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Synthesis method of ester oil

A synthesis method and technology of ester oil, applied in chemical instruments and methods, petroleum industry, carboxylate preparation, etc., can solve the problems of difficult removal of harmful substances, large amount of catalyst, slow reaction speed, etc., and improve thermal oxidation Stability, fast response, effect of reducing dosage

Active Publication Date: 2010-07-14
辽宁海华科技股份有限公司
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  • Abstract
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  • Claims
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AI Technical Summary

Problems solved by technology

Some use concentrated sulfuric acid as a catalyst, the esterification reaction is relatively complete, but there are many side reactions, resulting in a darker product color; some use phosphoric acid and phosphoric acid ester as a catalyst, the product color is lighter, but the reaction speed is slow and the esterification time is long; If the inorganic zinc oxide is used as the catalyst, an acid decomposition process must be added in the reaction process, the production time is long and the yield is low; in foreign countries, p-toluenesulfonic acid is used as the catalyst, and there are harmful substances that are difficult to remove in the product. Precipitation is easy to occur at high temperature
The amount of the above catalysts is about 1.5%-5.0%, and there are problems such as large amount of catalysts and difficulty in separation.

Method used

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preparation example Construction

[0029] A method for synthesizing ester oil, the method comprising the steps of:

[0030] 1) Add the composition of sulfuric acid and phosphoric acid as a combined catalyst to the alcohol and acid reactor; in the combined catalyst of sulfuric acid and phosphoric acid, the molar ratio of sulfuric acid and phosphoric acid is: 1: (2~4); The amount is 0.05-0.1% of the total weight of alcohol and acid.

[0031] 2) Carry out esterification reaction at 160°C-180°C, and generate crude ester after reacting for 2-6 hours;

[0032] 3) Blow ammonia or epoxy gas into the reactor for chemical deacidification; then blow one or more of nitrogen, steam, and argon into the reactor for physical deacidification; the addition of gas can be Quickly and efficiently remove free acid and other reaction by-products and residues in esterification products, and significantly improve the thermal oxidation stability, low temperature fluidity and other important properties of ester synthetic oils.

[0033]...

Embodiment 1

[0038] Preparation of Trimethylolpropane Trioleate

[0039] Put trimethylolpropane and oleic acid into the reaction kettle at a molar ratio of 3.2:1, add an appropriate amount of sulfur and phosphoric acid combined catalyst twice under stirring, raise the temperature to 120-130°C, and control the vacuum degree at -0.94MPa, React for 3 hours, then raise the temperature to 170-180°C, add the remaining combined catalyst for the third catalysis, so that the esterification continues to obtain crude ester, continue to react for 2 hours, and then blow epoxy gas into the kettle for a period of time 15h, the flow control is 18L / min, and then nitrogen is blown into the kettle for 20h, and the flow control is 25L / min. Chemical deacidification, further distilling the crude ester under reduced pressure, then dehydrating and drying under vacuum conditions and adding a polymerization inhibitor CPL, precision filtration, adding a polymerization inhibitor to the obtained filtrate to obtain tri...

Embodiment 2

[0043] Preparation of Pentaerythritol Tetraoleate

[0044] Put pentaerythritol and oleic acid into the reaction kettle in a molar ratio of 4:1, add an appropriate amount of sulfur and phosphoric acid combined catalyst in two times under stirring, raise the temperature to 120-130°C, control the vacuum degree at -0.94MPa, react for 3 hours, and then Raise the temperature to 170-180°C, add the combined catalyst again for the third catalysis, so that the esterification will continue to occur to obtain the crude ester, and after continuing the reaction for 2 hours, blow epoxy gas into the kettle for 13 hours, and the flow rate is controlled as 15L / min, and then blow nitrogen into the kettle, the feeding time is 20h, and the flow rate is controlled at 13L / min. They interact with the unreacted acid and half ester contained in the crude ester for physical deacidification and chemical deacidification, and further The crude ester was distilled under reduced pressure, then dehydrated and...

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Abstract

The invention relates to a method for synthesizing ester oil, wherein sulfuric acid and phosphoric acid are adopted in a molar ratio of 1: (2-4) and a composition with the amount thereof accounting for 0.05 to 0.1% of the total weight of alcohol and acid is added into an alcohol-acid reactor as a composite catalyst. The adding method of the composite catalyst comprises the steps of adding the composition in three stages during the alcohol and acid esterification reaction; subjecting the mixture to the reaction for 2 to 6 hours to generate raw ester; blowing epoxy gas into the reactor and then blowing one or more gases selected from nitrogen, steam and argon into the reactor and carrying out chemical deacidification and physical deacidification; then, carrying out reduced pressure distillation, dehydrating and drying under the vacuum condition; and finally, adding polymerization inhibitor into the reactor for precise filter, and obtaining the ester oil with high purity and high quality. The synthesis method has the advantages of rapid reaction speed, high esterification efficiency and greatly improving the purity of the product.

Description

technical field [0001] The invention relates to a new method for synthesizing ester oil, which belongs to the technical field of ester compound synthesis. Background technique [0002] Under the circumstances of increasing shortage of petroleum resources and deteriorating environmental pollution, energy saving, environmental protection and high efficiency have become the most concerned topics in society, and have become the main trend of lubricant research and development. Among them, synthetic ester base oils with renewable raw materials, biodegradable finished products and long service life are more and more widely used, and the synthesis technology of ester base oils has also been developed to a certain extent. [0003] The existing ester synthetic oil synthesis technologies at home and abroad mainly include alkyd esterification technology and transesterification technology. The alkyd esterification process is mainly obtained by esterification and dehydration of organic ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10M105/32C10M177/00C07C67/08C07C67/60C07C67/48C07C69/58C07C69/76
Inventor 李元鸿杜尚君赵丽
Owner 辽宁海华科技股份有限公司
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