Method of Boehmite Composite Alkaline Ionic Liquid Catalyzed Transesterification Reaction

A technology of transesterification and basic ions, applied in catalytic reactions, chemical instruments and methods, organic compound/hydride/coordination complex catalysts, etc., can solve catalyst recovery and recycling loss, increase equipment investment and operation Difficulty, harsh process conditions of transesterification reaction, etc., to achieve the effect of reducing equipment investment, facilitating large-scale industrial production, and excellent thermal stability

Active Publication Date: 2020-12-01
YANCHENG TEACHERS UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, there have been research reports on the catalyzed transesterification reaction of basic ionic liquids, mainly using imidazole-type basic ionic liquids and pyridine-type basic ionic liquids, such as [bmim]Br, [bmim]OH, [Emim]Im , [bPy]OH to catalyze the transesterification reaction, but these methods have one or more of the following defects: high catalyst cost, complex synthesis; harsh process conditions for the transesterification reaction, high temperature and pressure are required; raw materials need to be pretreated Removal of moisture increases equipment investment and operational difficulty; catalyst is not stable enough when heated (K.Guo, M.J.Thompson, B.Chen.J.Org.Chem.2009, 74, 6999-7006); catalyst recovery and recycling The loss is serious; the catalytic system is a homogeneous liquid system, and it is difficult to separate the catalytic system after the reaction, etc.

Method used

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  • Method of Boehmite Composite Alkaline Ionic Liquid Catalyzed Transesterification Reaction
  • Method of Boehmite Composite Alkaline Ionic Liquid Catalyzed Transesterification Reaction
  • Method of Boehmite Composite Alkaline Ionic Liquid Catalyzed Transesterification Reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Preparation of basic ionic liquid: In a 100mL round bottom flask, add 0.1mol (15.8g) (2-chloroethyl) trimethyl ammonium chloride, 0.1mol (5.61g) potassium hydroxide and 30mL absolute ethanol, room temperature Under the conditions, stirring and reacting for 2 to 3 hours, filtering to remove potassium chloride precipitate, reducing price distillation to remove the ethanol solvent, vacuum drying to obtain a colorless liquid which is the target ionic liquid, and the yield is 95%;

[0032] Boehmite composite ionic liquid: in a 50mL round bottom flask, add alkaline ionic liquid, boehmite (mass percentage of alkaline ionic liquid and boehmite=1:0.5~1.0), and 20mL cyclohexane successively, Stir and react under reflux for 5-6 hours, cool, filter, wash with absolute ethanol, and dry to obtain the target compound ionic liquid complex with a yield of 98%.

Embodiment 2

[0034] In a 100mL round bottom flask, add 0.067mol (20g) of fatty acid methyl ester, 0.067mol (4.97g) of n-butanol and 0.1g of boehmite composite basic ionic liquid catalyst, heat to 58°C, and mix and stir under normal pressure React for 1.0 hour, cool to room temperature, filter to separate and recover the catalyst, transfer the filtrate to a separatory funnel and let it stand for stratification. The lower layer is a mixture of methanol and unreacted butanol. Pressure distillation separates methanol and butanol, which can be reused; the upper layer is the crude product of fatty acid n-butyl ester, washed with water, dried, and can be refined by distillation under reduced pressure at 400Pa or rectification with a rectifying tower, and the yield is 81 %.

Embodiment 3

[0036] In a 100mL round bottom flask, add 0.067mol (20g) of fatty acid methyl ester, 0.067mol (4.97g) of n-butanol and 1.0g of boehmite composite basic ionic liquid catalyst, heat to 62°C, and mix and stir under normal pressure After reacting for 6.0 hours, it was cooled to room temperature, and the remaining operations were the same as in Example 2, and the yield was 85%.

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Abstract

The invention discloses a boehmite composite basic ionic liquid catalysis method of transesterification. By using a compound of boehmite and a basic ionic liquid as a catalyst, fatty acid methyl esterand fatty alcohol which are used as raw materials are heated and stirred at normal pressure to obtain a transesterification product. in comparison with the prior art, the method of the invention hasthe following advantages: (1) the compound catalyst has a wide source of raw materials and is convenient to prepare; the catalyst has high activity and low dosage; (2) there is no need to pretreat rawmaterials, and the pretreatment process is simplified; and (3) the catalyst has excellent heat stability, is a heterogeneous catalysis system is convenient to separate and recover, can be recycled, has environmental and economic double benefits, and is beneficial to large-scale industrial production.

Description

[0001] A technical field [0002] The invention relates to a method for catalyzing a transesterification reaction with a boehmite composite alkaline ionic liquid, and belongs to the technical field of chemical material preparation. This method is suitable for the occasion where fatty acid methyl ester and fatty alcohol are used as raw materials to carry out transesterification reaction under normal pressure and heating conditions. [0003] Two background technology [0004] Biomass energy is one of the world-recognized new energy sources. Many countries, including China, have a large amount of renewable resources such as oils and fats, which will produce a large number of by-products in the production process, including fatty acid glycerides in the form of esters, and free fatty acids. The carbon chain of the fatty acid here is a long-chain fatty acid. When the carbon chain of the fatty acid is 12-18, its methyl ester is the basic component of biodiesel, and a new road has bee...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C11C3/10C10L1/02B01J31/26
CPCB01J31/0239B01J31/26B01J2231/49C10L1/02C11C3/10
Inventor 方东董浩浩仲云雷刘文雨李佳琪
Owner YANCHENG TEACHERS UNIV
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