Supported catalysts for the preparation of 1,2‑propylenediamine

A supported catalyst, propylenediamine technology, applied in the direction of physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, preparation of amino-substituted functional groups, etc., can solve side reactions, insufficient reactions, rapid, etc. Problems, to achieve the effect of convenient operation, beneficial to industrial production, and reduce production costs

Inactive Publication Date: 2017-06-16
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As a result, the reaction is not sufficient and rapid enough, resulting in more side reactions

Method used

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  • Supported catalysts for the preparation of 1,2‑propylenediamine
  • Supported catalysts for the preparation of 1,2‑propylenediamine

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Accurately weigh 1g SiO 2 Suspend it in 20 mL distilled water, then weigh 0.3196 g CuCl 2 2H 2 O, it was added to the suspension, and the mixture was sonicated for 30min so that the SiO 2 for uniform dispersion. Heat the mixed solution after ultrasonication at 100°C until the solution is evaporated to dryness, then transfer it to an incubator at 120°C for 2 hours, and finally transfer it to a muffle furnace for calcination at 400°C for 3 hours . The prepared catalyst CuO / SiO 2 for the next catalytic reaction. The content of CuO is 15% of the weight of the carrier. Add 5 mL of 1,2-dichloropropane, 0.5 g CuO / SiO to the reaction kettle 2 , 100mL ammonia water. The reaction kettle was put into a homogeneous reactor and rotated at a constant speed, and the temperature was raised to 160° C. for 3 hours. The temperature was lowered to room temperature, unreacted ammonia gas was removed, and gas chromatography was used to detect that the yield of 1,2-propanediamine was...

Embodiment 2

[0022] Accurately weigh 1g TiO 2 Suspend it in 20 mL distilled water, then weigh 0.3196 g CuCl 2 2H 2 O, it was added to the suspension, and the mixture was sonicated for 30min so that the TiO 2 for uniform dispersion. Heat the mixed solution after ultrasonication at 100°C until the solution is evaporated to dryness, then transfer it to an incubator at 120°C for 2 hours, and finally transfer it to a muffle furnace for calcination at 400°C for 3 hours . The prepared catalyst CuO / TiO 2 for the next catalytic reaction. The content of CuO is 15% of the weight of the carrier. Add 5 mL of 1,2-dichloropropane, 0.5 g CuO / TiO to the reaction kettle 2 , 100mL ammonia water. The reaction kettle was put into a homogeneous reactor and rotated at a constant speed, and the temperature was raised to 160° C. for 3 hours. The temperature was lowered to room temperature, unreacted ammonia gas was removed, and gas chromatography was used to detect that the yield of 1,2-propanediamine was...

Embodiment 3

[0024] Accurately weigh 1g Al 2 o 3 Suspend it in 20 mL distilled water, then weigh 0.3196 g CuCl 2 2H 2 O, it was added to the suspension, and the mixture was sonicated for 30 minutes to remove Al 2 o 3 for uniform dispersion. Heat the mixed solution after ultrasonication at 100°C until the solution is evaporated to dryness, then transfer it to an incubator at 120°C for 2 hours, and finally transfer it to a muffle furnace for calcination at 400°C for 3 hours . The prepared catalyst CuO / Al 2 o 3 for the next catalytic reaction. The content of CuO is 15% of the weight of the carrier. Add 5 mL of 1,2-dichloropropane, 0.5 g CuO / Al to the reaction kettle 2 o 3 , 100mL ammonia water. The reaction kettle was put into a homogeneous reactor and rotated at a constant speed, and the temperature was raised to 160° C. for 3 hours. Cool down to room temperature, remove unreacted ammonia gas, and detect by gas chromatography, the yield of 1,2-propanediamine is 68.39%.

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Abstract

The invention discloses a supported catalyst for preparation of 1, 2-propane diamine through catalysis. The 1, 2-propane diamine is prepared by a method comprising main synthesis steps of adding 1, 2-propylene dichloride, ammonia water, and the supported catalyst into a reaction kettle; rotating the reaction kettle in a homogeneous phase reactor at constant speed; carrying out amination at reaction temperature of 140 DEG C-170 DEG C so as to prepare the 1, 2-propane diamine, wherein the yield of the 1, 2-propane diamine is more than 65%; and after reaction, firstly removing unreacted ammonia gas, and then distilling at normal pressure so as to obtain a 1, 2-propane diamine aqueous solution. The supported catalyst has the advantages that the yield of the 1, 2-propane diamine prepared by catalysis of the supported catalyst is relatively high; the byproduct 1, 2-propylene dichloride generated in production of chloropropene is taken as the raw material, so that the production cost is greatly lowered; the reaction process is simple, the operation is convenient; the method is safe and environment-friendly and is beneficial to industrial production.

Description

[0001] Technical field: [0002] The invention belongs to the technical field of chemical synthesis, relates to the preparation of a class of supported catalysts, and uses the catalysts to catalyze the synthesis of 1,2-propanediamine. [0003] technical background: [0004] 1,2-Propylenediamine is an important organic chemical intermediate and raw material. Its applications include the production of beneficiation agents, metal deactivators, and aviation resin curing agents; in the production of rubber vulcanization accelerators Also has a certain use value; at the same time, 1,2-propylenediamine is also used in dyes, electroplating and reagents for analyzing metals (in the determination of elements such as mercury, copper and silver); for the production of 1,2-propylenediaminetetraacetic acid ; Use in pharmaceuticals, including as an intermediate in the production of propylene imine anticancer drugs. [0005] At present, with the gradual expansion of the scope of application o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/11C07C209/08B01J23/72
Inventor 孙国新牟晓磊崔玉聂永夏光明
Owner UNIV OF JINAN
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