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Preparation and purification method for trimethylolpropane fatty acid triester

A technology of trimethylolpropane fatty acid and methylolpropane fatty acid is applied in the field of degradable biological lubricating oil to achieve the effect of improving the utilization rate of raw materials

Active Publication Date: 2012-07-04
JINAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There is no report about the preparation of trimethylolpropane fatty acid triesters in the existing literature

Method used

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  • Preparation and purification method for trimethylolpropane fatty acid triester
  • Preparation and purification method for trimethylolpropane fatty acid triester
  • Preparation and purification method for trimethylolpropane fatty acid triester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Synthesis of trimethylolpropane fatty acid triesters: in a 500ml three-neck round bottom flask, add 6.7g (0.05M) TMP, then add 59.0g palm oil fatty acid methyl ester (4 times the molar weight of TMP) and 0.69g of potassium carbonate (0.10 times the molar weight of TMP), connect condensed water, water temperature 30 ℃; carry out transesterification reaction 60min under the condition of temperature 128 ℃ and pressure 300Pa, control the cooling water temperature in the reflux condenser, make ester The methanol generated by the exchange is vacuumed away, and the trimethylolpropane is condensed and refluxed to obtain a transesterification reaction mixture;

[0025] (2) Neutralization and washing of the reaction solution: the transesterification reaction mixture obtained in step (1) is added to a phosphoric acid solution of 10% by weight of the transesterification reaction mixture, and the phosphoric acid solution contains phosphoric acid that neutralizes 90% of the theore...

Embodiment 2

[0030] (1) Synthesis of trimethylolpropane fatty acid triesters: in a 500ml three-necked round-bottomed flask, add 6.7g (0.05M) TMP, then add 63.4g palm oil fatty acid methyl ester (4.3 times the molar weight of TMP) And 0.20g sodium hydroxide (0.10 times the molar weight of TMP), connect condensed water, water temperature 40 ℃; Carry out transesterification reaction 300min under the condition of temperature 110 ℃ and pressure 100Pa, control the cooling water temperature in the reflux condenser, make The methanol generated by the transesterification is vacuumed away, and the trimethylolpropane is condensed and refluxed to obtain a transesterification reaction mixture;

[0031] (2) Neutralization and washing of reaction solution: with step (1) gained transesterification reaction mixture, add the phosphoric acid solution of transesterification reaction mixture weight 20%, contain the phosphoric acid of neutralizing sodium hydroxide theoretical molar weight 100% in the phosphoric ac...

Embodiment 3

[0034] (1) Synthesis of trimethylolpropane fatty acid triesters: in a 500ml three-neck round bottom flask, add 6.7g (0.05M) TMP, then add rapeseed oil fatty acid methyl ester (5.5 times the molar weight of TMP) and Potassium hydroxide (0.15 times the molar weight of TMP), connected to condensed water, water temperature 80 ° C; under the conditions of temperature 110 ° C and pressure 5000 Pa, carry out transesterification reaction for 30 minutes, control the cooling water temperature in the reflux condenser, so that the transesterification produces The methanol is vacuumed away, and the trimethylolpropane is condensed and refluxed to obtain a transesterification reaction mixture;

[0035] (2) Neutralization and washing of the reaction solution: with step (1) gained transesterification reaction mixture, add the phosphoric acid solution of transesterification reaction mixture weight 30%, contain the phosphoric acid of neutralizing potassium hydroxide theoretical molar weight 120% ...

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Abstract

The invention discloses a preparation and purification method for trimethylolpropane fatty acid triester, which comprises the following steps: taking fatty acid methyl ester and trimethylolpropane as raw materials; adding base catalyst; carrying out ester exchange reaction under the vacuum condition to obtain an ester exchange reaction mixture; adding phosphoric acid solution, and carrying out neutralization reaction to remove the base catalyst; after the reaction is finished, standing for layering or carrying out centrifugal layering; washing an upper oil layer by hot water; standing for layering or carrying out centrifugal layering to obtain an oil layer and a water layer; and dewatering and drying the oil layer in vacuum, wherein the obtained heavy phase is a purified trimethylolpropane fatty acid triester product with a knifing type molecular distillation method, and the obtained light phase is the recovered fatty acid methyl ester. According to the preparation and purification method for the trimethylolpropane fatty acid triester, the trimethylolpropane fatty acid triester has high content which occupies more than 95%. The trimethylolpropane fatty acid triester is purified by molecular distillation, the excessive fatty acid methyl ester is recovered, so that the use ratio of raw materials can be improved, and the product can be purified at lower temperature.

Description

technical field [0001] The invention belongs to the field of biodegradable lubricating oils, and in particular relates to a method for preparing trimethylolpropane fatty acid triesters from fatty acid methyl esters derived from various animal and vegetable oils. Background technique [0002] Traditional lubricants are derived from petroleum and, like plastic, do not biodegrade after use and disposal. Waste lubricating oil has become the world's largest source of liquid pollution. my country's waste lubricating oil (engine oil) reaches more than 6 million tons every year, which directly affects the protection of the environment and the sustainable development of the economy. Without lubricants, there would be no modern industry. Any place with transmission and friction needs lubricating oil to reduce wear and improve machine life. Biolubricant is a new substitute for petroleum lubricating oil that has been studied in Europe and the United States in recent years and gradual...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/003C07C67/03C07C67/48C07C67/54
Inventor 汪勇王尔佩唐书泽
Owner JINAN UNIVERSITY
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