Method of producing trimethylolpropane oleate with single kettle

A technology of methylolpropane oleate and trimethylolpropane, which is applied in the field of synthesis of ester compounds, can solve the problems of complex separation of liquid catalyst products, poor product quality, and many side reactions, so as to reduce by-products and The content of residual acid, the effect of increasing the reaction esterification rate and reducing by-products

Inactive Publication Date: 2013-06-19
SHENYANG POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The invention uses a solid catalyst p-toluenesulfonic acid to catalyze the production of trimethylolpropane oleate, the catalyst is easily separated from the system, and solves the problems of complex separation of liquid catalyst products, poor product quality, deep color, many side reactions, and environmental pollution. question

Method used

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  • Method of producing trimethylolpropane oleate with single kettle

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The production of trimethylolpropane oleate in a single tank uses oleic acid, trimethylolpropane and p-toluenesulfonic acid as reactants.

[0020] Above-mentioned reactant reacts according to the following steps:

[0021] Add oleic acid and trimethylolpropane at a ratio of 3:1 to the reaction kettle, and add p-toluenesulfonic acid accounting for 0.2% of the total mass fraction of the reactants, heat to 160°C under stirring, and vacuum to 0.05MPa, after reacting for 4 hours, add activated carbon accounting for 0.5% of the total mass of the reactants for decolorization, continue to react for 9 hours, feed water vapor for stripping to remove residual acid, until the acid value drops below 0.05gKOH / g, Cool to below 50°C, filter activated carbon and solid catalyst to obtain trimethylolpropane oleate.

Embodiment 2

[0023] The production of trimethylolpropane oleate in a single tank uses oleic acid, trimethylolpropane and p-toluenesulfonic acid as reactants.

[0024] Above-mentioned reactant reacts according to the following steps:

[0025] Add oleic acid and trimethylolpropane with a substance amount of 3.5:1 into the reaction kettle, and add p-toluenesulfonic acid accounting for 0.6% of the total mass fraction of the reactants, heat to 200°C under stirring, and vacuum to 0.15MPa, after reacting for 4 hours, add activated carbon accounting for 1.5% of the total mass of the reactants for decolorization, continue to react for 7 hours, then pass in water vapor for stripping to remove residual acid, until the acid value drops below 0.05gKOH / g, Cool to below 50°C, filter activated carbon and solid catalyst to obtain trimethylolpropane oleate.

Embodiment 3

[0027] The production of trimethylolpropane oleate in a single tank uses oleic acid, trimethylolpropane and p-toluenesulfonic acid as reactants.

[0028] Above-mentioned reactant reacts according to the following steps:

[0029] Add oleic acid and trimethylolpropane with a substance quantity of 3.05:1 into the reaction kettle, and add p-toluenesulfonic acid accounting for 0.4% of the total mass fraction of the reactants, heat to 180°C under stirring, and evacuate to 0.09MPa, after reacting for 4 hours, add activated carbon accounting for 1% of the total mass of the reactants for decolorization, continue to react for 7 hours, then pass in water vapor for stripping to remove residual acid, until the acid value drops below 0.05gKOH / g, Cool to below 50°C, filter activated carbon and solid catalyst to obtain trimethylolpropane oleate.

[0030] According to the scheme carried out in the foregoing examples, the obtained trimethylolpropane oleate has an esterification rate of more th...

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Abstract

The invention provides a method of producing trimethylolpropane oleate with a single kettle. The method is characterized in that reactants are oleic acid and trimethylol propane, a catalyst is p-methylbenzene sulfonic acid; and the method comprises steps: adding the oleic acid and the trimethylol propane with a ratio of 3-4 : 1 in accordance with amount of substance into the reaction vessel, adding the p-methylbenzene sulfonic acid with an amount accounting for 0.2-0.6 % of a total mass fraction of the reactants, heating with stirring to 160-200 DEG C, vacuumizing to 0.05-0.15 MPa, reacting for 4 hours, adding active carbon with an amount accounting for 0.5-1.5 % of a total mass of the reactants for decoloration, continuously reacting for 7-9 hours, introducing water vapor, performing stream stripping to remove residual acids to reduce an acid value to be less than 0.05 g KOH/g, cooling to below 50 DEG C, and filtering the active carbon and the solid catalyst to obtain the trimethylolpropane oleate. The method solves problems that liquid catalysts are difficult to separate, poor in product quality and deep in color, have many side reactions, and pollute the environment.

Description

technical field [0001] The invention belongs to the technical field of synthesis of ester compounds in organic compounds. Background technique [0002] At present, in industrial production, sulfuric acid is generally used as a catalyst in the synthesis of trimethylolpropane oleate. Because it is easy to corrode equipment, the catalyst is difficult to separate from the system, and the yield is also low. Moreover, the kettle needs to be poured during post-processing, and oxygen will be introduced during the process, which will cause the color of the oil to become darker and reduce the quality of the product. Contents of the invention [0003] The invention uses a solid catalyst p-toluenesulfonic acid to catalyze the production of trimethylolpropane oleate, the catalyst is easily separated from the system, and solves the problems of complex separation of liquid catalyst products, poor product quality, deep color, many side reactions, and environmental pollution. question. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/58C07C67/08
Inventor 吴晓艺马川张宗成
Owner SHENYANG POLYTECHNIC UNIV
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