Synthetic method of 3-[2-(ethylhexyl)oxyl]-1,2-propandiol

A technology of octyloxyglycerin and a synthesis method, which is applied in the field of synthesis of daily chemical additives, can solve problems such as low yield, unfeasible economy, long reaction time, etc., and achieve easy large-scale production, good reaction repeatability, The effect of simple reaction process

Active Publication Date: 2017-09-29
HUBEI ARTEC CARBOHYDRATE CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Chinese patent application CN2014106267923 uses glycidyl ether and sodium acetate, strong base and water to react at 90-95 ° for 8-10 hours, and the yield is 84%. Not only the reaction time is long, but the yield is not high
After adding carboxylic acid (salt) to alkyl glycidyl ether, it is hydrolyzed under alkaline conditions, and it is easy to produce a large amount of self-polymer of alkyl glycidyl ether, which reduces the yield and is difficult to handle
[0005] Chinese patent application CN2015102399330 is a method for prepa

Method used

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  • Synthetic method of 3-[2-(ethylhexyl)oxyl]-1,2-propandiol

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Embodiment 1

[0034] In a 3-liter pressure-resistant reactor equipped with a magnetic stirrer and a thermometer, add 376.3 grams (99.0% of purity) of 2-ethylhexyl glycidyl ether, 267.9 grams of acetic anhydride (99.0% of purity), 10.2 grams of triethyl amine. While stirring, raise the temperature to 110-115° C., feed nitrogen, and keep the reaction pressure between 0.15-0.16 Mpa to react for 90 minutes. Lower the temperature to 70°C, and slowly add 50% sodium hydroxide solution within 30 minutes to 40 minutes to adjust the pH value of the system to be greater than 12. Continue to keep warm for 1 hour.

[0035] Stand for liquid separation, wash the oil phase with 5% ammonium chloride solution twice the volume of the oil phase, and then wash once with deionized water. The oil phase is rectified under vacuum, and if necessary, degassed to obtain the high-aging and high-yield octyloxyglycerin of the present invention. According to gas chromatography analysis, the purity is 99.12%, and the yie...

Embodiment 2

[0037] In a 3-liter pressure-resistant reactor equipped with a magnetic stirrer and a thermometer, add 376.3 grams (99.0% of purity) of 2-ethylhexyl glycidyl ether, 226.7 grams of acetic anhydride (99.0% of purity), 10.2 grams of triethyl amine. While stirring, raise the temperature to 115-120° C., feed nitrogen, and keep the reaction pressure between 0.15-0.16 Mpa to react for 90 minutes. Lower the temperature to 70°C, and slowly add 50% sodium hydroxide solution within 30 minutes to 40 minutes to adjust the pH value of the system to be greater than 12. Continue to keep warm for 1 hour.

[0038] Stand for liquid separation, wash the oil phase with 5% ammonium chloride solution twice the volume of the oil phase, and then wash once with deionized water. The oil phase is rectified under vacuum, and if necessary, degassed to obtain the high-efficiency, high-yield octyloxyglycerin of the present invention. According to gas chromatography analysis, the purity is 99.08%, and the y...

Embodiment 3

[0040] In a 3-liter pressure-resistant reactor equipped with a magnetic stirrer and a thermometer, add 376.3 grams (99.0% of purity) of 2-ethylhexyl glycidyl ether, 412.2 grams of acetic anhydride (99.0% of purity), 5.0 grams of triethyl amine. While stirring, raise the temperature to 115-120° C., feed nitrogen, and keep the reaction pressure between 0.15-0.16 Mpa to react for 90 minutes. Lower the temperature to 65°C, and slowly add 50% sodium hydroxide solution within 30 minutes to 40 minutes to adjust the pH value of the system to be greater than 12. Continue to keep warm for 1 hour.

[0041] Stand for liquid separation, wash the oil phase with 5% ammonium chloride solution twice the volume of the oil phase, and then wash once with deionized water. The oil phase is rectified under vacuum and degassed if necessary to obtain the high-aging and high-yield octyloxyglycerin of the present invention, which is analyzed by gas chromatography with a purity of 99.02% and a yield of...

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Abstract

The invention discloses a synthetic method of 3-[2-(ethylhexyl)oxyl]-1,2-propandiol, which relates to the field of synthesis of daily chemical additives. The invention aims at providing a synthetic method with high yield. According to the technical scheme, the synthetic method comprises the following steps: step 1: adding 1,2-epoxy-3-[(2-ethylhexyl)oxy]-propane and a catalyst into acetic anhydride, and reacting for 1 to 2h to obtain a midbody; step 2: adjusting the pH of the system to be 12 to 14, stirring for 1h, standing, and layering; and step 3: washing an oil phase by successively utilizing ammonium chloride solution and water, rectifying the oil phase, and obtaining the 3-[2-(ethylhexyl)oxyl]-1,2-propandiol. The synthetic method is used for preparing high-purity 3-[2-(ethylhexyl)oxyl]-1,2-propandiol.

Description

technical field [0001] The invention relates to the synthesis field of daily chemical additives, in particular to a synthesis method of octyloxyglycerin. Background technique [0002] Octyloxyglycerin (also known as ethylhexylglycerin, 3-[2-(Ethylhexyl)oxyl]-1,2-propandiol) is a new multifunctional cosmetic additive with antiseptic effect and moisturizing and deodorizing effect, especially As one of the most important representatives of "no added preservatives", it is used in combination with other polyols in daily chemical products, and has the functions of moisturizing skin care, antisepsis and deodorization, and has been widely used in the field of cosmetics. In particular, using the synergistic effect of octyloxyglycerin and other traditional preservatives can greatly reduce the amount of traditional preservatives added, reduce the toxicity of the preservative system, and significantly improve the safety of the human body. [0003] The main raw material of octyloxyglyce...

Claims

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Application Information

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IPC IPC(8): C07C43/13C07C41/26C07C41/42
CPCC07C41/26C07C41/42C07C43/13
Inventor 丁圣峰
Owner HUBEI ARTEC CARBOHYDRATE CHEM
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