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Preparation method of sorbitan octoate

A technology of sorbitan and monocaprylate, applied in the field of preparation of daily chemical additives, can solve the problems of insufficient stability of the system, violent reaction, short time, etc., and achieves improved antiseptic and antibacterial effect, obvious synergistic effect, and a reaction process. simple effect

Inactive Publication Date: 2016-08-17
SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0008] In the past, the commonly used catalysts for dehydration of sorbitol were strong acid catalysts such as concentrated sulfuric acid and p-toluenesulfonic acid. Although the catalytic ability to the dehydration reaction was strong, the time to complete the dehydration (etherification) was too short and the reaction was violent, which made the system not stable enough. , it is difficult to control the removal of one molecule of water from sorbitol, and usually a large amount of sorbitol dehydrated from two or more molecules of water will be formed, which is very unfavorable for the preparation of sorbitan octanoate
[0009] Strong acid is a common esterification catalyst, although it has been reported that solid acid and heteropolyacid catalyst can be used for esterification catalysis, but for the high viscosity sorbitan monocaprylate product, catalyst separation is just very difficult; Equipment requirements are also higher

Method used

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  • Preparation method of sorbitan octoate
  • Preparation method of sorbitan octoate
  • Preparation method of sorbitan octoate

Examples

Experimental program
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Embodiment 1

[0030] Add 150 grams of sorbitol and 1.5 grams of phosphoric acid to a 500 ml flask equipped with a vacuum dehydration device, nitrogen inlet pipe and water separator, heat to 150°C-175°C for dehydration under nitrogen, and keep the vacuum at 5000-6000pa for 100 minutes; Then, 132.5 grams of octanoic acid and 2.65 grams of potassium carbonate were added to the flask, and the process was protected by nitrogen. At the same time, it took 60 minutes to heat up to 190 ° C, and continued to stir and react at a pressure of 4000 to 5000 Pa. After 30 minutes, the temperature was raised to 210 ° C to continue the reaction; Acid value, when the acid value is less than 6.0mgKOH / g, cool down to stop the reaction; filter the product to obtain a transparent light yellow crude product, the acid value of the product is 4.3mgKOH / g, the saponification value is 208mgKOH / g, and the content of sorbitan monocaprylate 61.5% (by weight), 21.3% of isosorbide (two anhydrous sorbitan) octanoate, and the r...

Embodiment 2( example 1

[0032] Embodiment 2 (instance 1 contrast, do dehydration and esterification catalyst with the vitriol oil)

[0033] Add 150 grams of sorbitol and 1.5 grams of concentrated sulfuric acid to a 500 ml flask with a vacuum dehydration device, nitrogen input pipe and water separator, heat to 150°C-175°C for dehydration with nitrogen gas, and keep the vacuum at 5000-6000pa for reaction 100min; then, add 132.5 grams of octanoic acid into the flask, protect the process with nitrogen, and at the same time raise the temperature to 190°C for 60min, continue stirring and reacting at 4000-5000pa, and continue to react after 30min at 210°C; then measure the acid value every 20min, when the acid value When the temperature is less than 6.0mgKOH / g, the temperature is lowered to stop the reaction; the product is filtered to obtain a brown crude product with peculiar smell. The acid value of the product is 3.2mgKOH / g, the saponification value is 193mgKOH / g, the content of sorbitan monocaprylate i...

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Abstract

The invention relates to a preparation method of sorbitan octoate. The preparation method includes: adding a dehydration catalyst into sorbitol for dehydration at 150-175 DEG C under nitrogen protection for a certain period of time, adding caprylic acid and an esterification catalyst, rising the temperature to 190-210 DEG C, and continuing the stirring reaction under the pressure of 4000-5000pa until the acid value and the saponification value meet the requirements; performing further molecular distillation to obtain the sorbitan octoate. The obtained sorbitan octoate is high in content and light in color, and tests prove that the sorbitan octoate is suitable for being used as the multifunctional additives of daily chemical products.

Description

technical field [0001] The invention belongs to the technical field of preparation of daily chemical additives, and relates to a preparation method of sorbitan monocaprylate (also known as sorbitan caprylate). Background technique [0002] Cosmetics are special products that come into direct contact with the human body. The stability and safety of the product not only involves the huge economic benefits of the enterprise, but also directly affects the personal safety and health of the users. At present, the internal quality of cosmetics on the market tends to be more and more natural raw materials, and eutrophication provides extremely favorable conditions for the reproduction and growth of microorganisms, which makes the antiseptic and antibacterial problems of cosmetics more serious. In the prior art, adding preservatives is the first choice for antisepsis and quality preservation in the cosmetics industry. Preservatives can kill or inhibit microbial activity, maintain th...

Claims

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Application Information

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IPC IPC(8): C07D307/20
CPCC07D307/20
Inventor 李程碑窦杰杨杰
Owner SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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