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Production method of dimethylamine

A manufacturing method and technology of dimethylamine, which are applied in the directions of organic chemistry methods, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems such as the decrease of DMA selectivity.

Inactive Publication Date: 2005-08-31
MITSUBISHI RAYON CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is an object of the present invention to provide a process for the production of dimethylamine using a novel zeolite catalyst as the catalyst used in the production of dimethylamine from methanol and / or a mixture of methylamine and ammonia, providing higher DMA selectivity and lower A new zeolite catalyst with TMA selectivity and higher methanol consumption reaction activity can improve the defect that the DMA selectivity drops sharply when the conversion rate of methanol is greater than or equal to 95% when using the existing zeolite catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The powdered sodium mordenite was refluxed and boiled for 6 hours with 20 times the weight of 3 equivalents (N) of ammonium nitrate solution. The mordenite was filtered out, and 3 equivalents (N) of ammonium nitrate solution was added again, and reflux was boiled for 6 hours, and a total of 4 cycles were performed. The mordenite obtained by filtration was washed with water, dried at 130° C. for 6 hours, and then fired at 450° C. for 3 hours to obtain H-type (hydrogen-type) mordenite. Mordenite having a sodium content of 0.4% by weight was prepared by boiling 100 g of the H-type mordenite with 1 liter of a 1 N (N) sodium nitrate solution at 40° C. for 20 hours under reflux. The molar ratio of Si / Al atoms in this H-type mordenite was 6.0. The mordenite was shaped into cylindrical particles with a diameter of 3 mm. 50 g of this H-type mordenite was immersed in 500 g of a toluene solution in which 50 g of triethylphosphate was dissolved, at 100° C. for 4 hours. After the...

Embodiment 2

[0027] 50 g of H-type mordenite obtained in Example 1 was treated in the same manner as in Example 1, except that 500 g of toluene solution in which 150 g of triethylphosphate was dissolved was used for the reaction. The phosphorus content in the obtained modified mordenite catalyst was 0.33% by weight. As a result, a methylamine mixture having the composition shown in Table 1 was obtained. In addition, by-products such as dimethyl ether were not found.

Embodiment 3

[0029] 50 g of H-type mordenite obtained in Example 1 was treated in the same manner as in Example 1, except that 500 g of toluene solution in which 250 g of triethylphosphate was dissolved was used for the reaction. The phosphorus content in the obtained modified mordenite catalyst was 0.36% by weight. As a result, a methylamine mixture having the composition shown in Table 1 was obtained. In addition, by-products such as dimethyl ether were not found.

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Abstract

Conventional zeolite catalysts for the preparation of dimethylamine from methanol or a methylamine mixture and ammonia have a disadvantage in that the selectivity for dimethylamine is steeply lowered when the conversion of methanol becomes 95% or above. The invention aims at overcoming the disadvantage to thereby provide a novel zeolite catalyst attaining a higher selectivity for dimethylamine, a lower selectivity for trimethylamine, and a higher activity for methanol-consumption reaction. A process for preparing dimethylamine by conducting a reaction between methanol and ammonia, among methanol, a methylamine mixture, and ammonia, or between a methylamine mixture and ammonia in the presence of a zeolite catalyst in a vapor phase, wherein the reaction is conducted in the presence of a zeolite catalyst treated with a solution of an organophosphorus compound.

Description

technical field [0001] The invention relates to a method for producing dimethylamine by gas-phase contact reaction of methanol and / or methylamine mixture with ammonia. More specifically, the present invention relates to a process for the production of dimethylamine using an improved zeolite as a catalyst. Dimethylamine is an important chemical intermediate used as a raw material for various solvents, pharmaceuticals, rubber preparations, surfactants, etc. [0002] Dimethylamine is generally produced by gas-phase reaction of methanol and ammonia at high temperature (about 400°C) in the presence of solid acid catalysts such as alumina and aluminum silicate that have dehydration and ammoniation functions. In this reaction, in addition to dimethylamine (hereinafter referred to as DMA), side reactions also occur to generate monomethylamine (hereinafter referred to as MMA) and trimethylamine (hereinafter referred to as TMA). These byproduct methylamines, due to their The requireme...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07B61/00C07C209/02C07C209/16C07C211/04
CPCC07C209/16
Inventor 广幡实男星野学兼子功
Owner MITSUBISHI RAYON CO LTD
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