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Sorbitan caprylate emulsifier

A technology of sorbitan caprylate and emulsifier, which is applied in the field of synthesis of sorbitan caprylate emulsifier, can solve the mass fraction, quality stability and color gap, the hydroxyl value is difficult to drop to the qualified range, and the quality of straight chain ester High scores and other issues, to achieve the effect of safety and mild performance, less fatty acid residue, and low ion content

Inactive Publication Date: 2017-05-31
ZHANGJIAGANG GREAT CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional one-step alkali-catalyzed process is mainly used in China. The products produced by this process have deep color, many by-products, low monoester mass fraction, mostly turbid state, and unstable quality.
The two-step synthesis process, esterification first and then etherification will easily lead to excessive esterification, high mass fraction of straight-chain esters, dark color, poor fluidity and poor transparency in liquid state, and it is difficult to reduce the hydroxyl value to the qualified range of the index. Especially in terms of product monoester, diester and polyester mass fraction, quality stability and color, there is still a certain gap compared with foreign countries.
However, due to the price of lipase and recycling problems, there is still a certain gap between it and industrialized production
[0004] At present, the research on sorbitan fatty acid esters mainly focuses on high carbon chain fatty acids such as lauric acid, palmitic acid, cocoic acid, oleic acid and stearic acid, and the synthesis method of sorbitan caprylate emulsifier is rarely reported.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Etherification: Add 1274kg of D-sorbitol and 1.274kg of sodium hypophosphite in sequence in the reaction kettle, and slowly heat up to 120°C. When the D-sorbitol starts to melt, stir slightly and keep warm until the melting is complete. Add 2.61kg of p-toluenesulfonic acid, continue to heat up to 160°C, and react at this temperature, distill off the water generated by the reaction. After reacting for 5 hours, the degree of etherification reaches 0.8, and cool the material to 60-90°C to obtain sorbus Tan crude product 1173.2kg;

[0024] (2) Esterification: Add 2.438kg of sodium hydroxide, 5.75kg of sodium hypophosphite, add 1059kg of octanoic acid with a mass fraction of 99%, connect the condensation reflux device, heat up to 150°C, and reflux for 3 hours to obtain an acid value of 30mgKOH / g of crude product.

[0025] (3) Deacidification: connect to the distillation device, adjust the amount of nitrogen gas to make the vacuum degree be -0.080~-0.085MPa, maintain th...

Embodiment 2

[0028] (1) Etherification: Add 1274kg of D-sorbitol and 2.5kg of sodium hypophosphite in sequence in the reaction kettle, and slowly heat up to 120°C. When the D-sorbitol starts to melt, stir it slightly and keep it warm until it melts completely. Add 4.5kg of phosphoric acid 85%, continue to heat up to 180°C, and react at this temperature, distill off the water generated by the reaction. After 6 hours of reaction, the degree of etherification reaches 1.0, and cool the material to 60-90°C to obtain sorbitan Crude product 1153.2kg;

[0029] (2) Esterification: Add 9.657kg of potassium hydroxide, 5.75kg of sodium hypophosphite, add 1677kg of octanoic acid with a mass fraction of 99%, connect the condensation reflux device, heat up to 150°C, and reflux for 3 hours to obtain an acid value of 28.9 mgKOH / g of crude product.

[0030] (3) Deacidification: connect to the distillation device, adjust the amount of nitrogen gas flow, make the vacuum degree be -0.080~-0.085MPa, maintain t...

Embodiment 3

[0033](1) Etherification: Add 1274kg of D-sorbitol and 1.274kg of sodium hypophosphite in sequence in the reaction kettle, and slowly heat up to 120°C. When the D-sorbitol starts to melt, stir slightly and keep warm until the melting is complete. Add 5.61kg of solid superacid, continue to heat up to 180°C, and react at this temperature, distill off the water generated by the reaction. After 10 hours of reaction, the degree of etherification reaches 1.2, and cool the material to 60-90°C to obtain Sorbitan Crude product 1089.2kg;

[0034] (2) Esterification: Add 5.68kg of sodium hydroxide, 7.35kg of sodium hypophosphite, add 1950kg of octanoic acid with a mass fraction of 99%, connect the condensation reflux device, heat up to 150°C, and reflux for 3 hours to obtain an acid value of 30mgKOH / g of crude product.

[0035] (3) Deacidification: connect to the distillation device, adjust the amount of nitrogen gas to make the vacuum degree be -0.080~-0.085MPa, maintain the temperatu...

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Abstract

The invention aims to provide a synthesis method of sorbitan caprylate emulsifier. The synthesis method is characterized by comprising the following steps: taking commercially available D-sorbitol and caprylic acid as raw materials, performing etherification and esterification, then vacuumizing, adding water, vacuumizing according to the vapor distillation principle, deacidifying in vacuum through a falling film evaporator to remove the caprylic acid, and finally adsorbing through granular magnesium silicate to prepare the sorbitan caprylate emulsifier. According to the invention, the material addition and proportioning in the reaction process are reasonably adjusted, the reaction temperature and time in deacidification and other working procedures are optimally selected, and the process is reasonable and simple to operate. The sorbitan caprylate emulsifier prepared by the invention is faint in smell, light in color, high in transparency, low in acid value, low in fatty acid residue, low in sodium ion content, less prone to acidification and favorable in stability; and meanwhile, the sorbitan caprylate emulsifier has the advantages of solubilization, emulsification assistance, tackification, corrosion resistance synergy, safe and mild performance and favorable compatibility, thereby being applicable to the fields of daily chemical cosmetics and the like.

Description

Technical field [0001] The invention relates to a method for synthesizing a sorbitan octanoate emulsifier and belongs to the technical field of synthesis of ester compounds in organic chemistry. Background technique [0002] Sorbitan fatty acid ester is often used as W / O emulsifier. It is an important nonionic surfactant with excellent emulsification and dispersion properties. In addition, it is non-toxic, non-irritating, low volatile and has no unpleasant odor. It has the characteristics of high critical micelle concentration and low micelle free energy, and can be widely used in petroleum, textile, plastics, pesticides, food, cosmetics, medicine and other industries. [0003] Sorbitan fatty acid ester products appeared in 1940. The earliest preparation method was direct esterification of sorbitol and fatty acids in a certain proportion in the presence of alkali / acidic catalysts at high temperatures. The U.S. I.C.I.A.M (formerly Atlas PowderCo.Lta ) company, first develope...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/20B01F17/42C09K23/42
CPCC07D307/20C09K23/00
Inventor 朱红军徐由江盛绕郭静波崔宜斌陆菲菲张海平朱志乾
Owner ZHANGJIAGANG GREAT CHEM
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