A kind of method utilizing hydrogenated oil to prepare pentaerythritol stearate

A technology of pentaerythritol stearate and pentaerythritol, applied in chemical instruments and methods, preparation of organic compounds, carboxylate preparation, etc., can solve the problems of long saponification time, incomplete saponification, and difficult saponification of saponification reaction, and achieve shortening The effect of high reaction time, saponification rate and short time

Active Publication Date: 2017-12-19
GUANGZHOU CARDLO BIOCHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] PETS 4 The preparation raw material stearic acid is usually made by palm oil through hydrogenation, saponification, acidolysis, the saponification reaction of hydrogenated palm oil, because hydrogenated palm oil and alkali solution are incompatible with each other, so saponification reaction exists saponification time is too long, saponification is not enough Complete or even difficult to saponify, etc. Under normal conditions, it generally requires a reaction temperature of 90-100°C and a reaction time of 3-4 hours to completely saponify

Method used

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  • A kind of method utilizing hydrogenated oil to prepare pentaerythritol stearate
  • A kind of method utilizing hydrogenated oil to prepare pentaerythritol stearate

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Embodiment 1

[0024] Embodiment 1, the present invention utilizes hydrogenated oil to prepare the method for pentaerythritol stearate

[0025] S1. Add 60 kg of 40% sodium hydroxide aqueous solution and 12 kg of polyethylene glycol-600 to 200 kg of hydrogenated palm oil, control the microwave power to 600w, and the reaction temperature to 65° C., and react for 2 hours under stirring to obtain a saponified product;

[0026] S2, adding a volume concentration of 20% sulfuric acid solution to the saponified product under stirring until the pH of the material is 2, stop the acidification, move the material into a distillation tower, and distill at a temperature of 240 °C and a pressure of 0.070 MPa. Obtain stearic acid;

[0027] S3, drop into described stearic acid 1945.8kg in reactor, heat while stirring, until stearic acid is fully melted and is transparent liquid state, continue to slowly drop into the catalyst of 245.1kg pentaerythritol and stearic acid weight 0.2%, open nitrogen protection a...

Embodiment 2

[0031] Embodiment 2, the present invention utilizes hydrogenated oil to prepare the method for pentaerythritol stearate

[0032] S1. Add 80 kg of 45% sodium hydroxide aqueous solution and 16 kg of polyethylene glycol-600 to 200 kg of hydrogenated palm oil, control the microwave power to 700w, and the reaction temperature to 75° C., and react for 3 hours under stirring to obtain a saponified product;

[0033] S2, adding a volume concentration of 25% sulfuric acid solution to the saponified product under stirring until the pH of the material is 1, stop the acidification, move the material into a distillation tower, and distill at a temperature of 250° C. and a pressure of 0.080 MPa. Obtain stearic acid;

[0034] S3, drop into described stearic acid 2048.3kg in reactor, heat while stirring, until stearic acid is fully melted and is transparent liquid state, continue to slowly drop into the catalyst of 245.1kg pentaerythritol and stearic acid weight 1%, open nitrogen protection an...

Embodiment 3

[0038] Embodiment 3, the present invention utilizes hydrogenated oil to prepare the method for pentaerythritol stearate

[0039] S1. Add 70 kg of 45% sodium hydroxide aqueous solution and 14 kg of polyethylene glycol-600 to 200 kg of hydrogenated palm oil, control the microwave power to 700w, and the reaction temperature to 65° C., and react for 2 hours under stirring to obtain a saponified product;

[0040] S2, under stirring, adding a volume concentration of 20% sulfuric acid solution to the saponified product until the pH of the material is 2, stop the acidification, move the material into a distillation tower, and distill at a temperature of 240 °C and a pressure of 0.080 MPa. Obtain stearic acid;

[0041] S3, drop into described stearic acid 1997.0kg in reactor, heat while stirring, until stearic acid is fully melted and is transparent liquid state, continue to slowly drop into the catalyst of pentaerythritol 245.1kg and stearic acid weight 0.6%, open nitrogen protection ...

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Abstract

The invention discloses a method for preparing pentaerythritol stearate from hydrogenated oil.The method includes the following steps that S1, a sodium hydroxide solution is added to hydrogenated palm oil, microwave processing is conducted, a reaction is conducted under stirring, and saponified matter is obtained; S2, a sulfuric acid solution is added to the saponified matter till the pH value is 1 to 2, the material is transferred into a distillation tower, and stearic acid is obtained after distillation is completed; S3, stearic acid, pentaerythritol and a catalyst are put, the material is heated, negative pressure is controlled, and a reaction is conducted; S4, then the vacuum degree is increased to 0.07-0.09 mpa, the material is heated to 155-165 DEG C, and a reaction is conducted for 130-150 min under heat preservation at constant pressure; S5, cooling is conducted after an esterification condensation reaction is completed, kieselguhr is added for decoloration and deordorization, the material enters a plate-and-frame filter press, filter cakes are removed, filtrate is taken and subjected to powder spraying, bead spraying and slicing, and packaging and storage are conducted.The method is stable, reliable, high in yield and capable of achieving industrial production, and the prepared pentaerythrityl tetrastearate product is good in whiteness, low in acid value and high in purity.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a method for preparing pentaerythritol stearate from hydrogenated oil. 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 pentaeryt...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/33C07C67/08B01J23/06
CPCB01J23/06C07C51/02C07C67/08C07C69/33C07C53/126
Inventor 徐怀义马银官
Owner GUANGZHOU CARDLO BIOCHEM TECH
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