Method for preparing hexamethylenediamine from adipic dialdehyde based on Ni-based catalyst

A catalyst, adipaldehyde technology, which is applied in reductive alkylation preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of dependence on imports, high price, high toxicity of adiponitrile, etc., and achieves low cost , easy to operate, reduce the loss of metal ions

Inactive Publication Date: 2020-04-28
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

[0005] Judging from the existing literature and technology, the raw material adiponitrile in the route of industrialized hydrogenation of adiponitrile to hexamethylenediamine is highly toxic, and it depends on imports and the price is high.

Method used

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  • Method for preparing hexamethylenediamine from adipic dialdehyde based on Ni-based catalyst
  • Method for preparing hexamethylenediamine from adipic dialdehyde based on Ni-based catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Embodiment 1 prepares NiMgAl-01 catalyst with hydrotalcite as precursor, (Ni 2+ +Mg 2+ ):Al 3+ The ratio is 3:1, Ni 2+ : Mg 2+The ratio is 0.1.

[0056] 9.52gNi(NO 3 ) 2 ·6H 2 O, 46.89gAl(NO 3 ) 3 9H 2 O and 83.92gMg(NO 3 ) 2 ·6H 2 O is completely dissolved in 500ml of water to obtain mixed solution I; weigh 26.5gNa 2 CO 3 and 70g of NaOH were completely dissolved in 1L of water to obtain the mixed solution II; the two mixed solutions were slowly added dropwise to 200mL of water at the same time, vigorously stirred at a speed of 600r / min, and the pH was maintained at 10. After the addition was completed, the obtained colloidal suspension Transfer to an oven, age at 65°C for 72h, wash with distilled water until neutral, and dry to obtain Ni-based hydrotalcite, and further roast the obtained Ni-based hydrotalcite precursor at 500°C for 4h to obtain highly dispersed Ni base catalyst.

Embodiment 2

[0057] Embodiment 2 prepares NiMgAl-02 catalyst with hydrotalcite as precursor, (Ni 2+ +Mg 2+ ):Al 3+ The ratio is 3:1, Ni 2+ : Mg 2+ The ratio is 1.0.

[0058] 52.34gNi(NO 3 ) 2 ·6H 2 O, 46.89gAl(NO 3 ) 3 9H 2 O and 46.15gMg(NO 3 ) 2 ·6H 2 O is completely dissolved in 500ml of water to obtain mixed solution I; weigh 26.5gNa 2 CO 3 and 70g of NaOH were completely dissolved in 1L of water to obtain the mixed solution II; the two mixed solutions were slowly added dropwise to 200mL of water at the same time, vigorously stirred at a speed of 600r / min, and the pH was maintained at 10. After the addition was completed, the obtained colloidal suspension Transfer to an oven, age at 65°C for 72h, wash with distilled water until neutral, and dry to obtain Ni-based hydrotalcite, and further roast the obtained Ni-based hydrotalcite precursor at 500°C for 4h to obtain highly dispersed Ni base catalyst.

Embodiment 3

[0059] Embodiment 3 prepares NiMgAl-03 catalyst with hydrotalcite as precursor, (Ni 2+ +Mg 2+ ):Al 3+ The ratio is 3:1, Ni 2+ : Mg 2+ The ratio is 3.0

[0060] 78.52gNi(NO 3 ) 2 ·6H 2 O, 46.89gAl(NO 3 ) 3 9H 2 O and 23.07gMg(NO 3 ) 2 ·6H 2 O is completely dissolved in 500ml of water to obtain mixed solution I; weigh 26.5gNa 2 CO 3 and 70g of NaOH were completely dissolved in 1L of water to obtain the mixed solution II; the two mixed solutions were slowly added dropwise to 200mL of water at the same time, vigorously stirred at a speed of 600r / min, and the pH was maintained at 10. After the addition was completed, the obtained colloidal suspension Transfer to an oven, age at 65°C for 72h, wash with distilled water until neutral, and dry to obtain Ni-based hydrotalcite, and further roast the obtained Ni-based hydrotalcite precursor at 500°C for 4h to obtain highly dispersed Ni base catalyst.

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Abstract

The invention discloses a method for preparing hexamethylenediamine from adipic dialdehyde based on a Ni-based catalyst. The raw material containing adipic dialdehyde reacts in the presence of ammoniagas, hydrogen and the Ni-based catalyst to generate hexamethylenediamine, wherein the Ni-based catalyst is prepared from hydrotalcite containing Ni < 2 + >. According to the method, hexamethylenediamine is prepared from catalytic adipic dialdehyde prepared from hydrotalcite containing Ni < 2 + > through reductive amination so that the use of a highly toxic raw material adiponitrile is avoided andthe route is clean and environment-friendly.

Description

technical field [0001] The application relates to a method for preparing hexamethylenediamine from adipaldehyde based on a Ni-based catalyst, which belongs to the field of chemistry and chemical engineering. Background technique [0002] Hexamethylenediamine is an important organic chemical raw material, which can be polycondensed with adipic acid to produce polyhexamethylene adipamide, also known as polyamide 66 (PA66) or nylon 66. In recent years, the application fields of hexamethylenediamine have expanded rapidly. With the continuous development of my country's automobile industry, my country has gradually become the world's largest automobile manufacturing country. Under the trend of lightweight, environmental protection and energy saving, the demand for nylon 66 in the automobile industry is also showing a rising trend. Nylon 66 is facing a relatively large Big gap between supply and demand. [0003] The production of hexamethylenediamine is mainly monopolized by some...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/26C07C211/12B01J23/755B01J23/78B01J23/80B01J35/00
CPCB01J23/78B01J23/80B01J35/0066B01J35/0073C07C209/26C07C211/12
Inventor 袁扬扬许磊赵晓炜李沛东陆标
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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