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Preparation method of sorbitan oleate servicing as medicinal auxiliary material

A technology of sorbitan and auxiliary oil, applied in the direction of organic chemistry and the like, can solve the problems of excessive water loss of sorbitol, dark product color, coking and other problems, and achieve the effects of simplifying the process, short reaction time and improving efficiency

Inactive Publication Date: 2013-05-08
HUBEI GEDIAN HUMANWELL PHARMA EXCIPENTS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In "Synthesis of High-Quality Sorbitan Monooleate" (Mao Lianshan, "Chemical Times", 2005, Volume 19, No. 5), it is mentioned that the method of first etherification and then esterification is used to prepare sorbitan monooleate. Oleate, but its etherification temperature is higher, 160-180°C, which may cause excessive dehydration of sorbitol and coking after long-term exposure to high temperature environment, resulting in darker color of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In a 250mL three-neck flask equipped with a thermometer, add 100g of solid sorbitol powder, stir, heat up to 95°C to melt, add 1g of sulfuric acid with a mass fraction of 20%, vacuumize to 0.01MPa, and heat up to 105°C for dehydration for 2.5h. Then lower the temperature to 30°C, neutralize with saturated calcium hydroxide solution, and filter to remove excess catalyst sulfuric acid. Add activated carbon for decolorization, filter to remove activated carbon, concentrate and dry to obtain 1,4-sorbitol.

[0023] In a 250mL three-neck flask equipped with a thermometer, a condenser tube and a nitrogen inlet tube, add 36g of 1,4-sorbitol, 74.3g of vegetable oleic acid with a mass fraction of 80% (the molar ratio of the two is 1:1.2) and 1.1g of sodium carbonate, blow nitrogen for 30min, stir and heat up to 200°C, esterification reaction for 4h. Cool down, add activated carbon for decolorization, filter, remove activated carbon, and obtain sorbitan oleate.

Embodiment 2

[0025] In a 250mL three-neck flask equipped with a thermometer, add 100g of pharmaceutical grade solid sorbitol powder, stir, heat up to 100°C to melt, add 1.5g of sulfuric acid with a mass fraction of 10%, vacuumize to 0.01MPa, heat up to 110°C for dehydration 2h. Then lower the temperature to 30°C, neutralize with saturated calcium hydroxide solution, and filter to remove excess catalyst sulfuric acid. Add pharmaceutical grade activated carbon for decolorization, filter to remove activated carbon, concentrate and dry to obtain 1, 4-sorbitol.

[0026] In a 250mL three-neck flask equipped with a thermometer, a condenser tube and a nitrogen inlet tube, add 36g of 1,4-sorbitol, 80.4g of vegetable oleic acid with a mass fraction of 80% (the molar ratio of the two is 1:1.3) and 1.16g of sodium carbonate, blow nitrogen for 30min, stir and heat up to 200°C, esterification reaction for 4h. Cool down, add pharmaceutical grade activated carbon for decolorization, filter, remove activ...

Embodiment 3

[0028] In a 250mL three-neck flask equipped with a thermometer, add 100g of solid sorbitol powder, stir, heat up to 100°C to melt, add 3g of sulfuric acid with a mass fraction of 30%, vacuumize to 0.01MPa, cool to 90°C for dehydration for 4h. Then cool down, neutralize with saturated calcium hydroxide solution, filter to remove excess catalyst sulfuric acid. Add activated carbon for decolorization, filter to remove activated carbon, concentrate, and dry to obtain 1, 4-sorbitol.

[0029] In a 250mL three-neck flask equipped with a thermometer, condenser tube and nitrogen inlet tube, add 36g of 1,4-sorbitol, 86.7g of oleic acid (the molar ratio of the two is 1:1.4) and 1.23g of sodium carbonate. Nitrogen was used to remove oxygen, the temperature was raised to 200°C with stirring, and the esterification reaction was carried out for 4 hours. Cool down, add activated carbon for decolorization, filter, remove activated carbon, and obtain sorbitan oleate.

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Abstract

The invention relates to a preparation method of sorbitan oleate servicing as a medicinal auxiliary material. The preparation method is characterized by comprising the following steps: adding powdered solid sorbitol into a reactor; stirring; heating to 80-105 DEG C to melt the powdered solid sorbitol; adding an acidic catalyst; agitating; dewatering at 90-110 DEG C at a vacuum condition; neutralizing the rest acidic catalyst after the reaction; filtering; decolouring; filtering; concentrating; drying to obtain 1,4-sorbitan; adding oleic acid into the reactor, the prepared 1, 4-sorbitan and a basic catalyst, wherein the mass ratio of the 1, 4-sorbitan to the oleic acid is 1:(2.06-2.41); pouring nitrogen and removing the oxygen; stirring and heating; carrying out esterification reaction at 190 to 210 DEG C; and then carrying out cooling, decolouring and filtering after the reaction so as to obtain the sorbitan oleate. The preparation method is simple in process and short in reaction time; the prepared product which is the sorbitan oleate is light in colour and high in purity; and the physicochemical performance of the sorbitan oleate meets the requirement of Section II of Pharmacopeia, Edition 2010.

Description

technical field [0001] The invention relates to a chemical synthesis method, in particular to a preparation method of sorbitan oleate as a pharmaceutical auxiliary material. Background technique [0002] Sorbitan oleate (also known as sorbitan monooleate or Span 80) is an important nonionic surfactant, often used as a W / O emulsifier. Due to its excellent emulsifying, dispersing and wetting surface activities, non-toxic, non-irritating, low volatility, high critical micelle concentration and low micelle free energy, it is widely used in petroleum, food, cosmetics and pharmaceutical industries. Wide range of applications. [0003] In the preparation of sorbitan oleate, the traditional one-step base-catalyzed method is to simultaneously etherify and esterify sorbitol and oleic acid at 190°C-260°C in the presence of a basic catalyst. For example, the patent CN102260228A discloses a production process for synthesizing sorbitan oleate by one-step method, which involves etherific...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/20
Inventor 李娟胡平张阳洋
Owner HUBEI GEDIAN HUMANWELL PHARMA EXCIPENTS
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