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Production technology of pentaerythrityl tetrastearate

A technology for pentaerythritol and production technology, applied in the production technology field of pentaerythritol tetra-stearate, can solve problems such as high reaction temperature, difficult layered operation, polluted environment, etc., achieves lower reaction temperature, stable and reliable process, and lower production cost Effect

Active Publication Date: 2016-09-07
GUANGZHOU CARDLO BIOCHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its shortcoming is that after the reaction is completed, the catalyst and excess isostearic acid in the product must be removed by alkali washing or pickling. Since pentaerythritol isostearate is a high-viscosity ester derived from long-chain saturated fatty acids, it is It is very easy to emulsify during washing, and it is difficult to separate layers, so it is difficult to perform normal layering operations. Even if the layers are barely separated, the acid value will not decrease significantly, but the yield of the product will be significantly reduced, and a large amount of waste water will be generated at the same time, which will pollute the environment. , this production method no longer meets the requirements of today's environmental protection policies and green chemistry
Since pentaerythritol has four hydroxyl groups, the steric hindrance effect is large and the esterification is difficult, so the esterification reaction time between polyols and fatty acids is long and the reaction temperature is high (about 200°C).

Method used

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  • Production technology of pentaerythrityl tetrastearate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1, the production technique of pentaerythritol stearate tetraester of the present invention

[0020] S1, put in 1945.8kg of stearic acid, heat while stirring, until the stearic acid is completely melted and becomes a transparent liquid, continue to slowly put in 245.1kg of pentaerythritol and a catalyst with 0.2% weight of stearic acid, and then seal the feeding manhole well, and the reaction kettle Control to normal pressure, then slightly open N 2 , until there is a small amount of N at the exhaust port 2 foam overflow;

[0021] S2. Raise the temperature of the material to 115°C, keep it warm for 30 minutes, turn off N2, turn on the water ring vacuum pump, control the negative pressure at 0.03mpa, then raise the temperature of the material to 137°C, then increase the negative pressure to 0.06mpa, and react for 100 minutes;

[0022] S3. After the foam of the reactant completely disappears, increase the vacuum degree to 0.09mpa, and raise the temperature of...

Embodiment 2

[0025] Embodiment 2, the production technology of pentaerythritol stearate tetraester of the present invention

[0026] S1, put in 2048.3kg of stearic acid, heat while stirring, until the stearic acid is completely melted and becomes a transparent liquid, continue to slowly add 245.1kg of pentaerythritol and a catalyst of 1% by weight of stearic acid, and then seal the feeding manhole well, and the reaction kettle Control to normal pressure, then slightly open N 2 , until there is a small amount of N at the exhaust port 2 foam overflow;

[0027] S2. Raise the temperature of the material to 125°C, keep it warm for 30 minutes, turn off N2, turn on the water ring vacuum pump, control the negative pressure at 0.01mpa, then raise the temperature of the material to 143°C, then increase the negative pressure to 0.05mpa, and react for 80 minutes;

[0028] S3. After the foam of the reactant completely disappears, increase the vacuum degree to 0.07mpa, and raise the temperature of the...

Embodiment 3

[0031] Embodiment 3, the production technology of pentaerythritol stearate tetraester of the present invention

[0032] S1, put in 1997.0kg of stearic acid, heat while stirring, until the stearic acid is completely melted and becomes a transparent liquid, continue to slowly put in 245.1kg of pentaerythritol and a catalyst with 0.5% weight of stearic acid, and then seal the feeding manhole well, and the reaction kettle Control to normal pressure, then slightly open N 2 , until there is a small amount of N at the exhaust port2 foam overflow;

[0033] S2. Raise the temperature of the material to 120°C, keep it warm for 30 minutes, and turn off the N 2 , turn on the water ring vacuum pump, control the negative pressure at 0.02mpa, then raise the temperature of the material to 140°C, then increase the negative pressure to 0.05mpa, and react for 90 minutes;

[0034] S3. After the foam of the reactant completely disappears, increase the vacuum degree to 0.08mpa, and raise the tempe...

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Abstract

The invention discloses a production technology of pentaerythrityl tetrastearate. The technology comprises the following steps: 1, adding stearic acid, heating stearic acid, and adding pentaerythritol and a catalyst after the stearic acid is completely molten; 2, heating above materials to 115-125DEG C, controlling the negative pressure to be 0.01-0.03mpa, heating the materials to 137-143DEG C, increasing the negative pressure to 0.05-0.06mpa, and carrying out a reaction; 3, increasing the vacuum degree to 0.06-0.09mpa, heating the obtained reaction material to 155-165DEG C, and carrying out a reaction at a constant temperature under a constant pressure; 4, cooling the obtained reaction product after the esterification condensation reaction ends, adding diatomite or active carbon, stirring, carrying out negative pressure temperature control, cooling the above obtained material, adding the cooled material to a plate-and-frame filter press, removing the obtained filter cake, taking the obtained filtrate, spraying powder, spraying beads, slicing the obtained product, packaging the sliced product, and warehousing the packaged product. The technology has the advantages of high stability and reliability, high output, and realization of industrial production, and the prepared pentaerythrityl tetrastearate product has the advantages of good whiteness, low acid value and high purity.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a production process of pentaerythritol stearate tetraester. Background technique [0002] Pentaerythritol tetraester stearate (PETS 4 ) is a white hard high melting point wax, soluble in ethanol, benzene and chloroform, insoluble in water. PETS 4 It is widely used as an auxiliary heat stabilizer, plasticizer, lubricating brightener in the plastic industry, and can also be used as a transparent lubricant for calendered film and blown film. [0003] PETS 4 The traditional esterification method is formed by the esterification reaction of pentaerythritol and stearic acid at high temperature under the action of acidic or basic catalysts such as p-toluenesulfonic acid and sodium hydroxide. Its shortcoming is that after the reaction is completed, the catalyst and excess isostearic acid in the product must be removed by alkali washing or pickling. Since pentaerythritol iso...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/33B01J23/80
CPCB01J23/002B01J23/80C07C67/08C07C69/33
Inventor 徐怀义马银官陈昊民邵磊
Owner GUANGZHOU CARDLO BIOCHEM TECH
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