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Method for preparing polyol ester lubricating oil by using composite solid acid catalyst

A composite solid acid and catalytic preparation technology is used in the preparation of polyol ester lubricating oils and the preparation of synthetic ester base oils for lubricating oils, and can solve the problems of complex post-treatment processes, poor catalytic performance, catalyst residues and the like, To achieve the effect of wide adaptability of raw material acid value, good catalytic effect and small catalyst residue

Inactive Publication Date: 2013-01-23
SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to overcome the use of strong acids or Lewis acid catalysts in the preparation of traditional polyol ester lubricating oils, poor catalytic performance, too many by-products, serious catalyst residue, complicated post-treatment process, large environmental pollution, Disadvantages such as high energy consumption and low product purity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Each take 20mlTiCl 4 and AlCl 3 The solution was fully stirred and hydrolyzed with 10% dilute ammonia water, and the solution was left to stand for 24 hours after being made alkaline, then filtered, and the precipitate was washed with distilled water until there were no chloride ions, and dried in an oven at 110°C. The dried mixed metal oxide Precipitate and grind into powder and place an equimolar amount of lanthanum sulfate in 2.0mol / L H at the same time 2 SO 4 Soak in the solution for 24 hours, then filter, and place the solid in a horse boiling furnace at 550°C to activate it for 3 hours to prepare the ternary composite solid acid catalyst SO 4 2- / TiO 2 -Al 2 o 3 -La 3+ , placed in a desiccator for later use.

[0025]Add 136.0 g of pentaerythritol, 528.0 g of n-heptanoic acid, 50.0 g of xylene and 1.32 g of the above-mentioned ternary composite solid acid catalyst prepared in a three-necked flask. Heat up to 160°C with stirring, measure the amount of wate...

Embodiment 2

[0027] Take 100mlTiCl 4 Solution, fully stirred and hydrolyzed with 8% dilute ammonia water, let the solution stand for 20 hours after being alkaline, then filtered, and washed the precipitate with distilled water until there were no chloride ions, and dried it in an oven at 110°C. The dried metal oxide precipitate Grind into powder and place an equimolar amount of lanthanum sulfate in 2.0mol / L of H at the same time 2 SO 4 Soak in the solution for 12 hours, then filter, and place the solid in a horse boiling furnace at 500°C to activate it for 5 hours to obtain a binary composite solid acid catalyst SO 4 2- / TiO 2 -La 3+ , placed in a desiccator for later use.

[0028] 13.6kg of pentaerythritol, 115.0kg of oleic acid, 25.0kg of toluene and 38.6g of the prepared binary composite solid acid catalyst were added to the reactor. Heat up to 180°C with stirring, measure the amount of water in the water separator, and stop heating after about 0.5 hours of reaction. After coolin...

Embodiment 3

[0030] Take 100mlZrCl 4 and 80mlAlCl 3 The solution was fully stirred and hydrolyzed with 12% dilute ammonia water, and the solution was left to stand for 12 hours after being made alkaline, then filtered, and the precipitate was washed with distilled water until there were no chloride ions, and dried in an oven at 110°C. The dried mixed metal oxide Precipitated and ground into powder, placed in 2.0mol / L H 2 SO 4 Soak in the solution for 12 hours, then filter, and place the solid in a horse boiling furnace at 600°C for 3 hours to activate it to obtain a binary composite solid acid catalyst SO 4 2- / ZrO 2 -Al 2 o 3 , placed in a desiccator for later use.

[0031] 13.4kg of trimethylolpropane, 43.5kg of isooctanoic acid, 5.0kg of xylene and 100g of the prepared binary composite solid acid catalyst were added to the reactor. Heat up to 140°C with stirring, measure the water volume in the water separator, and stop heating after about 1.0 hours of reaction. After cooling d...

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Abstract

The invention relates to a method for preparing polyol ester lubricating oil by using a composite solid acid catalyst. The method comprises the following steps of: adding a water carrying agent into polyol ester and monobasic fatty acid, performing esterification reaction under the action of the composite solid acid catalyst, and dehydrating and esterfying to obtain raw ester; performing filter pressing on the raw ester to separate the raw ester from the solid acid catalyst, wherein the catalyst can be recycled; and performing reduced pressure distillation on the raw ester to remove the residual fatty acid, and then deacidifying and decolorizing to refine with heating by using a refining adsorption bed layer respectively to obtain low-acid value polyol ester lubricating oil. The method has the advantages that the catalyst can be recycled, the esterification rate is high, an aftertreatment process is simple, and a product is low in acid value, high in purity, environment-friendly and suitable to be produced industrially. The reaction esterification rate can reach over 99 percent, and the acid value of the ester product obtained through refining can be controlled to be less than 0.01mg KOH / g. The product is excellent in visco-temperature performance, high in lubricity and thermal stability, strong in hydrolytic stability, low in volatility and excellent in electrical insulation property.

Description

technical field [0001] The invention relates to a preparation method of synthetic ester base oil for lubricating oil. More specifically, the present invention relates to a method for preparing polyol ester lubricating oil using a composite solid acid catalyst. It belongs to the field of organic synthesis. Background technique [0002] Polyol esters are esterified from polyols (such as trimethylolpropane, pentaerythritol, etc.) and monobasic fatty acids. Since there is no hydrogen in the ?-position carbon of polyols, the thermal oxidation stability of the corresponding esters is better. Due to its many ester groups, strong polarity, low evaporation loss, good lubricity, it has the advantages of high flash point, low pour point and excellent high and low temperature performance. [0003] Compared with traditional mineral lubricating oil, polyol ester technology lubricating oil has excellent viscosity-temperature performance, good thermal stability, low volatility, biodegrad...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/33C07C69/58C07C69/30C10M105/38
CPCY02P20/584
Inventor 杨东元段宝民许磊李霁阳刘世川
Owner SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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