Method for catalytically synthesizing di-2-ethyhexyl carbonate by alkali ionic liquid

A technology of diisooctyl carbonate and synthesis method, which is applied in the direction of organic carbonate preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems such as no report of diisooctyl carbonate, and achieve high selectivity , simple operation process and high yield

Inactive Publication Date: 2010-06-16
DALIAN POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the use of acidic or alkaline ionic liquids as catalysts to catalyze transesterification, the preparation of di-isooctyl carbonate technology has no report

Method used

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  • Method for catalytically synthesizing di-2-ethyhexyl carbonate by alkali ionic liquid
  • Method for catalytically synthesizing di-2-ethyhexyl carbonate by alkali ionic liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] In a 250mL four-necked flask equipped with a stirrer, a thermometer, a condenser, and a constant pressure dropping funnel, add 64.37g of isooctyl alcohol and 0.86g of 1-ethyl-3-methylimidazolium chloride, heat up to 60°C, and slowly Add 22.26 g of dimethyl carbonate dropwise at a constant speed, and drop it for about 1 hour. Keep the reaction at 60°C for 9 hours, and then connect to a water separator to distill out the methanol and unreacted dimethyl carbonate generated by the reaction. Then, the temperature was raised to 110° C. for 3 hours, and after the reaction was completed, the mixture was cooled and distilled under reduced pressure, and allowed to stand and separate into layers. The upper liquid was distilled under reduced pressure at 3 mmHg to collect a colorless liquid at 170°C to obtain 39.60 g of the product with a yield of 55.92%.

Embodiment 2

[0022] In a 250mL four-neck flask equipped with a stirrer, a thermometer, a condenser, and a constant pressure dropping funnel, add 124.04g of isooctyl alcohol and 2.91g of 1-butyl-3-methylimidazolium imidazolium salt, heat up to 70°C, and slowly Add 21.45g of dimethyl carbonate dropwise at a constant speed, and drop it for about 1 hour. After keeping at 70°C for 8 hours, connect the water separator to distill out the methanol and unreacted dimethyl carbonate generated by the reaction. Then, the temperature was raised to 140° C. for 4 hours, and after the reaction was completed, it was cooled and distilled under reduced pressure, and allowed to stand for stratification. The viscous liquid in the lower layer is 1-butyl-3-methylimidazolium imidazolium salt which can be used twice. The upper liquid was distilled under reduced pressure at 6mmHg to collect a colorless liquid at 180°C to obtain 49.28g of the product with a yield of 72.23 %.

Embodiment 3

[0024] In a 250mL four-neck flask equipped with a stirrer, a thermometer, a condenser, and a constant pressure dropping funnel, add 90.20g of isooctyl alcohol and 2.23g of 1-ethyl-3-methylimidazole hydroxide, and heat up to 80°C , Slowly add 21.42g of dimethyl carbonate dropwise at a uniform speed, and drop it for about 1 hour. Keep the reaction at 80°C for 6 hours and then connect to the water separator to distill out the methanol and unreacted dimethyl carbonate generated by the reaction. Then the temperature was raised to 100° C. for 5 hours, and after the reaction was completed, the mixture was cooled and distilled under reduced pressure, and allowed to stand for stratification. The viscous liquid in the lower layer is 1-ethyl-3-methylimidazole hydroxide which can be used twice. The upper liquid is distilled under reduced pressure at 10 mmHg to collect a colorless liquid at 240 ° C to obtain 40.94 g of the product. The yield is 49.09%.

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Abstract

The invention provides a catalytic synthesis method for ionic liquid of di-2-ethyhexyl carbonate and belongs to the technical field of synthesis of ester compounds in organic chemistry. The method comprises the following steps of: performing the two-step ester exchange reaction of isooctanol and methyl carbonate serving as raw materials by alkali ionic liquid serving as a catalyst, and distilling the products by decompression to obtain the di-2-ethyhexyl carbonate, wherein the negative ion in the alkali ionic liquid is one of [OAc]-, Im-, OH-, Br-, Cl- and I- ions or a compound system formed by more of [OAc]-, Im-, OH-, Br-, Cl- and I- ions, the positive ion is 1-alkyl 3-methylimidazole, and the length of the carbon chain of the alkyl group is 1 to 13. The ionic liquid is added in an amount of 1 to 50 percent based on the total mass of the reaction raw materials, and the yield of the di-2-ethyhexyl carbonate is 45 to 85 percent. The alkali ionic liquid is used as the catalyst in the method, so that the method has the advantages of recovery of the catalyst, stable quality and yield of the product, advanced and reasonable process and easy operation.

Description

technical field [0001] The invention relates to an ionic liquid catalytic synthesis method of diisooctyl carbonate, belonging to the technical field of catalytic synthesis of ester compounds in organic chemistry. Background technique [0002] Diisooctyl carbonate is a colorless clean oil with strong polar ester group, good lubricating properties, low freezing point and pour point, good compatibility with hydrocarbon oils, and high thermal oxidation stability. One of the important chemical raw materials for synthetic base oil. Compared with other ester compounds, diisooctyl carbonate is not easy to saponify, and can rapidly biodegrade. It has a strong absorption effect on ultraviolet rays between 200-320nm, and can also be used as ultraviolet shielding in the fields of daily chemicals and functional materials. agent. The synthetic route of di-isooctyl carbonate mostly adopts dimethyl carbonate and iso-octanol as raw materials, uses solid base as catalyst, and synthesizes th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/96C07C68/06B01J31/02
Inventor 张绍印潘素娟王大鸷
Owner DALIAN POLYTECHNIC UNIVERSITY
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