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Method for preparing pentaerythritol tetraisostearate

A technology of isostearate and pentaerythritol tetraisostearate, which is applied in the field of preparation of pentaerythritol tetraisostearate, can solve the problems of poor product quality and high reaction temperature, and achieve the effects of simple method, lower reaction temperature and shorter reaction time

Active Publication Date: 2016-07-27
GUANGZHOU CARDLO BIOCHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Metal oxides such as zinc oxide, aluminum oxide, stannous oxide, etc. can catalyze some esterification reactions, such as Chinese patent application CN101293828A using zinc oxide or ferric chloride to catalyze the synthesis of pentaerythritol isostearate, but it still has a reaction temperature High, the problem of poor product quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1, the preparation method of pentaerythritol tetraisostearate of the present invention

[0020] S1, put 27.2kg of pentaerythritol and 227.6kg of isostearic acid into the reactor, and start stirring;

[0021] S2. Add the composite metal oxide of 0.2% by weight of isostearic acid, and react at 140° C. for 5 hours under the protection of nitrogen. ℃ decompression to negative 0.1Mpa, distill off the organic solvent and water, and obtain the pentaerythritol tetraisostearate product after filtration, the yield is 97.4%, the product color (Gardner method) ≤ 1, and the acid value is 0.20.

[0022] The preparation method of described composite metal oxide is as follows: Weigh ZnCl 2 2H 2 O and FeCl 2 4H 2 O is made into a mixed salt solution, and another NaOH and NaOH are weighed 2 CO 3 Prepare a mixed alkali aqueous solution; the two solutions are simultaneously added to a rotating liquid film reactor according to a volume ratio of 1:1 to rapidly nucleate, and...

Embodiment 2

[0024] Embodiment 2, the preparation method of pentaerythritol tetraisostearate of the present invention

[0025] S1, put 27.2kg of pentaerythritol and 239.0kg of isostearic acid into the reactor, start stirring;

[0026] S2, add the composite metal oxide of 1% by weight of isostearic acid, under the protection of nitrogen, react at 150 DEG C for 4h, after the reaction is completed, separate the composite metal oxide to obtain the crude product of pentaerythritol tetraisostearate, which is obtained at 130 ℃ depressurized to negative 0.05Mpa, distilled off the organic solvent and water, and filtered to obtain the pentaerythritol tetraisostearate product with a yield of 98.0%, product color (Gardner method) ≤ 1, and acid value 0.18.

[0027] The preparation method of described composite metal oxide is as follows: Weigh ZnCl 2 2H 2 O and FeCl 2 4H 2 O is made into a mixed salt solution, and another NaOH and NaOH are weighed 2 CO 3 Prepare a mixed alkaline aqueous solution;...

Embodiment 3

[0029] Embodiment 3, the preparation method of pentaerythritol tetraisostearate of the present invention

[0030]S1, put 27.2kg of pentaerythritol and 233.3kg of isostearic acid into the reactor, start stirring;

[0031] S2, add the composite metal oxide of 0.6% by weight of isostearic acid, under the protection of nitrogen, react at 140 ℃ for 4.5h, after the reaction is finished, separate the composite metal oxide to obtain the crude product of pentaerythritol tetraisostearate, the crude product is in Reduce the pressure at 120°C to negative 0.05Mpa, distill off the organic solvent and water, and obtain the product of pentaerythritol tetraisostearate after filtration, the yield is 99.2%, the product color (Gardner method) ≤ 1, acid value is 0.10.

[0032] The preparation method of described composite metal oxide is as follows: Weigh ZnCl 2 2H 2 O and FeCl 2 4H 2 O is made into a mixed salt solution, and another NaOH and NaOH are weighed 2 CO 3 Prepare a mixed alkali aq...

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Abstract

The invention belongs to technical field of chemical synthesis, in particular to a method for preparing pentaerythritol tetraisostearate. The method comprises the following steps: S1. taking pentaerythritol and isostearic acid according to a mole ratio of 1:4.0-4.2 and putting into a reaction kettle, and starting to stirring; S2. adding a composite metal oxide, reacting at a temperature of 140 to 150 DEG C for 4 to 5 h, finishing the reaction, separating the composite metal oxide to obtain a crude pentaerythritol tetraisostearate product, reducing pressure to minus 0.05 to 0.1 Mpa at a temperature of 100 to 130 DEG C, removing an organic solvent and water by distilling, and obtaining the pentaerythritol tetraisostearate product after filtering. The method has the advantages of low reaction temperature and short reaction time, and the pentaerythritol tetraisostearate has high yield and purity.

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 kind of liquid oil with relatively large relative molecular weight, basically odorless, with the combination of 4 ester bonds to form a three-dimensional structure, which belongs to hindered ester; it has high thermal stability and has Film, water resistance, emollient function, is an emollient with excellent performance. Pentaerythritol tetraisostearate is mainly used in skin cream, sunscreen products, make-up, shampoo and conditioner and other products. [0003] The traditional esterification method of pentaerythritol tetraisostearate is formed by the esterification reaction of pentaerythritol and isostearic acid at high temperature under the action of an acidic catalyst such as p-toluenesulfonic acid. Its shortcoming is that aft...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/33B01J23/80
CPCB01J23/80C07C67/08C07C69/33
Inventor 徐怀义马银官
Owner GUANGZHOU CARDLO BIOCHEM TECH
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