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Dimethylamine production method

A manufacturing method and technology of dimethylamine, applied in the direction of organic chemical methods, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of increased usage of modifiers, low activity, low production rate, etc.

Inactive Publication Date: 2007-09-05
MITSUBISHI RAYON CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In JP-A No. 61-254256, it is described that a modified zeolite catalyst is used to treat chabazite and erionite with a compound containing at least one element selected from silicon, aluminum, phosphorus and boron. , zeolite rho or zeolite ZK-5, to precipitate elements on zeolite, but because only the modifier is used, the amount of modifier used is increased. In addition, in terms of reaction results, the activity is also small, and the formation from methanol to methylamine The rate is also low, and there is a problem that a large amount of by-products such as dimethyl ether are produced

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] In 1000 ml of 2N hydrochloric acid solution, the natural mordenite with a crystallinity of 64% was immersed at 80° C. for 8 hours. After the treatment, it was washed with water, dried at 130° C. for 4 hours, and calcined at 570° C. for 4 hours to obtain H-type mordenite. The Na content at this time was 0.3% by mass. In addition, when the particle size distribution is calculated from the cumulative distribution curve, the catalyst with a particle size of 5 mm or more is 3.8% by mass, and the catalyst with a particle size of 2 mm or less is 1.0% by mass. Using this mordenite catalyst, a reaction for producing dimethylamine from ammonia and methanol was performed. The reaction results at 72 hours after the start of the reaction are as follows.

[0041] Methanol conversion rate: 93.1%

[0042] Monomethylamine selectivity: 27.3%

[0043] Dimethylamine selectivity: 62.9%

[0044] Trimethylamine selectivity: 9.9%

[0045] Reaction rate constant k: 0.21[1 / s]

Embodiment 2

[0047] In 1000 ml of 2N hydrochloric acid solution, 200 g of naturally occurring mordenite with a crystallinity of 57% was dipped at 80° C. for 8 hours. After the treatment, it was washed with water, dried at 130° C. for 4 hours, and calcined at 570° C. for 4 hours to obtain H-type mordenite. The Na content at this time was 0.2% by mass. In addition, when the particle size distribution is obtained from the cumulative distribution curve, the catalyst with a particle size of 5 mm or more is 4.0% by mass, and the catalyst with a particle size of 2 mm or less is 1.3% by mass. Using this mordenite catalyst, a reaction for producing dimethylamine from ammonia and methanol was performed. The reaction results at 72 hours after the start of the reaction are as follows.

[0048] Methanol conversion rate: 92.8%

[0049] Monomethylamine selectivity: 28.3%

[0050] Dimethylamine selectivity: 60.9%

[0051] Trimethylamine selectivity: 10.8%

[0052] Reaction rate constant k: 0.20[1 / s]...

Embodiment 3

[0054] In 1000 ml of 2N hydrochloric acid solution, 200 g of naturally occurring mordenite with a crystallinity of 46% was dipped at 80° C. for 8 hours. After the treatment, it was washed with water, dried at 130° C. for 4 hours, and calcined at 570° C. for 4 hours to obtain H-type mordenite. The Na content at this time was 0.2% by mass. In addition, when the particle size distribution is calculated from the cumulative distribution curve, the catalyst with a particle size of 5 mm or more is 4.1% by mass, and the catalyst with a particle size of 2 mm or less is 1.3% by mass. Using this mordenite catalyst, a reaction for producing dimethylamine from ammonia and methanol was performed. The reaction results at 72 hours after the start of the reaction are as follows.

[0055] Methanol conversion: 92.1%

[0056] Monomethylamine selectivity: 25.9%

[0057] Dimethylamine selectivity: 57.4%

[0058] Trimethylamine selectivity: 16.7%

[0059] Reaction rate constant k: 0.21[1 / s]

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Abstract

The invention provides a new zeolite catalyst which improves the defect of the conventional zeolite catalyst that the DMA (dimethylamine) selectivity rapidly decreases when the conversion of methanol comes to 95% or more, has a higher methanol consumption reaction activity, and gives a high DMA selectivity and a low TMA (trimethylamine) selectivity.A method for preparing dimethylamine comprises reacting methanol with ammonia, methanol and a methylamine mixture with ammonia or a methylamine mixture with ammonia in the presence of a catalyst in the gas phase, and natural mordenite having a degree of crystallinity of >=40% is used as the catalyst.

Description

technical field [0001] The present invention relates to a method for producing dimethylamine through gas-phase contact reaction of methanol and ammonia using zeolite catalyst. More specifically, it relates to a method for producing dimethylamine using natural mordenite having sufficient crystallinity as a zeolite catalyst. Dimethylamine is an important chemical intermediate as a raw material for various solvents, pharmaceuticals, rubber chemicals, surfactants, etc. Background technique [0002] Generally, methylamine is produced by reacting methanol and ammonia in the gas phase at high temperature (about 400° C.) in the presence of a solid acid catalyst having dehydration and amination functions of alumina, silica-alumina, and the like. Dimethylamine (hereinafter, referred to as DMA), monomethylamine (hereinafter, referred to as MMA), and trimethylamine (hereinafter, referred to as TMA) are produced in this reaction. Since MMA and TMA require significantly less than DMA, t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/04C07C209/02C07C209/16C07C209/68C07C209/22C07B61/00
Inventor 广幡实男星野学
Owner MITSUBISHI RAYON CO LTD