Technology for synthesizing trimethylolpropane trioleate

A technology of trimethylolpropane oleate and methylolpropane oleate, which is applied in the field of synthesis technology of trimethylolpropane oleate, can solve the problem of slow esterification rate, difficulty in product separation, corrosion of equipment, etc. The problem is to improve the reaction esterification rate, the process equipment is simple, and the reaction speed is improved.

Pending Publication Date: 2018-04-20
浙江工业大学上虞研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] As a polybasic hindered alcohol, the steric hindrance effect in the esterification process is serious. In addition, the activity of the carbonyl group in the carboxylic acid is very low, and the esterification rate is very slow. Conventional catalysts su

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Catalyst preparation:

[0026] I. Weigh a certain amount of carbon nanotubes with an outer diameter of 3nm, and add 30% HNO 3 Solution and 30ml of H with a mass fraction of 15% 2 O 2 The solution was heated to reflux at 120°C for 3 hours, taken out and cooled to room temperature, washed, filtered, and dried by conventional methods to obtain surface-modified carbon nanotubes;

[0027] II. Dissolve zirconium nitrate, lanthanum nitrate and cetyltrimethylammonium bromide in 30ml of deionized water, mix and stir for 1.5h, then add H with a concentration of 0.95mol / L 2 SO 4 And 2.05mol / L HCl mixed solution, and finally add 100mg of the surface-modified carbon nanotubes obtained by the above I, stir evenly at 35~40℃, and heat at 115℃ for 3~5h, cool to room temperature and pass After washing, filtering, drying and roasting by conventional methods, SO with high specific surface area is obtained 4 2- / La 2 O 3 -ZrO 2 @CNTS super acid.

Embodiment 2

[0029] Catalyst preparation:

[0030] I. Weigh a certain amount of carbon nanotubes with an outer diameter of 5nm, and add 30% HNO 3 Solution and 30ml of H with a mass fraction of 15% 2 O 2 The solution was heated to reflux at 110°C for 3 hours, taken out and cooled to room temperature, washed, filtered, and dried by conventional methods to obtain surface-modified carbon nanotubes;

[0031] II. Dissolve zirconium nitrate, lanthanum nitrate and cetyltrimethylammonium bromide in 20ml of deionized water, mix and stir for 0.5h, and then add H with a concentration of 1.0mol / L 2 SO 4 And 2.0mol / L HCl mixed solution, finally add 70mg of the surface-modified carbon nanotubes obtained by the above I, stir evenly at 35~40℃, and heat at 110℃ for 3~5h, cool to room temperature and pass After washing, filtering, drying and roasting by conventional methods, SO with high specific surface area is obtained 4 2- / La 2 O 3 -ZrO 2 @CNTS super acid.

Embodiment 3

[0033] (1) Put industrial oleic acid into the reactor, add 10wt% elemental iodine and 35wt% methyl acrylate, heat to 180°C, keep the temperature for 3h, cool to room temperature, and distill under reduced pressure to obtain high-purity oleic acid;

[0034] (2) Put the above-mentioned high-purity oleic acid and trimethylolpropane in a molar ratio of 3:1 into the reaction kettle, heat it to 82°C, wait until the trimethylolpropane is completely dissolved, add 0.3wt% of the prepared in Example 1 A solid super acid with a high specific surface area is used as an esterification catalyst. Keep the vacuum in the kettle at 85kPa, react for 3 hours, add 1.5% of the total mass of the reactants, stir and decolorize at 25°C for 4 hours, and pass water vapor for stripping removal Residual acid, when the acid value drops below 0.05gKOH / g, cool to below 50°C, filter activated carbon and solid catalyst to obtain trimethylolpropane oleate. After testing, the esterification rate reached 99.3%, and ...

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PUM

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Abstract

The invention relates to a technology for synthesizing trimethylolpropane trioleate. The trimethylolpropane trioleate is prepared through a direct esterification method of highly pure oleic acid and trimethylol propane, a SO<4><2->/La2O3-ZrO2@CNTS super strong acid having a high specific surface area is used as an esterification catalyst in the esterification reaction, and the catalyst has a goodcatalytic activity and an excellent reuse performance in the esterification reaction of the trihydroxymethane and the oleic acid at a lower temperature.

Description

Technical field [0001] The invention relates to the field of organic chemical synthesis, in particular to a synthesis process of trimethylolpropane oleate. Background technique [0002] With the rapid development of society, people pay more and more attention to the environment and resources. Especially after entering the 21st century, lubricants have been widely used in aviation, automobiles, machinery and other industrial fields. They have the ability to lubricate, seal and prevent equipment. Many excellent properties such as rust, heat dissipation and cooling. At present, there are many varieties of lubricants, including animal and vegetable oils, mineral oils, synthetic oils and water-based liquids. Traditional lubricating oils are mostly mineral oil-based lubricating oils, which play an important role in the lubrication of equipment, prevent equipment corrosion, and extend the service life of machinery. However, in some special cases, equipment is used and transported in th...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/58C07C51/50C07C51/44C07C57/12B01J27/053
CPCB01J27/053C07C51/44C07C51/50C07C67/08C07C69/58C07C57/12
Inventor 贾建洪
Owner 浙江工业大学上虞研究院有限公司
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