Preparation method of pentaerythritol unsaturated fatty acid ester

A technology of pentaerythritol and fatty acid ester, applied in the field of preparation of unsaturated fatty acid ester, can solve the problems of complex treatment process, serious equipment corrosion, a large number of azeotropic solvents, etc., and achieves high catalytic efficiency, improved efficiency and short reaction time. Effect

Inactive Publication Date: 2015-11-25
JIANGXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When preparing pentaerythritol unsaturated fatty acid ester with strong protonic acid such as concentrated sulfuric acid catalysis, although these catalysts are relatively cheap, and catalytic activity is better, but it belongs to homogeneous reaction, and equipment corrosion is serious, very easily produces a large amount of waste liquids, And the follow-up processing process is complex
However, when the solvent azeotropic dehydration process is used to prepare the pentaerythritol unsaturated fatty acid ester, a large amount of azeotropic solvent needs to be used, the reaction time is long, and the energy consumption is relatively large.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Add 1 mol of pentaerythritol, 5 mol of unsaturated fatty acid diesel antiwear agent and 0.03 mol of cerium oxide into the reactor with magnetic stirring and temperature control device; close the reactor and evacuate it to 200 Pa, then raise the temperature to 200°C , constant temperature reaction for 6h, when the acid value of the reaction system is no longer significantly reduced, the reaction is stopped, the reaction solution is filtered and separated while it is hot, and the cerium dioxide catalyst is recovered for reuse. Separation and purification of the esterification product, control the acid value of the product below 0.2mgKOH / g to obtain pentaerythritol unsaturated fatty acid ester, the yield is 96.8%.

Embodiment 2

[0015] Add 1 mol of pentaerythritol, 4 mol of unsaturated fatty acid diesel antiwear agent and 0.02 mol of cerium oxide into the reaction kettle with magnetic stirring and temperature control device; close the reaction kettle and evacuate the vacuum to 400Pa, then raise the temperature to 210°C , constant temperature reaction for 8 hours, when the acid value of the reaction system is no longer significantly reduced, the reaction is stopped, the reaction solution is filtered and separated while it is hot, and the ceria catalyst is recovered for reuse. Separation and purification of the esterified product, controlling the acid value of the product below 0.2 mgKOH / g to obtain pentaerythritol unsaturated fatty acid ester, the yield is 95.4%.

Embodiment 3

[0017] Add 1 mol of pentaerythritol, 6 mol of unsaturated fatty acid diesel antiwear agent and 0.05 mol of cerium oxide into the reactor with magnetic stirring and temperature control device; close the reactor and evacuate it to 100 Pa, then raise the temperature to 180°C , constant temperature reaction for 6h, when the acid value of the reaction system is no longer significantly reduced, the reaction is stopped, the reaction solution is filtered and separated while it is hot, and the cerium dioxide catalyst is recovered for reuse. Separation and purification of the esterification product, controlling the acid value of the product to be below 0.2 mgKOH / g to obtain pentaerythritol unsaturated fatty acid ester, the yield is 94.6%.

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Abstract

The invention discloses a preparation method of pentaerythritol unsaturated fatty acid ester. The preparation method includes: adding pentaerythritol, fatty acid type diesel anti-wear agent and cerium dioxide according to a molar ratio of 1:(4-6):(0.02-0.05) into a reaction kettle for mixing and stirring. Cerium dioxide which is reusable is adopted as a heterogeneous catalyst and is short in reaction time and high in catalyzing efficiency; in the process of preparing pentaerythritol unsaturated fatty acid ester, using of a lot of azeotropic solvent and removing of the catalyst are not needed, only simple filtering is needed, processes of neutralizing and washing are not needed, and no wastewater is discharged in subsequent treatment processes, so that preparation efficiency is improved greatly, and the preparation method is enabled to meet national requirements on environment protection.

Description

technical field [0001] The invention relates to a preparation method of unsaturated fatty acid ester, in particular to a preparation method of pentaerythritol unsaturated fatty acid ester. Background technique [0002] Pentaerythritol unsaturated fatty acid ester can not only be used as a plasticizer, but also a stabilizer, release agent, and dispersant in the processing of plastic materials, and it is also an important neopentyl polyol ester. Because of its good thermal oxidation stability, strong lubricating performance, low temperature performance and good viscosity-temperature performance, it is an ideal base oil for synthetic ester-type fire-resistant hydraulic oil, and it has been widely used as an oily agent in cold rolling of steel plates. fluid, steel pipe drawing oil and other metalworking fluids. At the same time, it is also an economical and effective improver for diesel lubricating performance. At present, there are many preparation methods for pentaerythritol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/003C07C67/08
CPCC07C67/08C07C69/003
Inventor 许招会廖维林林春花刘德勇
Owner JIANGXI NORMAL UNIV
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