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Preparation method of 3-(1-ethylpropoxy)propionic acid-1-ethylpropyl ester

A technology of ethyl propoxy and ethyl propyl ester, applied in the preparation of carboxylate, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problem of low gloss, poor leveling performance, and unsatisfactory requirements And other issues

Inactive Publication Date: 2019-05-10
SHAOGUAN HEZHONG CHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to increase the production capacity of some coil baking paint lines, the baking time is required to be several minutes, and the baking temperature is more than 200 degrees. When only propylene carbonate, ethylene carbonate and other solvents with low boiling points are used, the leveling performance is not good. The gloss is not high enough to meet the requirements. Using 1-ethylpropyl 3-(1-ethylpropoxy)propionate can also solve this problem

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 3-(1-ethylpropane)oxypropanoic acid-1-ethylpropyl ester, its preparation method is as follows:

[0025] (1) First add 128 parts (mass percentage) of 1-ethylpropyl acrylate and 96 parts of 1-ethylpropanol, heat to 45 degrees, add dropwise 10% isopropanol solution of sodium 1-ethylpropoxide 6 gram, after reacting to 1-ethylpropyl acrylate content less than 1%, cool down to 60 degrees;

[0026] (2) Add acetic acid to the mixture obtained in step (1) to neutralize until the acid value is 0.8 mgKOH / g, vacuum distill off 1-ethyl propanol to a concentration of less than 1%, and cool down to 60 degrees;

[0027] (3) Add 5% sodium carbonate aqueous solution to neutralize to acid number 0.3mgKOH / g in the mixture obtained in step (2), leave standstill, layering, separate the water layer;

[0028] (4) Heating the mixture obtained in step (3), vacuum distillation to remove light components until the concentration of 3-(1-ethylpropoxy)propionate-1-ethylpropyl in the distillate reach...

Embodiment 2

[0030] 3-(1-ethylpropoxyl) propionate-1-ethylpropyl ester, its preparation method is as follows:

[0031] (1) First add 128 parts (mass percentage) of 1-ethylpropyl acrylate and 88 parts of 1-ethylpropanol, heat to 45 degrees, drop 10% 1-ethylpropanol sodium 1-ethylpropoxide 8 grams of alcohol solution, after reacting to 1-ethylpropyl acrylate content less than 1%, cool down to 60 degrees;

[0032] (2) Add acetic acid to the mixture obtained in step (1) to neutralize until the acid value is 0.8 mgKOH / g, vacuum distill off 1-ethyl propanol to a concentration of less than 1%, and cool down to 60 degrees;

[0033] (3) Add 5% sodium carbonate aqueous solution to neutralize to acid number 0.3mgKOH / g in the mixture obtained in step (2), leave standstill, layering, separate the water layer;

[0034] (4) Heating the mixture obtained in step (3), vacuum distillation to remove light components until the concentration of 3-(1-ethylpropoxy)propionate-1-ethylpropyl in the distillate reach...

Embodiment 3

[0036] 3-(1-ethylpropoxyl) propionate-1-ethylpropyl ester, its preparation method is as follows:

[0037] (1) First add 128 parts (mass percentage) of 1-ethylpropyl acrylate and 82 parts of 1-ethylpropanol, heat to 45 degrees, drop 10% 1-ethylpropanol sodium 1-ethylpropoxide 9 grams of alcohol solution, after reacting to 1-ethylpropyl acrylate content less than 1%, cool down to 60 degrees;

[0038] (2) Add acetic acid to the mixture obtained in step (1) to neutralize until the acid value is 0.8 mgKOH / g, vacuum distill off 1-ethyl propanol to a concentration of less than 1%, and cool down to 60 degrees;

[0039] (3) Add 5% sodium carbonate aqueous solution to the mixture obtained in step (2) to neutralize to an acid value of 0.2mgKOH / g, leave standstill, layering, and separate the water layer;

[0040] (4) Heating the mixture obtained in step (3), vacuum distillation to remove light components until the concentration of 3-(1-ethylpropoxy)propionate-1-ethylpropyl in the distill...

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Abstract

The invention relates to a preparation method of 3-(1-ethylpropoxy) propionic acid-1-ethylpropyl ester, which includes the following steps: firstly, adding acrylic acid 1-ethylpropyl propyl ester and1-ethylpropanol, heating to the required reaction temperature, dropping catalyst solution, reacting to the required conversion of 3-(1-ethylpropoxy) propionic acid-1-ethylpropyl ester, cooling, and adding acid substance to neutralize, removing 1-ethyl propanol until the concentration meets the requirement by vacuum distillation, cooling and adding alkaline aqueous solution to neutralize to neutral, standing, stratifying, separating water layer, heating and removing light components until distillate meets the requirements by vacuum distillation, and finally collecting products. In the preparation process of 3-(1-ethylpropoxy)propionic acid-1-ethylpropyl ester, suitable reaction temperature, catalyst and droplet acceleration, distillation vacuum and temperature are selected, and thus, the best yield of the product is achieved.

Description

technical field [0001] The invention relates to a preparation method of 1-ethylpropyl 3-(1-ethylpropoxy)propionate, which belongs to the technical field of organic solvent synthesis. technical background [0002] At present, the solvents with high boiling point on the market include propylene carbonate and ethylene carbonate, both of which have a boiling point of more than 240 degrees, but they are polar solvents, which have poor solubility for many high-temperature resins, paints, inks, ceramic materials, etc. When the amount added is small, the viscosity of the paint and the viscosity of the ceramic raw material cannot be well reduced, and a large amount must be added to meet the viscosity requirement. The market needs some high-boiling point solvents that are not too polar and have good solubility. Therefore, a less toxic solvent, 3-(1-ethylpropoxy) propionate-1-ethylpropyl ester, has been developed. Its boiling point is higher than that of propylene carbonate and ethylen...

Claims

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Application Information

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IPC IPC(8): C07C67/31C07C69/708
Inventor 陈有权康伦国姚东生阳京辉
Owner SHAOGUAN HEZHONG CHEM CO LTD
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