Preparation method of N-methylamine compound

A technology of secondary amine compounds and compounds, applied in the field of preparation of N-methylamine compounds, which can solve the problems of complex preparation process, difficult separation of products, high production cost, etc.

Active Publication Date: 2017-01-11
SHANGHAI INST OF APPLIED PHYSICS - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved in the present invention is in order to overcome methylating reagent (such as formaldehyde, methyl iodide, dimethyl sulfate and dimethyl carbonate), organic reducing agent (organic reducing agent) when preparing N-methylamine compound in the prior art Silane, sodium borohydride, phenyl organic hydrogen source) are toxic and costly, and the use of CO 2 When reacting with amine to prepare N-methylamine, the preparation process is complicated, the raw material is expensive, it is not easy to separate from the product, it cannot be reused, the catalyst activity is low, the universality is poor, the reaction time is long, the catalyst is difficult to recycle, and the production cost is high. Due to the disadvantages of poor benefit and low safety, a preparation method for N-methylamine compounds is provided

Method used

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  • Preparation method of N-methylamine compound
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  • Preparation method of N-methylamine compound

Examples

Experimental program
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Effect test

Embodiment 1

[0079] Embodiment 1 (Al 2 o 3 carrier preparation)

[0080] Take a certain amount of aluminum nitrate and dissolve it in deionized water (0.8 mol / L), and add 2.6 mol / L ammonia solution while stirring until the pH value of the solution reaches about 9. Then stir at room temperature for 4 hours, then age for 2 hours, filter and wash for more than 3 times until there is no nitrate ion in the solution, and wash with ethanol for the last time. Al 2 o 3 carrier.

Embodiment 2

[0081] Embodiment 2 (Au / Al 2 o 3 Catalyst Preparation)

[0082] Au / Al with a theoretical loading of 1wt% 2 o 3 The catalyst is taken as an example, prepared by urea deposition precipitation method (DPU). The catalyst was prepared in a beaker wrapped in tin foil to avoid light. Under the condition of stirring at room temperature, the Al prepared in 1g embodiment 1 2 o 3 The carrier was added to 100 mL of chloroauric acid aqueous solution containing 0.48 mmol / L* (calculated as Au). Then add a certain amount of urea (urea / Au=200, molar ratio). The temperature of the water bath was then raised to 80°C under constant stirring and kept at this temperature for 6 hours. After cooling down to room temperature, filter and wash for more than 3 times until there is no chloride ion in the solution. After vacuum drying at 350°C using 5vol.% H 2 / Ar reduction for 2 hours, the heating rate was 5°C / min, and a powdered catalyst sample was prepared. The actual gold loading of the cata...

Embodiment 3

[0085] Embodiment 3 (Pt / Al 2 o 3 , Rh / Al 2 o 3 , Ir / Al 2 o 3 Catalyst Preparation)

[0086] Pipette an appropriate amount of chloroplatinic acid, rhodium nitrate, and chloroiridic acid aqueous solution in three beakers with 100 mL of deionized water respectively, and then add 1 gram of Al 2 o 3 The powder was uniformly stirred for 2 hours at 80°C, and then the water was evaporated to dryness at 90°C. The obtained solid was transferred into a watch glass and dried in a vacuum oven for 24 hours. The sample was placed in a muffle furnace for 400 ℃ roasting for 2 hours, and finally the roasted sample in 5vol.%H 2 / Ar atmosphere for 2 hours, the heating rate is 5° C. / min, and the powdery supported noble metal catalyst sample is prepared. Expressed as: 1%Pt / Al 2 o 3 , 1%Rh / Al 2 o 3 , 1%Ir / Al 2 o 3 .

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Abstract

The invention discloses a preparation method of a N-methylamine compound. The preparation method comprises the following steps: under an inertia organic solvent or solvent-free condition and under a support-type nano-sized gold catalyst effect, a primary amine compound or a secondary amine compound is subjected to a N-methylation reaction with carbon dioxide and hydrogen to obtain the product. The preparation method takes CO2 as a methyl source, takes hydrogen as a reducing agent, and takes the support-type nano-gold as a catalyst, and has the advantages that process is simple, catalyst activity is high, reaction rate is fast, the catalyst recovery and utilization are convenient, the application scope of a substrate is wide, the production cost is low, the benifit is high, the post-treatment is simple, repeatability is good, safe performance is high, and environmental protection is achieved, and the method is adapted to industrial production.

Description

technical field [0001] The invention relates to a preparation method of N-methylamine compounds. Background technique [0002] With the greenhouse gas CO in the air 2 With the gradual increase of the concentration, more and more scientists are paying attention to the CO 2 effective use. with CO 2 Synthesizing chemicals from raw materials, especially high value-added chemicals, has attracted extensive attention of researchers. CO 2 As a raw material, the industrialized process includes the following: Bosch-Meiser process (CO 2 react with NH3 to generate urea); Kolbe-Schmitt process (CO 2 Reaction with phenol to synthesize salicylic acid); synthesis of cyclic or polycarbonate. [0003] N-methylamine is an important chemical intermediate, which has a wide range of applications in industrial production, such as the manufacture of high value-added chemicals such as polymers, dyes, fragrances, fungicides, and synthetic leather. However CO 2 For a long time, there have bee...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/48C07C209/00C07C211/52C07C211/35C07C211/03C07C211/27C07D207/06C07D209/08C07D215/06C07D295/03C07D295/023C07D295/033C07D223/22C07D211/14B01J23/52B01J23/42B01J23/46
Inventor 杜贤龙关成志王建强
Owner SHANGHAI INST OF APPLIED PHYSICS - CHINESE ACAD OF SCI
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