Preparation method of pentaerythritol tetraisostearate

A technology of isostearate and pentaerythritol tetra, applied in the field of preparation of pentaerythritol tetraisostearate, can solve the problems of high reaction temperature, dark color of reaction solution, difficult removal of acid, etc., and achieves reduction of reaction temperature and reaction conditions. Mild, short response time effect

Pending Publication Date: 2020-10-30
NANJING NUTRABUILDING BIO TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] 1. The reaction usually requires a higher reaction temperature (at least ≥140°C, most reports are 160-240°C) and a longer reaction time, which consumes a lot of energy and requires special equipment;
[0005] 2. When using an acidic catalyst, long-term high temperature will greatly shorten the life of the reactor;
[0006] 3. Esterification efficiency is of

Method used

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  • Preparation method of pentaerythritol tetraisostearate
  • Preparation method of pentaerythritol tetraisostearate

Examples

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Embodiment 1

[0025] The synthesis of embodiment 1 isostearyl chloride

[0026] To a solution of isostearic acid (100 g, 352 mmol) in dichloromethane (100 mL) was added dropwise thionyl chloride (46.1 g, 387 mmol) at 10-20°C under nitrogen atmosphere. After dropping, the temperature was raised to 35-45°C and stirred for 2 hours. TLC showed that the reaction was complete. After concentration, 107.6 g of light yellow liquid was obtained, which was set aside.

Embodiment 2

[0027] The synthesis of embodiment 2 isostearyl chloride

[0028] To a solution of isostearic acid (100 g, 352 mmol) in dichloromethane (100 mL) was added dropwise oxalyl chloride (46.9 g, 370 mmol) at 10-20 °C under nitrogen atmosphere. After dropping, the temperature was raised to 35-45°C and stirred for 2 hours. TLC showed that the reaction was complete. After concentration, 106.8 g of nearly colorless liquid was obtained, which was set aside.

Embodiment 3

[0029] The synthesis of embodiment 3 isostearyl chloride

[0030] To a solution of isostearic acid (100 g, 352 mmol) in dichloromethane / DMF (100 mL / 1 mL) was added triphosgene (41.8 g, 141 mmol) at 10-20 °C under nitrogen atmosphere. After the addition was complete, the temperature was raised to 35-45°C and stirred for 2 hours. TLC showed that the reaction was complete. After concentration, 108.2 g of nearly colorless liquid was obtained, which was set aside.

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Abstract

The invention provides a preparation method of pentaerythritol tetraisostearate. The preparation method specifically comprises the following steps: S1, taking pentaerythritol and isostearoyl chlorideaccording to a molar ratio of 1: (3.8-4.8), and putting the pentaerythritol and the isostearoyl chloride into a reaction kettle; and S2, carrying out a reaction for 0.5-12 h at a reaction temperatureof 80-150 DEG C under a vacuum pressure of-0.1 MPa to-0.05 MPa so as to obtain the pentaerythritol tetraisostearate product. The method does not need a catalyst; the reaction conditions are mild, thereaction temperature is greatly reduced, and a conventional enamel reaction kettle can be used; reaction time is short, and energy consumption is low; the product is light in color and high in quality; the method is simple in post-reaction treatment and suitable for industrialization.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method of pentaerythritol tetraisostearate. Background technique [0002] Pentaerythritol tetraisostearate is a colorless, odorless, transparent oil, which belongs to hindered ester. Pentaerythritol tetraisostearate has high thermal stability, and has functions such as film-forming, water-repellent, and emollient, and is a non-sticky moisturizer. At the same time, pentaerythritol tetraisostearate has good powder dispersibility and suspension, anti-sedimentation, and good skin-adherence. It is an excellent cosmetic additive and an excellent substitute for castor oil. [0003] The traditional preparation method is dehydration and esterification of pentaerythritol and isostearic acid at high temperature and normal pressure under the catalysis of protonic acid such as p-toluenesulfonic acid, etc. or Lewis acid such as ferric chloride. This metho...

Claims

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Application Information

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IPC IPC(8): C07C67/14C07C69/33
CPCC07C67/14C07C69/33
Inventor 张健廖琪林
Owner NANJING NUTRABUILDING BIO TECH CO LTD
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