technique [0002] Ethyl 3-ethoxypropionate (structural formula as shown below) is a colorless liquid with a special fragrance, with a boiling point of 169-171°C and is non-toxic to the human body. It is an important organic solvent and an intermediate in organic synthesis. It has good solubility for a wide range of coating polymers, can replace traditional alcohol ether and ether ester solvents and has better performance, and has a great role in the coating industry and microelectronics industry (photoresist remover, thinner). potential application market. [0003] [0004] Literature [Journal of Organic Chemistry, 39 (12), 1770-1; 1974; J.IndianChem.Soc., 23, 388-9] reports that the reaction is carried out according to the following scheme: [0005] [0006] This scheme uses ethyl 3-bromopropionate ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/708C07C67/31
Inventor 俞小鸥邓一建黄卫国王树敏
Owner LINHAI LIANSHENG CHEM
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