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Preparation of isotridecanol stearate

A technology of tridecyl ester and stearic acid, applied in the field of preparation of isotridecyl stearate, can solve the problems of a large amount of industrial waste water, corroded equipment, unfavorable environmental protection, etc., and achieves eliminating process operations, saving costs, and simplifying The effect of craftsmanship

Inactive Publication Date: 2011-09-21
上海华谊(集团)上硫化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyst used in this production method is sulfuric acid. Although it is cheap, there are many disadvantages. First, it is troublesome to discharge sewage. Because sulfuric acid is a catalyst and does not participate in the esterification reaction, a large amount of water will be consumed during washing, and a large amount of industrial waste water will be generated at the same time. , not good for the environment
In addition, sulfuric acid is a kind of strong acid, which will corrode the equipment and accelerate the aging of the equipment. Today, when environmental protection and ecological environment are emphasized, these shortcomings are urgently needed to be improved.

Method used

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  • Preparation of isotridecanol stearate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 270 grams of stearic acid, 200 grams of isotridecanol, 4.7 grams of solid sodium bisulfate, and 0.47 grams of hypophosphorous acid into the esterification kettle. Steam is introduced. When the temperature reaches 60°C, the materials are all dissolved and slowly opened. Temperature, the reaction temperature is kept at 115-120°C, the vacuum degree is controlled at 60mmHg column to 30mmHg column, the reaction time is 4 hours, sampling analysis shows that the acid value of the reaction solution is less than 4, and the qualified crude product is obtained, and the qualified crude product is put into the dealcoholization kettle, according to Add sodium carbonate to the acid value, and carry out neutralization reaction under stirring. The reaction temperature is kept at 75°C to 80°C. The value is equal to 0.45. Input the neutralized reaction solution into the dealcoholization kettle, pass in steam, turn on the vacuum pump, keep the temperature at about 140°C, and the vacuum ...

Embodiment 2

[0022] In addition to putting 270 grams of stearic acid, 210 grams of isotridecanol, 4.8 grams of sodium bisulfate, and 0.48 grams of hypophosphorous acid into the esterification kettle, the temperature of the esterification reaction is 120-125 ° C, and the vacuum degree of the esterification reaction is controlled at 45 mmHg. Column left and right, except for the esterification reaction time of 4.5 hours, the remaining operating steps and reaction parameters are the same as in Example 1, and the acid value of the qualified product is equal to 0.45, the hydroxyl value is <5, and the yield is 93% by weight.

Embodiment 3

[0024] In addition to putting 270 grams of stearic acid, 240 grams of isotridecanol, 5.1 grams of sodium bisulfate, and 0.51 grams of hypophosphorous acid into the esterification kettle, the temperature of the esterification reaction was kept at 115-125 °C, and the vacuum degree of the esterification reaction was controlled at 30mmHg column, except the esterification reaction time of 5 hours, the remaining operation steps and reaction parameters are the same as in Example 1, and the acid value of the qualified product is equal to 0.27, the hydroxyl value<5, and the yield is 88% by weight.

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Abstract

The invention relates to a preparation method of isotridecyl stearate. The preparation method comprises the following steps: (1) esterification reaction: stearic acid, isotridecyl alcohol, and sodium hydrogen sulfate (a catalyst) and hypophosphorous acid (a stabilizer) are added to an esterification kettle and are communicated with steam to keep the esterification reaction with 60mm-30mmHg of vacuum degree at the temperature of 115-125 DEG C for 4-5 hours, therefore, an acceptable crude product is obtained with acid value less than 4; the crude product is imported to a dealcholization kettle and is added with sodium carbonate according to the acid value of the crude product for neutralization reaction at the temperature of 70-80 DEG C for 2 hours; when the reaction solution is cooled below 60 DEG C, the catalyst is precipitated in a solid manner and filtered, and the acid value of the filtrate is less than 0.5. (2) dehydration and dealcholization: the neutralization reaction solution is imported to the dealcholization kettle, and is provided with steam at the temperature of about 140 DEG C with the vacuum degree less than 15mmHg; then the water and the alcohol are steamed to obtain the acceptable product with the acid value less than 0.5 and with the hydroxyl value less than 5.

Description

technical field [0001] The present invention relates to a kind of preparation method of isotridecanthyl stearate, more precisely relate to a kind of stearic acid and isotridecanol as raw material, with sodium bisulfate as catalyst, hypophosphorous acid as color retaining agent The method for preparing isotridecyl stearate. Background technique [0002] Isotridecanthyl stearate is an important surfactant. It is widely used in cosmetics as an oily additive. It is also a solubilizer and chemical fiber oil agent. [0003] The traditional production method of isotridecanyl stearate is esterification of stearic acid and isotridecanol under the catalyst of sulfuric acid, followed by neutralization, dehydration and dealcoholization under high temperature and reduced pressure. The catalyst used in this production method is sulfuric acid. Although it is cheap, there are many disadvantages. First, it is troublesome to discharge sewage. Because sulfuric acid is a catalyst and does not ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08C07C69/24
Inventor 周月红唐勇炜
Owner 上海华谊(集团)上硫化工有限公司