Technology for preparing trihydroxymethylpropyl trioleate through ester exchange method
A technology of trihydroxypropane oleate and trimethylolpropane, which is applied in the field of preparing trihydroxypropane oleate by transesterification method, can solve the problems of serious steric hindrance effect, difficult product separation, slow esterification rate, etc. Improve the reaction speed and transesterification conversion rate, simple process equipment, and improve the effect of product color
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Embodiment 1
[0023] Catalyst preparation:
[0024] 1. Take a certain amount of carbon nanotubes with an outer diameter of 3nm, and add HNO with a mass fraction of 30% 3 solution and 30ml mass fraction of 15% H 2 o 2 The solution was heated to reflux at 120°C for 3 hours, taken out, cooled to room temperature, washed by conventional methods, suction filtered, and dried to obtain surface-modified carbon nanotubes;
[0025] II. Dissolve zirconium nitrate and cetyltrimethylammonium bromide in deionized water of 30ml respectively, mix and stir for 1.5h, then add concentration of 0.95mol / L H 2 SO 4 Mix the solution with 2.05mol / L HCl, finally add 100mg of the surface-modified carbon nanotubes obtained by the above I, stir evenly at 35-40°C, heat at 115°C for 3-5h, cool to room temperature and pass After conventional methods of washing, suction filtration, drying, and roasting, SO with a high specific surface area is obtained. 4 2- / ZrO 2 @CNTS super acid.
Embodiment 2
[0027] Catalyst preparation:
[0028] 1. Take a certain amount of carbon nanotubes with an outer diameter of 5nm, and add a mass fraction of 30% HNO 3 solution and 30ml mass fraction of 15% H 2 o 2 The solution was heated to reflux at 110°C for 3 hours, taken out, cooled to room temperature, washed by conventional methods, suction filtered, and dried to obtain surface-modified carbon nanotubes;
[0029] II. Dissolve zirconium nitrate and cetyltrimethylammonium bromide in deionized water of 20ml respectively, mix and stir for 0.5h, then add H2O with a concentration of 1.0mol / L 2 SO 4 Mix the solution with 2.0mol / L HCl, finally add 70mg of the surface-modified carbon nanotubes obtained by the above I, stir evenly at 35-40°C, heat at 110°C for 3-5h, cool to room temperature and pass After conventional methods of washing, suction filtration, drying, and roasting, SO with a high specific surface area is obtained. 4 2- / ZrO 2 @CNTS super acid.
Embodiment 3
[0031](1) Add industrial oleic acid to the reaction kettle, add a certain amount of methanol and concentrated sulfuric acid, heat to 100 ° C, react for 3 hours, cool to room temperature, and distill under reduced pressure to obtain high-purity methyl oleate;
[0032] (2) Add the above-mentioned methyl oleate and trimethylolpropane in a molar ratio of 2.5:1 into the reaction kettle, heat to 70°C, and wait until the trimethylolpropane is completely dissolved, add 0.4wt% of the high-alcohol prepared in Example 1 specific surface area of SO 4 2- / ZrO 2 @CNTS solid super acid is used as a transesterification catalyst, keep the vacuum in the kettle at 80kPa, react for 3 hours, add activated carbon accounting for 1.5% of the total mass of the reactants to decolorize, filter the activated carbon and solid catalyst, and distill under reduced pressure to obtain trimethylolpropane Oleate. After testing, the transesterification rate reaches 100%, and the yield reaches 96.4%.
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