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Preparation method for polyoxyethylene mono-caprylic-capric acid glyceride

A technology of glyceryl caprylate and polyoxyethylene, which is applied in the field of synthesis of nonionic surfactants in organic chemistry, can solve the problems of troublesome process, large environmental pollution, dark color, etc., and achieves convenient operation and simple reaction equipment , no pollution effect

Active Publication Date: 2014-08-13
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] It has been reported that alkali is used as catalyst to produce the crude product of glyceryl monocaprylyl caprate, and the color of the esterification product produced by alkali is very dark; the method of solvent recrystallization is used to purify glycerol monocaprylate, the process is very troublesome, and the environmental pollution is large

Method used

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  • Preparation method for polyoxyethylene mono-caprylic-capric acid glyceride
  • Preparation method for polyoxyethylene mono-caprylic-capric acid glyceride

Examples

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Effect test

Embodiment 1

[0015] 1) Esterification reaction: Add 644 grams of glycerin and 1036 grams of caprylic acid into a 2L flask by weight, add 0.336 grams of solid catalyst stannous chloride under stirring, slowly raise the temperature, and separate the esterification reaction in time under the condition of nitrogen flow The generated water was heated up to 180°C under the reaction conditions, kept warm for 3.0 hours, then cooled to 60°C, and discharged. The conversion rate of the acid was 99.9%.

[0016] 2) Purification of monocaprylic capric acid ester: use a rotary scraper thin film evaporator to collect about 700 grams of monocaprylic capric acid glycerides in light fractions at a temperature of 130 ° C and a pressure of 8 Pa, and the other fraction is dicaprylic capric acid glycerides by-product .

[0017] 3) Condensation reaction of ethylene oxide: Add 400 grams of monocaprylic capric acid glyceride into a 2L addition kettle, stir and add 7.6 grams of potassium hydroxide, replace with nitr...

Embodiment 2

[0020] 1) Esterification reaction: Add 644 grams of glycerin and 1085 grams of caprylic acid into a 2L flask by weight, add 0.5187 grams of solid catalyst stannous oxide under stirring, slowly raise the temperature, and separate out the esterification reaction in time under the condition of nitrogen flow. The water was heated up to 150°C under the reaction conditions, and kept for 6.0 hours, then cooled to 50°C and discharged, and the conversion rate of the acid was 99.8%.

[0021] 2) Purification of monocaprylic capric acid ester: use a rotary scraper film evaporator to collect about 750 grams of monocaprylic capric acid glycerides in light fractions at a temperature of 140 ° C and a pressure of 10 Pa, and the other fraction is dicaprylic capric acid glycerides by-product .

[0022] 3) Condensation reaction of ethylene oxide: add 400 grams of monocaprylic capric acid glyceride into a 2L addition kettle, stir and add 3.6 grams of sodium hydroxide, replace nitrogen three times ...

Embodiment 3

[0025] 1) Esterification reaction: Add 644 grams of glycerin and 1141 grams of caprylic acid in a 2L flask by weight, add 0.7140 grams of solid catalyst stannous chloride under stirring, slowly raise the temperature, and separate the esterification reaction in time under the condition of nitrogen flow The generated water was heated up to 160°C under the reaction conditions, kept warm for 5.0 hours, then cooled down to 70°C, and discharged. The conversion rate of the acid was 99.99%.

[0026] 2) Purification of monocaprylic acid ester: use a rotary scraper film evaporator to collect about 790 grams of monocaprylic acid glycerides in light fractions at a temperature of 135 ° C and a pressure of 12 Pa, and the other fraction is dicaprylic capric acid glycerides by-product .

[0027] 3) Ethylene oxide condensation reaction: Add 400 grams of monocaprylic capric acid glyceride into a 2L addition kettle, stir and add 2.4 grams of sodium hydroxide, replace nitrogen three times and the...

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Abstract

The invention discloses a preparation method of polyoxyethylene monocaprylic capric acid glyceride, comprising the following steps: 1) esterification reaction: using glycerol and caprylic capric acid as raw materials, adding a solid catalyst, separating water under nitrogen flow, and heating to 150 ℃ ℃-180℃, keep the temperature for 3-6h, then drop to 50-70℃; 2) Purify monocaprylic acid ester; 3) Condensation reaction of ethylene oxide: take the purified monooctanoic acid glyceride as raw material, add alkali After 20-40min, slowly introduce ethylene oxide for 3-5h, add and ripen, depressurize, cool down and degas the material to obtain the product. The present invention has the characteristics of reasonable process, high product purity and better use performance.

Description

technical field [0001] The invention relates to a preparation method of polyoxyethylene monocaprylic capric acid glyceride, which belongs to the technical field of synthesis of nonionic surfactants in organic chemistry. Background technique [0002] Polyoxyethylene monocaprylic acid glyceride is a polyol-type nonionic surfactant. It is a high-quality and efficient emulsifier with good emulsifying, dispersing and stabilizing effects. Glycerin has good softening, emulsifying, lubricating, antifogging, antistatic and solubilizing properties, low toxicity, little irritation to the skin, and easy degradation. It has a wide range of uses in the fields of food, medicine, cosmetics, and metal processing. In particular, this product is a colorless (or slightly yellow), odorless and highly hydrophilic food emulsifier. It has both good hydrophilic and lipophilic properties and acid resistance. With the improvement of oxirane , HLB value can reach a higher level. Because of its medium...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/28C07C69/30C07C67/29B01F17/42C09K23/42
Inventor 万庆梅金一丰王胜利刘志湘
Owner ZHEJIANG HUANGMA TECH
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