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Catalyst for preparing hexamethylenediamine and its preparation method and application

A catalyst, hexamethylenediamine technology, used in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of high toxicity of adiponitrile, dependence on imports, high price, etc. Stability, effect of route cleaning

Active Publication Date: 2021-09-03
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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  • Catalyst for preparing hexamethylenediamine and its preparation method and application
  • Catalyst for preparing hexamethylenediamine and its preparation method and application
  • Catalyst for preparing hexamethylenediamine and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] The preparation of embodiment 1 metal@molecular sieve catalyst

[0075] (1) 0.03gRuCl 3 ·3H 2 O was dissolved in water, and the volume was adjusted to 12mL, and 10g of HBeta molecular sieve (SiO 2 / Al 2 o 3 Molar ratio = 800, SiO 2 The mass content is 98.9%), the RuCl 3 ·3H 2 O was loaded on HBeta, dried in an oven at 100°C for 12 h, and H 2 Reduction at 500°C for 4 hours in the atmosphere to obtain metal-loaded Ru / HBeta molecular sieves;

[0076] (2) Place the metal-loaded Ru / HBeta molecular sieve in 15 mL of TPAOH aqueous solution with a mass fraction of 35.0%, immerse at room temperature for 2 hours, and dry in an oven at 100° C. for 12 hours to obtain the / HBeta molecular sieve with TPAOH adsorbed in the pores;

[0077] (3) Mix the / HBeta molecular sieve with TPAOH adsorbed in the channel with 0.6g sodium hydroxide and 20mL deionized water, and crystallize at 90°C for 6 hours to obtain Ru@ZSM-5 molecular sieve;

[0078] (4) Roast Ru@ZSM-5 molecular sieve at...

Embodiment 2-10

[0080] The preparation of embodiment 2-10 metal@molecular sieve catalyst

[0081] The same steps in Example 1 were used to prepare M@ZSM-5, and the metal type and loading amount were adjusted by changing the type and concentration of the metal salt solution. The specific synthesis conditions are listed in Table 1. The mass content of metals in M@ZSM-5 was tested by ICP-OES.

[0082] The specific synthetic conditions of each embodiment of table 1

[0083]

[0084]

[0085] In the table, in the catalyst nA@ZSM-5, A represents the noble metal, ZSM-5 is the abbreviation of HZSM-5, n represents the mass loading of the noble metal in M / HBeta, W(%) represents the amount of metal in M@ZSM-5 mass content.

[0086] Embodiment 1-10 Characterization of metal@molecular sieve catalyst

[0087] figure 1 It is the XRD spectrogram of the HBeta molecular sieve used in Example 1; the catalyst obtained in Examples 1 to 10 is a ZSM-5 molecular sieve, and a typical representative is as ...

Embodiment 11-20

[0088] Reaction Performance Evaluation of Embodiment 11-20 Metal @ Molecular Sieve Catalyst

[0089] Pack 2.0g of the above-mentioned catalyst in a stainless steel fixed-bed reactor with an inner diameter of 10mm and a length of 300mm. Both ends of the catalyst are filled with quartz sand. First, a reducing gas is introduced at a flow rate of 30mL / min, and the catalyst is reduced at 400°C. 4h, wherein the reducing gas is composed of H 2 / N 2 Composition by volume ratio 1 / 4.

[0090] After the reduction, the temperature of the reactor was lowered to 130°C, the reaction pressure was raised to 6.0Mpa, and H 2 , liquid ammonia and adipaldehyde for reductive amination reaction, wherein liquid ammonia and adipaldehyde are respectively injected into the reactor through a high-pressure micro-feed pump, and the mass space velocity of adipaldehyde is 1.0h -1 , H 2 :NH 3 : the mol ratio=15:30:1 of adipaldehyde, react 10h sampling analysis, and reaction result is listed in table 2. ...

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Abstract

The application discloses a catalyst for preparing hexamethylenediamine and its preparation method and application. The catalyst for preparing hexamethylenediamine is a noble metal catalyst encapsulated by HZSM-5 molecular sieve, which is used as a catalyst to catalyze the reduction of adipaldehyde The preparation of hexamethylenediamine by amination avoids the use of adiponitrile, a highly toxic raw material, and the route is clean and environmentally friendly; the catalyst encapsulates the metal in the pores of the molecular sieve, and effectively improves the selectivity of the target product and the stability of the catalyst by using the confinement effect of the molecular sieve .

Description

technical field [0001] The application relates to a ZSM-5 molecular sieve-encapsulated metal catalyst used for preparing hexamethylenediamine, its preparation method and application, and belongs to the field of chemistry and chemical engineering. Background technique [0002] Nylon 66 can be used for injection molding, extrusion, blow molding, spraying, casting, machining, welding, and bonding. Nylon 66 can be produced by polycondensation reaction of hexamethylenediamine and adipic acid. About 90% of hexamethylenediamine produced in the world is used in the production of nylon 66. [0003] 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 photochemical reaction. HDI is a new type of polyurethane plastic,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/44C07C209/26C07C211/12
CPCB01J29/44B01J2229/186C07C209/26C07C211/12
Inventor 许磊袁扬扬张晓敏赵晓炜陆标史鑫
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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