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Separation of methylamine mixed gas and method for co-production of formamide compounds

A technology of mixed gas and formamide, which is applied in the preparation of organic compounds, chemical instruments and methods, purification/separation of amino compounds, etc., can solve problems such as large energy consumption, achieve low energy consumption, simple preparation, and reduced energy consumption Effect

Active Publication Date: 2021-08-17
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The amount of trimethylamine used as a feed additive is still relatively small, but there is still a lot of room for growth
Therefore, the preparation and separation of the three methylamine molecules need to go through a complicated rectification section
Due to the azeotropic phenomenon between methylamine molecules, there is a large energy consumption in the separation process

Method used

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  • Separation of methylamine mixed gas and method for co-production of formamide compounds

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Weigh 20g MoO 3 impregnated in 48.6mmol·L -1 hydrated ruthenium trichloride solution, stirred at room temperature for 20h, dried at 130°C, and reduced at 350°C for 3h in a hydrogen atmosphere to obtain 2wt% Ru / MoO 3 , forming a 14-25 mesh catalyst and filling it into the reaction tube, filling the 15mm bed, and under the pressure of 3.0MPa, the flow rate of the mixed gas of methylamine is 10mL·min -1 , wherein monomethylamine: dimethylamine: trimethylamine=1:2:1 (volume ratio), the flow rate of raw material CO is 10mL min -1 . Reaction at 200°C, sampling every 2 hours, the concentration of trimethylamine increased to 73%; chromatographic analysis showed that the total selectivity of formamide compounds was 90%.

Embodiment 2

[0021] Weigh 20g CuO and impregnate in 48.6mmol L -1 in a solution of ruthenium trichloride hydrate, stirred at room temperature for 20 hours, dried at 130°C, and reduced for 3 hours at 350°C in a hydrogen atmosphere to obtain 2wt% Ru / CuO, and filled the reaction tube with a 14-25 mesh catalyst by forming a sieve. 15mm bed layer, after filling the catalyst in the reaction tube, place the reaction tube in a fixed bed reactor, under the pressure of 3.0MPa, the flow rate of the mixed gas of methylamine is 10mL·min -1 , wherein monomethylamine: dimethylamine: trimethylamine=1:2:1 (volume ratio), the flow rate of raw material CO is 10mL min -1 . Reaction at 200°C, sampling every 2 hours, the concentration of trimethylamine increased to 78%; chromatographic analysis showed that the total selectivity of formamide compounds was 92%.

Embodiment 3

[0023] Weigh 20g Co 3 o 4 impregnated in 48.6mmol·L -1 hydrated ruthenium trichloride solution, stirred at room temperature for 20 h, dried at 130 ° C, and reduced for 3 h at 350 ° C in a hydrogen atmosphere to obtain 2wt% Ru / Co 3 o 4 , take 14-25 mesh catalyst and fill it into the reaction tube, fill the 15mm bed layer, put the reaction tube in the fixed bed reactor after filling the catalyst in the reaction tube, under the pressure of 3.0MPa, the mixture gas of methylamine The flow rate is 10mL·min -1 , wherein monomethylamine: dimethylamine: trimethylamine=1:2:1 (volume ratio), the flow rate of raw material CO is 10mL min -1 . Reaction at 200°C, sampling every 2 hours, the concentration of trimethylamine increased to 86%; chromatographic analysis showed that the total selectivity of formamide compounds was 89%.

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Abstract

The invention relates to a method for the separation of methylamine mixed gas and the co-production of formamide compounds. The methylamine mixed gas, especially monomethylamine and dimethylamine in the methylamine mixed gas with a high ratio of monomethylamine and dimethylamine, is combined with CO undergoes carbonylation and transamidation reactions, and after separation and transformation, high-purity trimethylamine is obtained, and formamide and N,N-dimethylformamide are co-produced simultaneously. Using the mixed gas of CO gas and methylamine as the reactant, the Ru / CeO 2 Under the action of the catalyst, monomethylamine is selectively carbonylated with CO to form formamide, and then formamide and dimethylamine are transacylated to form N,N-dimethylformamide, so as to achieve the purpose of purifying trimethylamine , to co-produce two formamide compounds simultaneously. The used catalyst can be reused after being calcined and reduced. The method of the invention is simple in operation and low in cost, can be used for large-scale separation of methylamine mixed gas, and co-produces formyl compounds in high yield.

Description

technical field [0001] The invention relates to a method for separating methylamine mixed gas, in particular to a method for obtaining high-purity trimethylamine after the separation and conversion of monomethylamine and dimethylamine in the methylamine mixed gas with CO. The separation of gas and the method of co-producing formamide compounds simultaneously, and the co-production of formamide compounds. Background technique [0002] Methylamine mixed gas is a general name for a mixture of monomethylamine (MMA), dimethylamine (DMA) and trimethylamine (TMA). Among them, methylamine is mainly used in pesticides, medicines, dyes, surfactants, water gel explosives, fuels, photographic developing drugs, gas purifiers and industrial solvents. Dimethylamine is mainly used in pesticides, medicines, rubber accelerators, fatty tertiary amines, industrial solvents (DMF), dimethylacetamide (DMA), etc., and organic intermediates. The amount of trimethylamine used as a feed additive is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/04C07C209/86C07C233/03C07C231/10C07C231/08
CPCC07C209/86C07C231/08C07C231/10C07C211/04C07C233/03
Inventor 王峰王业红张健张志鑫
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI