Method for preparing 1, 6-hexamethylenediamine by ammoniating hexamethyleneimine

A technology of cyclohexamethyleneimine and hexamethylenediamine, which is applied in the field of ammoniation of cyclohexylimine to prepare 1,6-hexamethylenediamine, which can solve the problems of inability to realize continuous production, poor stability, and low catalyst activity.

Active Publication Date: 2021-06-04
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] As can be seen from the above review, the preparation of 1,6-hexanediamine by the amination of cyclohexyl imine by the existing technology has

Method used

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  • Method for preparing 1, 6-hexamethylenediamine by ammoniating hexamethyleneimine

Examples

Experimental program
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Effect test

Embodiment 1

[0080] Preparation and Application of Ni5-Ru3-Os1 / Activated Carbon Catalyst

[0081] Take 9.1 grams of 20-40 mesh activated carbon and treat it at 150°C for 1 hour under an ammonia atmosphere. Configuration 20ml contains 2.477 grams of Ni (NO 3 ) 2 ·6H 2 O, 0.776 g RuCl 3 ·3H 2 O, 0.184 g OsCl 3 ·3H 2 O aqueous solution, impregnate the above-mentioned activated carbon carrier with this aqueous solution, dry it naturally, dry at 120°C for 4h, and roast at 500°C for 6h in an argon atmosphere. Before the reaction, the catalyst is reduced and activated in a fixed bed device. The activation conditions are: 0.1MPa, temperature 450°C, hydrogen volume space velocity 500h -1 , Time 4h. After the reduction process, the temperature of the reactor is adjusted to 160°C and the pressure is 8MPa. After the system is stable, the molar ratio of cycloheximide and ammonia is mixed at a ratio of 1:10. After preheating at 100°C, it is pumped into the fixed bed reactor. The catalytic react...

Embodiment 2

[0083] Ni5-Re2-W0.5 / Al 2 o 3 Catalyst preparation and application

[0084] Take 9.25 grams of 20-40 mesh Al 2 o 3 , treated at 200°C for 2h under an ammonia atmosphere. Configuration 20ml contains 2.477 grams of Ni (NO 3 ) 2 ·6H 2 O, 0.288 g NH 4 ReO 4 , 0.077 g (NH 4 ) 2 WO 4 Aqueous solution, impregnating the above Al with this aqueous solution 2 o 3 The carrier was air-dried, dried at 120°C for 4h, and calcined in a muffle furnace at 450°C for 6h. Before the reaction, the catalyst is subjected to reduction and activation treatment in a fixed bed device, the activation conditions are: 0.1MPa, temperature 390°C, hydrogen volume space velocity 500h -1, time 5h. After the reduction process, the temperature of the reactor is adjusted to 150°C and the pressure is 8MPa. After the system is stable, the molar ratio of cyclohexylimine and ammonia is 1:5, and it is pumped into the fixed bed reactor after preheating at 100°C. The catalytic reaction is carried out in, wh...

Embodiment 3

[0086] Preparation and Application of Fe8-Re3-Ir1.5 / Activated Carbon Catalyst

[0087] Take 8.75 g of 60-80 mesh activated carbon and treat it at 150°C for 2 hours under an ammonia atmosphere. Disperse activated carbon in water to form a suspension, and stir at a medium speed at a constant temperature of 50°C. Configuration contains 3.465 g Fe(NO 3 ) 3 , 0.432 g NH 4 ReO 4 , 0.275 g IrCl 3 ·3H 2 Precursor fluid of O. The precipitating agent used is 4mol / L KOH solution. Add the precursor liquid and the precipitating agent dropwise to the above suspension at a rate of 1ml / min at the same time, keep the pH value at 9 until the precipitation is complete, wash the precipitate with deionized water until neutral, filter, dry in the air, and dry at 120°C 4h, and baked at 500°C for 4h in an argon atmosphere. Before the reaction, the catalyst is subjected to reduction and activation treatment in a fixed bed device, the activation conditions are: 0.1MPa, temperature 400°C, hydro...

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Abstract

The invention relates to a method for preparing 1, 6-hexamethylenediamine by ammoniating hexamethyleneimine. The catalyst in the method comprises an active component, an auxiliary agent and a carrier, the active component is one or a combination of transition metals Ni, Fe, Ru and Re, the auxiliary agent is one or a combination of elements W, B, Ir, Pt, Os, Co, Cu, Rh and Mo, and the carrier is one or a combination of Al2O3, activated carbon, a molecular sieve, SiO2 and Al2O3-SiO2 which are subjected to ammoniation treatment. The weight of the active component in the catalyst accounts for 1-45% of the weight of the catalyst, and the weight of the auxiliary agent accounts for 0.05-15% of the weight of the catalyst. The catalyst is used for preparing 1, 6-hexamethylenediamine by ammoniating hexamethyleneimine in a hydrogen atmosphere, has the advantages of high activity, high target product yield, good stability, good economical efficiency and the like, and has a wide application prospect.

Description

technical field [0001] The present invention relates to a method for preparing 1,6-hexamethylenediamine through ammoniation of cyclohexyl imine, and in more detail, relates to a method for catalyzing the ammoniation reaction of cyclohexyl imine and ammonia to generate 1,6- Hexamethylenediamine catalyst. Background technique [0002] As an important class of organic amine products, 1,6-hexamethylenediamine is widely used in the production of polyhexamethylene adipamide (nylon 66), hexamethylene isocyanate, synthetic resins, organic crosslinking agents, etc. . With the rapid development of the synthetic material industry at home and abroad, the demand for 1,6-hexanediamine is increasing, so the research and development of new catalysts for the synthesis of 1,6-hexanediamine has broad market prospects. [0003] Common 1,6-hexanediamine production processes mainly include: 1,6-adiponitrile hydrogenation method, 1,6-hexanediol or 6-amino-1-hexanol amination method, caprolactam ...

Claims

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Application Information

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IPC IPC(8): C07C209/52C07C211/12B01J23/656B01J23/883B01J23/889B01J23/89
CPCC07C209/52B01J23/892B01J23/8896B01J23/6567B01J23/8986B01J23/8898B01J23/883B01J23/8906C07C211/12
Inventor 马雷丁云杰严丽程显波
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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