Method for preparing dimethylamino propylamine through hydrogenating dimethylamino propionitrile in presence of nickel

A technology for catalyzing dimethylaminopropionitrile and dimethylaminopropionitrile is applied in the preparation of amino compounds, chemical instruments and methods, preparation of organic compounds, etc., and achieves the improvement of selectivity, activity and selectivity, and reduction of operating costs. Effect

Active Publication Date: 2015-04-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, judging from the reaction results, there is still a lot of room for improvement in its effect.

Method used

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  • Method for preparing dimethylamino propylamine through hydrogenating dimethylamino propionitrile in presence of nickel
  • Method for preparing dimethylamino propylamine through hydrogenating dimethylamino propionitrile in presence of nickel
  • Method for preparing dimethylamino propylamine through hydrogenating dimethylamino propionitrile in presence of nickel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] 1.5kg nickel, 1.0kg aluminum, 0.4kg Mo 10 Al 90 Add the alloy and 0.1kg cobalt into the graphite crucible, heat it in a high-frequency furnace until it melts, and then spray the molten liquid from the nozzle of the crucible onto a nickel roller with a rotation speed of 600 to 1000 rpm. Cooling water and alloy liquid are rapidly cooled at a cooling rate of 1000°C / s and then thrown out along the tangent line of the nickel roll to form scale-like strips, which are ground to a particle diameter of less than 70 microns to obtain a master alloy. Slowly add 50 g of the master alloy into a three-neck flask filled with 500 g of 20 wt % sodium hydroxide aqueous solution, control its temperature at 80° C. and keep stirring at constant temperature for 1 hour. After stopping heating and stirring, the liquid was filtered off and washed with distilled water at 100°C until the pH value was 7. The prepared catalyst is numbered Catalyst-1, and the composition of Catalyst-1 is shown in ...

Embodiment 2

[0017] 1.5kg nickel, 1.0kg aluminum, 0.4kg Mo 5 Al 95 Add the alloy and 0.1kg iron into the graphite crucible, heat it in a high-frequency furnace until it melts, and then the molten liquid is sprayed from the nozzle of the crucible onto a nickel roller with a rotation speed of 900 rpm, and cooling water is passed through the nickel roller , the alloy liquid is rapidly cooled at a cooling rate of 1000°C / s, and then thrown out along the tangent line of the nickel roller to form scale-like strips, which are ground to a particle diameter of less than 70 microns to obtain a master alloy. Slowly add 50 g of the master alloy into a three-neck flask filled with 500 g of 20 wt % sodium hydroxide aqueous solution, control its temperature at 80° C. and keep stirring at constant temperature for 1 hour. After stopping heating and stirring, decant the liquid and wash with distilled water at 80°C until the pH value is 7. The prepared catalyst is numbered Catalyst-2, and the composition of...

Embodiment 3

[0019] 1.2kg nickel, 1.0kg aluminum, 0.5kg Mo 10 Al 90 Add the alloy and 0.3kg manganese into the graphite crucible, heat it in a high-frequency furnace until it melts, spray the melt from the nozzle of the crucible onto a nickel roller with a rotation speed of 900 rpm, and pass cooling water through the nickel roller , the alloy solution is 1×10 5 After rapid cooling at the cooling rate of ℃ / s, it is thrown out along the tangent line of the nickel roll to form scale-like strips. The scale-like strips are ground to a particle diameter of less than 70 microns to obtain a master alloy. Slowly add 50 g of the master alloy into a three-neck flask filled with 500 g of 20 wt % sodium hydroxide aqueous solution, control its temperature at 80° C. and keep stirring at constant temperature for 1 hour. After stopping heating and stirring, decant the liquid and wash with distilled water at 80°C until the pH value is 7. The prepared catalyst is numbered Catalyst-3, and the composition o...

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Abstract

The invention relates to a method for preparing dimethylamino propylamine through hydrogenating dimethylamino propionitrile in the presence of nickel. The method comprises the following step: under the reaction condition thatdimethylamino propionitrile is hydrogenated to prepare dimethylamino propylamine in the presence of a catalyst, contacting dimethylamino propionitrile with hydrogen for reaction, wherein the catalyst contains at least one amorphous Ni-Al-Mo-M catalyst; by taking the weight of the catalyst as a reference, the weight ratio of Ni to Al to Mo to M is (5-500):(1-150):(1-150):1; and M is selected from one or more of transition metals in IB group, IIB group, IIIB group, IVB group, VIIB group, VIB group except for Mo and VIII group except for Ni. Compared with the prior art, the invention has the advantage that the selectivity of the dimethylamino propylamine prepared through hydrogenation by dimethylamino propionitrile is obviously increased.

Description

technical field [0001] The invention relates to a method for preparing dimethylaminopropylamine through hydrogenation of dimethylaminopropionitrile. Background technique [0002] Dimethylaminopropylamine (DMAPA for short) is an important intermediate in organic synthesis. It is mainly used to prepare dyes, ion exchange resins, epoxy resin curing agents, oils and cyanide-free galvanizing additives, fiber and leather treatment agents and fungicides, etc.; it can also be used to inhibit corrosion in the process of boiler water treatment, and is also a synthetic Intermediate component of gasoline and lubricating oil additives. Because the molecule of the product contains both primary and tertiary amino groups, it can be used as a curing agent for epoxy resin and has both functions of curing agent and accelerator. [0003] Industrially, dimethylaminopropylamine is mainly prepared by hydrogenation of dimethylaminopropionitrile, and the commonly used catalyst is Raney Ni or Raney...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/11C07C209/48B01J23/883B01J23/885B01J23/889
Inventor 张晓昕吴佳王宣孟祥堃
Owner CHINA PETROLEUM & CHEM CORP
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