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Method of preparing methylamine by methanol gaseous phase amination

A technology for preparing methylamine and methanol, applied in chemical instruments and methods, preparation of amino compounds, preparation of organic compounds, etc., can solve the problems of low dimethylamine selectivity and low catalytic activity, and achieve high conversion rate and high selectivity. performance, good handling stability and mechanical strength

Active Publication Date: 2005-05-25
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is that the balanced catalysts in the previous literature have the problems of low catalytic activity and low selectivity of dimethylamine, and a new method for producing methylamine by gas-phase amination of methanol is provided

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Weigh 100 grams of NaM (commercially available, where M is mordenite, SiO 2 / Al 2 O 3 Molar ratio=13) Exchange 2-10 times the amount of 1N ammonium nitrate aqueous solution at 95℃ for 10 hours, filter and wash, repeat the above process 2 to 3 times, the molecular sieve is exchanged into ammonium type NH 4 M(Na 2 O<0.2% by weight), dried at 130°C for 5 hours, exchanged with 1000 ml of 1N sodium nitrate aqueous solution at room temperature for 7 hours, and then dried and calcined to obtain NaHM.

[0032] Weigh 13.5 parts of pseudo-boehmite and an appropriate amount of dilute nitric acid aqueous solution to prepare a slurry aluminum sol under stirring. Take 3.5 parts of NaHM obtained above and 27.5 parts of silico-aluminum oxide (containing 20% ​​by weight of silicon) and mix, pour into the above-mentioned aluminum sol, knead evenly, extrude on an extruder, and cure overnight at room temperature, and dry at 130°C6 Then heat treatment at 550°C for 3 hours to cut into φ2×1~2mm. ...

Embodiment 2

[0034] 100 grams of NaM (commercially available, SiO 2 / Al 2 O 3 Molar ratio=25) Take 7 parts of this molecular sieve and 27.0 parts of silico-aluminum oxide (10% by weight of silicon) and 13.5 parts of pseudo-boehmite and mix well with Example 1 after ammonium and sodium exchange, and add dilute nitric acid, Kneading for 15 minutes, then adding 2 ml of 85% phosphoric acid dropwise, kneading for 15 minutes, extruding into a strip, curing overnight, drying at 130°C for 6 hours, and calcining at 550°C for 3 hours to obtain a modified catalyst. Shape and cut into φ2×1~2mm, take 2 grams of the catalyst and investigate the same as in Example 1. The tail gas sampling and analysis results are: methanol conversion rate 99.35%, monomethylamine selectivity 22.32%, dimethylamine selectivity 31.65%, The selectivity of trimethylamine is 46.03%.

Embodiment 3

[0036] 4.0 parts of NaM (commercially available, SiO 2 / Al 2 O 3 Molar ratio=13) After calcination at 550°C for 3 hours, mix with 30 parts of silico-aluminum oxide (containing 30% by weight of silicon) and 0.5 part of magnesium acetate, and add to the mixture made of 10.5 parts of pseudo-boehmite and appropriate amount of dilute nitric acid The aluminum sol was fully kneaded to form a dough, extruded, and dried in health. The catalyst was prepared and investigated in the same manner as in Example 1. The sampling and analysis results were: methanol conversion rate 99.16%, monomethylamine selectivity 21.37, and dimethylamine selectivity 30.81 , The selectivity of trimethylamine is 47.81%.

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Abstract

A process for preparing the methylamine from methanol by gas phase amination features the reaction between methanol and ammonia under existance of the catalyst consisting of crystalline silicoaluminate and composition of aluminium oxide and silicon oxide. Its advantages are high catalytic activity and high selectivity.

Description

Technical field [0001] The invention relates to a method for producing methylamine by gas-phase amination of methanol, and more specifically, to a method for producing methylamine by gas-phase amination of methanol and ammonia using a balanced catalyst. Background technique [0002] At present, the method for synthesizing methylamine on an industrial scale at home and abroad is generally based on γ-Al 2 O 3 , Al 2 O 3 -SiO 2 , AlPO, MgO, ThO 2 It is prepared by continuously passing methanol and ammonia through the reactor in the presence of a solid acid catalyst. The reaction is generally prepared by reaction at 0.5-4.0Mpa and 350-500°C. The reaction products generate three different methylamines, namely monomethylamine (MMA), dimethylamine (DMA) and trimethylamine (TMA) due to the difference in the number of methyl substitutions. Since the amorphous solid acid catalyst does not have a shape-selective function, the reaction product is controlled by th...

Claims

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Application Information

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IPC IPC(8): C07C209/16C07C211/04
Inventor 姜向东程文才杨德琴林遇春方志德
Owner CHINA PETROLEUM & CHEM CORP
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