Synthetic method of trimethylolpropane tricaprylate

Abstract

The invention relates to a synthetic method of trimethylolpropane tricaprylate, which belongs to the technical field of esters compound synthesizing in organic chemistry. Taking trimethylolpropane and isocaprylic acid as material, an esterification reaction is preformed in nitrogen gas under the action of metallic oxide catalyst, the trimethylolpropane tricaprylate is obtained after depickle and filtration; the mass ratio of the trimethylolpropane and the isocaprylic acid is 1:3.15-3.95; the metallic oxide catalyst is stannous oxide or ferric oxide or magnesia, and the like, and the adding amount of the catalyst accounts for 0.03 to 0.10 percent by weight of the total weight of the trimethylolpropane and the isocaprylic acid. The invention reasonably selects metal oxide as the catalyst, and the metal oxide does not erode equipment, can be removed by filtration after the reaction is finished and can be recovered for recycle use; and the invention has advanced and reasonable process and less equipment investment through reasonable regulation of the adding amount of the trimethylolpropane and the isocaprylic acid and the proportion of the metal oxide catalyst and the optimal selection of reaction temperature and reaction time.

Description

technical field

[0001] The invention relates to a method for synthesizing trimethylolpropane triisooctanoate, and belongs to the technical field of synthesizing ester compounds in organic chemistry. Background technique

[0002] Trimethylolpropane triisooctanoate is a biodegradable polyol ester with excellent low temperature properties, good antioxidant stability and low volatility, excellent lubricity and hydrolytic stability. Used in high temperature greases, gear oils, chain oils and air compressors.

[0003] The existing synthetic method of trimethylolpropane triisooctanoate is mainly an acid alcohol esterification method, using trimethylolpropane and isooctanoic acid as raw materials, using p-toluenesulfonic acid, sulfuric acid, etc. as catalysts, and dehydration through esterification. to make. "Liaoning Chemical Industry", Vol. 34, No. 10, 2005, reported the synthesis of trimethylolpropane triisooctanoate by direct esterification of trimethylolpropane (TMP) and isoo...

Examples

Embodiment 1

[0016] Embodiment 1: successively add trimethylolpropane 174g, isooctanoic acid 646g, stannous oxide 0.41g in the reactor, pass N 2 , heat up to 215 ℃ under stirring, and react at this temperature to distill out the water generated by the reaction, after 8 hours of reaction, anhydrous distillates, and then the material is transferred to the deacidification kettle, the vacuum degree is 50Pa, the temperature is 140 ℃ Deacidified for 1.0h, cooled to 70°C and filtered to obtain trimethylolpropane isooctanoate.

Embodiment 2

[0017] Embodiment 2: successively add trimethylolpropane 174g, isooctanoic acid 683g, iron oxide 0.5999g in the reactor, pass N 2 , heat up to 200°C under stirring, and react at this temperature to distill out the water generated by the reaction, after 9 hours of reaction, anhydrous distillates, then the material is transferred to the deacidification kettle, the vacuum degree is 60Pa, the temperature is 130°C Deacidified for 1.0h, cooled to 70°C and filtered to obtain trimethylolpropane isooctanoate.

technical field

[0001] The invention relates to a method for synthesizing trimethylolpropane triisooctanoate, and belongs to the technical field of synthesizing ester compounds in organic chemistry. Background technique

[0002] Trimethylolpropane triisooctanoate is a biodegradable polyol ester with excellent low temperature properties, good antioxidant stability and low volatility, excellent lubricity and hydrolytic stability. Used in high temperature greases, gear oils, chain oils and air compressors.

[0003] The existing synthetic method of trimethylolpropane triisooctanoate is mainly an acid alcohol esterification method, using trimethylolpropane and isooctanoic acid as raw materials, using p-toluenesulfonic acid, sulfuric acid, etc. as catalysts, and dehydration through esterification. to make. "Liaoning Chemical Industry", Vol. 34, No. 10, 2005, reported the synthesis of trimethylolpropane triisooctanoate by direct esterification of trimethylolpropane (TMP) and isoo...

Examples

Embodiment 1

[0016] Embodiment 1: successively add trimethylolpropane 174g, isooctanoic acid 646g, stannous oxide 0.41g in the reactor, pass N 2 , heat up to 215 ℃ under stirring, and react at this temperature to distill out the water generated by the reaction, after 8 hours of reaction, anhydrous distillates, and then the material is transferred to the deacidification kettle, the vacuum degree is 50Pa, the temperature is 140 ℃ Deacidified for 1.0h, cooled to 70°C and filtered to obtain trimethylolpropane isooctanoate.

Embodiment 2

[0017] Embodiment 2: successively add trimethylolpropane 174g, isooctanoic acid 683g, iron oxide 0.5999g in the reactor, pass N 2 , heat up to 200°C under stirring, and react at this temperature to distill out the water generated by the reaction, after 9 hours of reaction, anhydrous distillates, then the material is transferred to the deacidification kettle, the vacuum degree is 60Pa, the temperature is 130°C Deacidified for 1.0h, cooled to 70°C and filtered to obtain trimethylolpropane isooctanoate.