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Method for preparing high-quality pentaerythritol oleate

A technology for pentaerythritol oleate and pentaerythritol, which is applied in the field of preparing high-quality pentaerythritol oleate, can solve the problems of shortening the service life of machinery, no method reported in literature, accelerated loss of mechanical lubrication system, etc., and achieves easy realization and simple and convenient operation. , the effect of high product quality

Inactive Publication Date: 2018-10-23
HUNAN INSTITUTE OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to corrosion of metals, the loss of the mechanical lubrication system is accelerated and the service life of the machine is shortened
[0008] The prior art shows that the synthesis and deacidification methods of pentaerythritol oleate have been reported in the literature, but the method for obtaining products with an acid value of less than 0.1mgKOH / g through reaction control has not been reported in the literature

Method used

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  • Method for preparing high-quality pentaerythritol oleate
  • Method for preparing high-quality pentaerythritol oleate
  • Method for preparing high-quality pentaerythritol oleate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 68.1g (0.5mol) of pentaerythritol, 557.9g (1.975mol) of oleic acid in the reactor successively, add p-toluenesulfonic acid accounting for 5‰ of the mass fraction of oleic acid as catalyst, and toluene as water-carrying agent, control oil bath heating Temperature 150-155°C, under the protection of nitrogen, stir and reflux, divide water for 1-1.5 hours, cool, add 4.5g acetic acid (0.075mol), pass nitrogen, heat the oil bath to 150-155°C, stir, continue to reflux and divide water 1 hour. After the reaction was complete, cool to room temperature, wash with water, and remove the toluene from the organic layer in a vacuum to obtain a light yellow oily transparent liquid with an acid value of 0.06 mgKOH / g and a yield of 98%.

Embodiment 2

[0028] In the reactor, add 68.1g (0.5mol) of pentaerythritol, 550.8g (1.95mol) of oleic acid, p-toluenesulfonic acid accounting for 5‰ of oleic acid mass fraction as a catalyst, and toluene as a water-carrying agent to control the heating temperature of the oil bath 150-155°C, under the protection of nitrogen, stir and reflux, divide water for 1-1.5 hours, cool, add 7.4g propionic acid (0.1mol), pass nitrogen, heat the oil bath to 150-155°C, stir, continue to reflux and divide water 1 hour. After the reaction was complete, cool to room temperature, wash with water, and remove the toluene from the organic layer in vacuum to obtain a light yellow oily transparent liquid with an acid value of 0.08 mgKOH / g and a yield of 98.5%.

Embodiment 3

[0030] In the reactor, add 68.1g (0.5mol) of pentaerythritol, 550.8g (1.95mol) of oleic acid, p-toluenesulfonic acid accounting for 5‰ of oleic acid mass fraction as a catalyst, and toluene as a water-carrying agent to control the heating temperature of the oil bath 150-155°C, under the protection of nitrogen, stir and reflux, divide water for 1-1.5 hours, cool, add 8.8g butyric acid (0.1mol), pass nitrogen, heat the oil bath to 150-155°C, stir, continue to reflux and divide water 1 hour. After the reaction is complete, cool to room temperature, wash with water, heat the organic layer to 60-80°C, add 20g of activated clay, stir for 0.5h, remove the toluene in vacuum after suction filtration, and obtain a light yellow oily transparent liquid with an acid value of 0.05mgKOH / g. The rate is 97%.

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Abstract

The invention discloses a method for preparing high-quality pentaerythritol oleate. The method is characterized by comprising the following steps of step 1, adding oleic acid and pentaerythritol according to a molar ratio of oleic acid to pentaerythritol being less than 4, adding a catalyst and a water carrying agent, and reacting; step 2, adding excessive micromolecular weight carboxylic acid, and enabling insufficiently reacted carboxylic acid to completely react, so as to obtain a micromolecular weight carboxylic ester mixture of pentaerythritol tetraoleate and pentaerythritol trioleate; step 3, after the action is completed, cooling to room temperature, washing by water, and removing the water carrying agent at an organic layer under the vacuum condition, so as to obtain the light yellow oily transparent liquid pentaerythritol oleate. Obtained pentaerythritol oleate has the advantages that the quality is high; only about 1.02% to 8.36% of pentaerythritol trioleate acetate is contained, the acid value is smaller than 0.1mgKOH / g, and the quality is better than the quality of the equivalent varieties on market; the price of the raw material is low, the raw material is easy to obtain, the operation is simple and convenient, and the industrialization is easy to realize.

Description

technical field [0001] The invention relates to the field of fine organic chemical industry, in particular to a method for preparing high-quality pentaerythritol oleate. Background technique [0002] Pentaerythritol tetraoleate has excellent lubricating properties, high viscosity index, good flame resistance, biodegradation rate greater than 90%, high-quality, low acid value can be used as an ideal base oil for synthetic ester type fire-resistant hydraulic oil, aviation Base oil for engine lubricating oils, environmentally friendly hydraulic oils, chainsaw oils and marine yacht engine oils. [0003] The production of pentaerythritol tetraoleate is obtained through esterification of pentaerythritol and oleic acid: [0004] [0005] In theory, 1 mol of pentaerythritol needs 4 mol of oleic acid. In order to ensure the complete reaction of pentaerythritol, an excess of oleic acid is generally used in actual production, that is to say, the molar ratio of oleic acid to pentaer...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/58C10M129/74C10N30/06C10N40/08C10N40/25
CPCC07C67/08C10M129/74C10M2207/283C10N2030/06C10N2040/08C10N2040/25C07C69/58
Inventor 廖德仲廖嘉树
Owner HUNAN INSTITUTE OF SCIENCE AND TECHNOLOGY
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