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Preparation method of 3-amyl penoxy propionate

A technology of pentyloxypentyl propionate and pentyl acrylate, which is applied in the field of preparation of 3-pentyloxypentyl propionate, and can solve problems such as poor leveling performance, failure to meet requirements, and low gloss

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, and the use of 3-pentyloxypentyl propionate can also solve this problem

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 3-pentyloxy pentyl propionate, its preparation method is as follows:

[0025] (1) First add 128 parts (mass percentage) of amyl acrylate and 96 parts of amyl alcohol, heat to 45 degrees, add dropwise 6 grams of amyl alcohol solution of 10% sodium amyl alcohol, and react until the amyl acrylate content is less than 1%. Cool down to 60 degrees;

[0026] (2) Add acetic acid to the mixture obtained in step (1) to neutralize to an acid value of 0.8 mgKOH / g, vacuum distill pentanol 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), and vacuum distilling to remove light components until the concentration of 3-pentyloxypentyl propionate in the distillate reaches 99.5%, the water content is less than 0.05%, and the acid value is...

Embodiment 2

[0030] 3-pentyloxy pentyl propionate, its preparation method is as follows:

[0031] (1) First add 128 parts (mass percentage) of amyl acrylate and 88 parts of amyl alcohol, heat to 45 degrees, add 8 grams of amyl alcohol solution of 10% sodium amyl alcohol dropwise, and react until the amyl acrylate content is less than 1%. Cool down to 60 degrees;

[0032] (2) Add acetic acid to the mixture obtained in step (1) to neutralize to an acid value of 0.8 mgKOH / g, vacuum distill pentanol 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), and vacuum distilling to remove light components until the concentration of 3-pentyloxypentyl propionate in the distillate reaches 99.5%, the water content is less than 0.05%, and the acid value is...

Embodiment 3

[0036] 3-pentyloxy pentyl propionate, its preparation method is as follows:

[0037] (1) First add 128 parts (mass percentage) of amyl acrylate and 82 parts of amyl alcohol, heat to 45 degrees, add 9 grams of 10% amyl alcohol solution of sodium amyl alcohol dropwise, and react until the amyl acrylate content is less than 1%. Cool down to 60 degrees;

[0038] (2) Add acetic acid to the mixture obtained in step (1) to neutralize to an acid value of 0.8 mgKOH / g, vacuum distill pentanol 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), and vacuum distilling to remove light components until the concentration of 3-pentyloxypentyl propionate in the distillate reaches 99.5%, the water content is less than 0.05%, and the acid...

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Abstract

The invention relates to a preparation method of 3-amyl penoxy propionate, which includes the following steps: firstly, adding amyl acrylate and amyl alcohol, heating to the required reaction temperature, dropping catalyst solution, reacting to the required conversion rate of 3-amyl penoxy propionate, cooling, adding acidic substance to neutralize, removing deamyl alcohol until the concentration meets the requirements 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-amyl penoxy propionate, 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 3-pentyloxypentyl 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—amyl 3-pentoxypropionate was developed. Its boiling point is similar to that of propylene carbonate and ethylene carbonate. It has good solubility for many hi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/31C07C67/48C07C69/708
Inventor 陈有权康伦国姚东生阳京辉
Owner SHAOGUAN HEZHONG CHEM CO LTD
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