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Preparation method of pentaerythritol tristearate

A technology of pentaerythritol tristearate, which is applied in the field of chemical synthesis, can solve the problems of high reaction temperature and long reaction time, and achieve the effects of simple post-processing, saving production cost and energy consumption, and good product indicators

Inactive Publication Date: 2015-04-22
GUANGZHOU CARDLO BIOCHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method has high reaction temperature and long reaction time

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Embodiment 1, the preparation method of pentaerythritol tristearate of the present invention:

[0016] Put stearic acid and pentaerythritol into the reactor according to the material molar ratio of 1.0: 1, stir and mix evenly, then add 0.2% solid superacid SO of stearic acid quality 4 2- / ZrO 2 -SiO 2 , under 5 Pa vacuum, 150 ℃, the reaction time is 3h, and the crude product of pentaerythritol tristearate is obtained after the reaction is completed, and then the crude product of pentaerythritol tristearate is decolorized to obtain the finished product of pentaerythritol tristearate, and the reaction ester is determined The conversion rate was 88%.

[0017] Solid Superacid SO 4 2- / ZrO 2 -SiO 2 The specific steps of the preparation method are: take zirconium oxychloride (ZrOCl 2 ·8H 2 O) be prepared into a zirconium oxychloride solution, add diatomaceous earth, let it stand for about 20min to fully impregnate it, then add 26% concentrated ammonia water to adjus...

Embodiment 2

[0018] Embodiment 2, the preparation method of pentaerythritol tristearate of the present invention:

[0019] Put stearic acid and pentaerythritol into the reactor according to the material molar ratio of 1.2: 1, stir and mix evenly, then add 0.6% solid superacid SO of stearic acid quality 4 2- / ZrO 2 -SiO 2 , under 50Pa vacuum, 180 ℃, the reaction time is 2h, and the crude product of pentaerythritol tristearate is obtained after the reaction is completed, and then the crude product of pentaerythritol tristearate is decolorized to obtain the finished product of pentaerythritol tristearate, and the reaction ester is determined The conversion rate was 89%.

[0020] Solid Superacid SO 4 2- / ZrO 2 -SiO 2 The specific steps of the preparation method are: take zirconium oxychloride (ZrOCl 2 ·8H 2 O) be prepared into a zirconium oxychloride solution, add diatomaceous earth, let it stand for about 20min to fully impregnate it, then add 26% concentrated ammonia water to adju...

Embodiment 3

[0021] Embodiment 3, the preparation method of pentaerythritol tristearate of the present invention:

[0022] Put stearic acid and pentaerythritol into the reactor according to the material molar ratio of 1.1: 1, stir and mix evenly, then add 0.5% solid superacid SO of stearic acid quality 4 2- / ZrO 2 -SiO 2 , under 30Pa vacuum, 160 ℃, the reaction time is 2h, and the crude product of pentaerythritol tristearate is obtained after the reaction is completed, and then the crude product of pentaerythritol tristearate is decolorized to obtain the finished product of pentaerythritol tristearate, and the reaction ester is determined The conversion rate was 92%.

[0023] Solid Superacid SO 4 2- / ZrO 2 -SiO 2 The specific steps of the preparation method are: take zirconium oxychloride (ZrOCl 2 ·8H 2O) be prepared into a zirconium oxychloride solution, add diatomaceous earth, let it stand for about 20min to fully impregnate it, then add 26% concentrated ammonia water to adjus...

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Abstract

The invention belongs to the field of chemical synthesis and relates to a preparation method of pentaerythritol tristearate. The preparation method comprises the following steps of adding stearic acid and pentaerythritol into a reactor according to a mole ratio of 1.0-1.2: 1, carrying out stirring mixing to obtain a uniform mixture, adding solid super acid into the mixture to cause a reaction lasting for 2-3h under the conditions of a temperature of 150-180 DEG C and pressure of 5-50Pa so that a pentaerythritol tristearate crude product is obtained by the reaction, and carrying out decoloring treatment on the pentaerythritol tristearate crude product to obtain a pentaerythritol tristearate finished product. The preparation method utilizes solid super acid SO4<2-> / ZrO2-SiO2 as a pentaerythritol tristearate synthesis catalyst, reduces the existing reaction high-temperature from 200 DEG C to 150-180 DEG C, reduces reaction time by 1-2h and greatly saves a production cost and energy consumption. The preparation method of pentaerythritol tristearate has a high esterification rate of 92% and good product indexes.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a preparation method of pentaerythritol tristearate. Background technique [0002] Pentaerythritol stearate (Pentaerythritol stearate), referred to as PETS, is a white hard high-melting wax, soluble in ethanol, benzene and chloroform, and insoluble in water. It is mainly used as high-efficiency lubricant, PVC stabilizer, plasticizer, etc. Due to its environmental friendliness and reproducibility, polyol esters represented by pentaerythritol stearate have attracted more and more attention from researchers at home and abroad. Harsh conditions and other issues urgently need further technical improvement. Pentaerythritol tristearate is widely used as an auxiliary heat stabilizer, plasticizer, lubricating brightener and transparent agent in the plastic industry. The most prominent advantages are good compatibility with other additives, high temperature resistance, and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/33C07C67/08B01J27/053
CPCB01J27/053C07C67/08C07C69/33
Inventor 徐怀义马银官
Owner GUANGZHOU CARDLO BIOCHEM TECH
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