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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

Inactive Publication Date: 2019-05-24
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 such as sulfuric acid have exposed many shortcomings, and it is difficult to separate from the product. and poor thermal stability, corrosion equipment, environmental pollution and difficult regeneration, so people pay more attention to solid superacid catalysts

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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PUM

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Abstract

The invention relates to a technology for preparing trihydroxymethylpropyl trioleate through an ester exchange method. By the adoption of the methyl oleate and trimethylolpropane ester exchange method, in ester exchange, SO42- / ZrO2@CNTS superacid with a high specific surface area is adopted as an ester exchange catalyst, and shows good catalytic activity and excellent performance of repeated usagein an ester exchange reaction of methyl oleate and trimethylolpropane at low temperature.

Description

technical field [0001] The invention relates to the field of organic chemical synthesis, in particular to a process for preparing trihydroxypropane oleate by transesterification. 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, lubricating oil has been widely used in aviation, automobile, machinery and other industrial fields. Rust, heat dissipation and cooling, and many other excellent properties. At present, there are many kinds of lubricating oils, including animal and vegetable oils, mineral oils, synthetic oils and water-based fluids. Traditional lubricating oils are mostly mineral oil-based lubricating oils, which play an important role in lubricating equipment, preventing equipment from rusting, and prolonging the service life of machinery. , Lubricating oil discharged through different forms is always inevitable. At the same time, bec...

Claims

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Application Information

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IPC IPC(8): C07C69/58C07C67/03C07C67/08B01J27/053
Inventor 贾建洪
Owner 浙江工业大学上虞研究院有限公司