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Preparation of pentaerythritol tetraoctyl stearate

A technology of isostearate and pentaerythritol tetra, which is applied in the technical field of polyol esterification, can solve the problems of inability to apply cosmetics, severe skin irritation, and low purity, and achieve high yield, light color, and high purity.

Active Publication Date: 2008-11-05
广州星业科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After the reaction of this method is not carried out after treatment, the acidic catalyst remains in the product, which is more irritating to the skin, and the color is too dark and the purity is not high, so it cannot be applied in cosmetics

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 40.8g of pentaerythritol, 357.8g of isostearic acid, and 1.8g of p-toluenesulfonic acid into the flask successively, under nitrogen protection, distill and react under normal pressure at 220°C for 12 hours, stop the reaction, lower the temperature to 70°C, and add n-hexane 200g, 150g of isopropanol, neutralized with 120g of 5% NaOH aqueous alkali washing, then washed the organic phase with water to make the pH value tend to be neutral 7, then decompressed to negative 0.1Mpa, distilled off the organic solvent and water, Filtration yielded 351.2 g of product. The yield of this example is 97.4%, the product color (Gardner) is less than 1, and the acid value is 0.23.

Embodiment 2

[0021] Add 40.8g of pentaerythritol, 340.8g of isostearic acid, and 1.2g of p-toluenesulfonic acid into the flask, under the protection of nitrogen, carry out atmospheric distillation at 240°C for 12 hours, stop the reaction, lower the temperature to 70°C, add 200g of n-hexane, iso Propanol 150g is neutralized with 60g of 10% NaOH aqueous alkali washing, and then the organic phase is washed to neutrality with clear water, then decompressed to -0.1MPa to distill off the organic solvent and water, and filter to obtain 345.3g product, yield 95.8%, The product color (Gardner) is less than 1, and the acid value is 0.16.

Embodiment 3

[0023] Add 40.8g of pentaerythritol, 357.8g of isostearic acid, and 1.2g of sulfamic acid into the flask, under nitrogen protection, and carry out atmospheric distillation reaction at 180°C for 20 hours, stop the reaction, cool down to 90°C, add 150g of cyclohexane, 150g of tert-butanol, washed and neutralized with 60g of 10% NaOH aqueous solution, then washed the organic phase with water to neutrality, then decompressed to -0.1MPa, distilled off the organic solvent and water, filtered to obtain 348.3g of product, yield 96.6 %, the product color (Gardner) is less than 1, and the acid value is 0.32.

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PUM

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Abstract

The invention relates to a preparation method of tetraisostearate: the mol ratio of pentaerythritol to isostearic acid is 1: 4.0 to 4.4; the temperature is raised to the range of 160 to 240 DEG C under normal pressure and reacted for 10 to 24 hours by distillation, wherein, the adding amount of a catalyst is 0.1 to 1 percent of the weight of the isostearic acid; after esterification is finished, the temperature is decreased to 50 to 90 DEG C; a nonpolar solvent and a polar solvent are added; the adding amounts of the nonpolar solvent and the polar solvent are respectively 5 to 80 percent and 5 to 80 percent of the weight of the isostearic acid; aqueous slkali is added for alkali washing neutralization; the adding amount is 0.5 to 3 percent of the weight of the isostearic acid; the concentration of the aqueous slkali is 5 to 30 percent; an organic phase is washed to neutral by water; the solvents and water are removed by reduced pressure distillation; then the product is obtained after filtration; each step is carried out under the protection of nitrogen; the preparation method of the invention has high yield; the obtained product has the advantages of light color, low acid value, high purity and being ideally applied to the cosmetic industry.

Description

technical field [0001] The invention relates to a preparation method of pentaerythritol tetraisostearate, which belongs to a polyol esterification process in organic chemistry. Background technique [0002] At present, pentaerythritol tetraisostearate is mainly used in the cosmetic industry. It is an excellent emollient that will not clog pores. It can give the skin a very soft feeling when rubbed on the skin. It also has low spreadability and high viscosity. Due to its consistency, it can be used in skin creams, sunscreen products, make-up and bath oils, and is an excellent substitute for castor oil. Since pentaerythritol has four hydroxyl groups, the steric hindrance effect is large and the esterification is difficult, so the esterification reaction time between polyol and fatty acid is long and the reaction temperature is high. After the reaction is completed, it is generally necessary to use alkali washing to remove the catalyst and excess isostearic acid in the product...

Claims

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Application Information

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IPC IPC(8): C07C69/33C07C67/08
Inventor 叶建忠孟巨光
Owner 广州星业科技股份有限公司
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