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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 one or more disadvantages such as low catalyst activity, low product yield, inability to realize continuous production, and poor stability. question

Method used

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