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Method for preparing hexamethylenediamine

A preparation process, the technology of hexamethylenediamine, applied in the direction of reductive alkylation preparation, metal/metal oxide/metal hydroxide catalyst, organic chemistry, etc., can solve the problem of high toxicity of adiponitrile, dependence on imports, high price, etc. problems, achieve the effects of reducing the occurrence of side reactions, low cost, and convenient operation

Inactive Publication Date: 2020-05-08
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

[0006] 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
  • Method for preparing hexamethylenediamine
  • Method for preparing hexamethylenediamine

Examples

Experimental program
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Effect test

Embodiment 1

[0049] 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.

[0050] 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

[0051] 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.

[0052] 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

[0053] 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

[0054] 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 by using a fixed bed reactor, and the method comprises the following steps: introducing raw materials containing adipic dialdehyde,ammonia gas and hydrogen into a reactor loaded with a catalyst, and carrying out contact reaction to generate the hexamethylenediamine; wherein the Ni-based catalyst is prepared from hydrotalcite containing Ni < 2 + >. According to the method, the Ni-based hydrotalcite catalyst loaded with an alkali metal is adopted to catalyze the adipic dialdehyde to prepare the hexamethylenediamine through reductive amination, so that the use of highly toxic raw material adiponitrile is avoided, and the 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. Nylon 66 can be used for injection molding, extrusion, blow molding, spraying, casting, machining, welding, and bonding. About 90% of hexamethylenediamine produced in the world is used in the production of nylon 66. React with sebacic acid to produce polyhexamethylene sebacamide (PA610), also known as polyamide 610 or nylon 610. Nylon 610 can be made into various nylon resins, nylon fibers and engineering plastic products, and is a rare intermediate in synthetic materials. HDI (1,6-hexamethylene diisocyanate) can be produced through photochemi...

Claims

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Application Information

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IPC IPC(8): C07C209/26C07C211/12B01J23/78B01J23/80B01J23/755
CPCB01J23/755B01J23/78B01J23/80C07C209/26C07C211/12
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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