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Synthesis method of triethylamine and catalyst used in method

A triethylamine and catalyst technology, applied in the field of organic compound synthesis, can solve the problems of difficult separation of triethylamine, complex reaction process, poor product quality, etc., and achieve low price, simple operation, and good atom economy Effect

Active Publication Date: 2014-01-01
ZHEJIANG JIANYE CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method of using haloethane as raw material is to react haloethane and ammonia in aqueous solution or alcohol solution to obtain triethylamine. The disadvantage of this method is that the reaction is a nucleophilic reaction, and the primary and secondary amines generated in the reaction Both triethylamine and tertiary amine are nucleophilic reagents, and the resulting mixture is primary amine, secondary amine, tertiary amine and quaternary ammonium salt, and it is difficult to separate triethylamine from the product
According to the report, the method for preparing triethylamine by the action of ethanol and ammonia is to enter the preheater (150±5° C.) for preheating after ethanol and liquid ammonia are vaporized in the presence of hydrogen, and then enter the copper-nickel- The first reactor (190±2°C) and the second reactor (165±2°C) of the clay catalyst are synthesized to generate a mixture of ethylamine, diethylamine, and triethylamine, which are condensed and then sprayed with ethanol Absorb the crude product of triethanolamine, and finally through separation, dehydration and fractionation, collect the fraction at 88-90°C to obtain triethylamine. The preparation of triethylamine by this method is complicated in the reaction process, consumes a lot of energy, and the final product contains water and other impurities. Poor quality
These two methods also have a disadvantage, that is, the water generated in the reaction process is easy to azeotrope with the amine compound, which leads to various problems such as difficult separation of products and decline in product quality.
In recent years, it has also been reported that ethylene and diethylamine are used as raw materials to synthesize triethylamine, as reported in the literature (Journal of Molecular Catalysis A: Chemical241 (2005) 175-183) with ethylene and diethylamine as raw materials, LiNEt 2 -TMED is used as a catalyst to synthesize triethylamine at 70bar and 140°C, and the yield can reach 83%, but the activity of the catalyst in this reaction is low, and the amount of catalyst used is large, which leads to an increase in production cost, which is not conducive to industrial production

Method used

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  • Synthesis method of triethylamine and catalyst used in method
  • Synthesis method of triethylamine and catalyst used in method
  • Synthesis method of triethylamine and catalyst used in method

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Embodiment 1

[0038] Embodiment 1, a kind of production method that ethylamine and diethylamine disproportionation reaction synthesizes triethylamine, carry out according to the following steps successively:

[0039] 1), preparation of nickel-copper-palladium catalyst (i.e., a supported catalyst for the synthesis of triethylamine);

[0040] a), commercially available γ-Al with a particle diameter of 2 to 3 mm 2 o 3 First roast at 240-260°C for 3 hours, and then roast at 290-310°C for 3 hours; get roasted γ-alumina. After testing: the specific surface area of ​​the γ-alumina after roasting is 230-250m 3 / g, the pore size is 10-11.5nm; the particle diameter remains unchanged.

[0041] b), the roasted γ-Al obtained in step a) 2 o 3 Immerse in water for 36 hours, and then measure the volume of water reduction, so as to obtain the γ-Al after calcination 2 o 3 The pore volume density is 0.75ml / g;

[0042]c), with 46.71g nickel nitrate solid (not containing crystal water, hereinafter the s...

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Abstract

The invention discloses a load type catalyst for synthesis of triethylamine. The catalyst comprises the components of the calcined gamma-aluminum oxide (Al2O3) serving as a carrier and active components loaded on the carrier; the active components consist of nickel, copper and palladium; the nickel accounts for 15 to 25 percent of the total weight of the nickel, the copper, the palladium and the calcined gamma-Al2O3; the copper accounts for 5 to 12 percent of the total weight of the nickel, the copper, the palladium and the calcined gamma-Al2O3; and the palladium accounts for 1 to 3 percent of the total weight of the nickel, the copper, the palladium and the calcined gamma-Al2O3. The invention further discloses a preparation method for the load type catalyst. The invention further discloses a method for synthesizing the triethylamine by utilizing the load type catalyst. The method comprises the following steps of mixing ethylamine and diethylamine in a mixed tank to obtain mixed liquid; vaporizing the mixed liquid; performing disproportionated reaction by using a fixed bed reactor containing the activated load type catalyst under the hydrogenation condition; condensing after the reaction is finished; collecting condensation products; and rectifying to obtain the triethylamine.

Description

technical field [0001] The invention relates to a method for synthesizing an organic compound and a method for preparing a catalyst, in particular to a method for synthesizing triethylamine through the disproportionation reaction of ethylamine and diethylamine and a method for preparing a nickel-copper-palladium catalyst. Background technique [0002] Triethylamine, also known as N, N-diethylethylamine, is the simplest three-substituted tertiary amine that is liquid at room temperature (boiling point is 89.5°C), so it is widely used as a solvent and base in organic synthesis used, generally abbreviated as Et 3 N.NEt 3 or TEA. In industry, it is mainly used as alkali, catalyst, solvent and raw material in organic synthesis, and also used as high-energy fuel, rubber vulcanization accelerator, polymerization inhibitor of tetrafluoroethylene, surfactant, wetting agent, preservative and bactericide. [0003] At present, the industrial method for preparing triethylamine is main...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/89C07C211/05C07C209/64
Inventor 陈新志贾银霞钱超冯烈陈云斌许京伟
Owner ZHEJIANG JIANYE CHEM
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