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Preparation method of biobased pentaerythritol fatty acid ester

A technology for pentaerythritol and fatty acid ester, which is applied in the field of esterification synthesis in organic chemistry, can solve the problems of long reaction time, reduced catalyst usage, cumbersome process, etc., and achieves good biodegradation performance, short time consumption, separation and purification process simple effect

Inactive Publication Date: 2017-05-31
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN 102260571 B (CN 102260571 B a kind of aviation base oil Chinese People's Liberation Army Air Force Fuel Research Institute 2013) patent adopts multi-stage esterification reaction process, which greatly reduces the amount of catalyst used (less than 100ppm), or even completely cancels the use of catalyst, which can realize High conversion rate, low hydroxyl value esterification effect, but the process is too cumbersome and the reaction takes a long time

Method used

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  • Preparation method of biobased pentaerythritol fatty acid ester

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Experimental program
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Effect test

Embodiment 1

[0024] Embodiment 1: Prepare stearic acid and oleic acid with waste oil as raw material

[0025] Put the waste oil and water that have been treated by the waste oil treatment plant after removing impurities into the high-pressure reactor, close the reactor, adjust the stirring speed to mix the materials evenly, add water vapor to increase the pressure of the system to 3.5MPa, and heat up Heat at 220°C, heat-preserve and hydrolyze for 6 hours. After the reaction, the reaction solution is centrifuged to obtain the upper crude fatty acid phase and the lower glycerol aqueous phase. The obtained crude fatty acid is refined by molecular distillation, and different fractions are collected to obtain pure stearic acid and oil respectively. Sour pure.

Embodiment 2

[0026] Embodiment 2: take palm oil as raw material to prepare palmitic acid

[0027] Add palm oil and water into the autoclave, close the autoclave, adjust the stirring speed to mix the materials evenly, add water vapor to pressurize the system to raise the pressure to 4.5MPa, and heat up to 210°C, heat preservation and hydrolysis for 4 hours, and react after reaction The upper layer of crude fatty acid phase and the lower layer of glycerin aqueous phase were obtained by liquid centrifugal separation, and the obtained crude fatty acid was refined by molecular distillation to obtain pure palmitic acid.

Embodiment 3

[0028] Embodiment 3: the preparation of pentaerythritol stearate

[0029] 100 grams of stearic acid (C 18:0 ) and 8 grams of pentaerythritol were added to the reaction kettle, the reaction kettle was closed, the stirring speed was adjusted to mix the materials uniformly, the system pressure was maintained at 0.04MPa by vacuuming, and the temperature was raised to 230° C., and the flow degassing and heat preservation reaction was carried out for 4 hours. After the reaction, the temperature of the reaction solution is lowered to 80°C, and the unreacted pentaerythritol solid and liquid reaction products are separated by natural sedimentation or suction filtration, and the pentaerythritol can be reused after being separated and recovered. The liquid reaction product is separated and purified by molecular distillation, and the heavy component collected is the pentaerythritol stearate product. The product yield is 95.2%, the acid value is 1.9mgKOH / g, and the degree of esterification...

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Abstract

The invention discloses a preparation method of biobased pentaerythritol fatty acid ester, which belongs to the technical field of esterification and synthesis in organic chemistry. Specifically, pentaerythritol is mixed with biobased fatty acid, flowing degassing is performed under a negative pressure condition for an autocatalytic esterification reaction, and refined processes of separation dealcoholization, distillation deacidification and the like are performed, so as to obtain biobased pentaerythritol fatty acid ester. The preparation method has the advantages that a catalyst does not need to be added in the autocatalytic esterification reaction, thereby preventing a residual catalyst existing in a combined-state form in product molecules in a synthesis process of the traditional catalytic esterification technology commonly adopted at present from affecting the overall performance of a product; separation and purification processes are simple, and are controlled easily; the degree of esterification is high, side reaction is less, and the product purity is high; the high-temperature stability of the product is good.

Description

technical field [0001] The invention relates to the technical field of esterification synthesis in organic chemistry, in particular to a preparation method of bio-based pentaerythritol fatty acid ester. Background technique [0002] With the development of modern industry and the improvement of environmental protection requirements, people pay more and more attention to environmental issues. At present, more than 95% of lubricating oil comes from petroleum, and the biodegradability of petroleum-based lubricating oil is very poor; on the other hand, the global petroleum resources are increasingly scarce, resulting in a shortage of petroleum-based lubricating oil resources. Therefore, the synthesis of biodegradable lubricant base oils from renewable resources has attracted extensive attention. Bio-based ester base oils have been more and more widely used because of their unique high and low temperature properties, viscosity-temperature properties, lubricating properties, and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/33C07C67/54C07C69/58C07C69/003
CPCC07C67/08C07C67/54C07C69/33C07C69/58C07C69/003
Inventor 李学兵郭鹏林冠楠
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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