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.
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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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