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Catalyst for preparing hexamethylenediamine as well as preparation method and application of catalyst

A catalyst, hexamethylenediamine technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of dependence on imports, high toxicity of adiponitrile, high price, etc., to achieve a clean route and improve selection performance and catalyst stability

Active Publication Date: 2020-04-24
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 as well as preparation method and application of catalyst
  • Catalyst for preparing hexamethylenediamine as well as preparation method and application of catalyst
  • Catalyst for preparing hexamethylenediamine as well as preparation method and application of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] Example 1 Preparation of metal@molecular sieve catalyst

[0075] (1) Add 0.03gRuCl 3 ·3H 2 O is dissolved in water, dilute to 12mL, and take 10g of HBeta molecular sieve (SiO 2 / Al 2 O 3 Molar ratio=800, SiO 2 The mass content is 98.9%), and the RuCl 3 ·3H 2 O is loaded on HBeta and placed in an oven at 100℃ to dry for 12h, H 2 Reduce at 500℃ for 4h in the atmosphere to obtain metal-loaded Ru / HBeta molecular sieve;

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

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

[0078] (4) Roasting Ru@ZSM-5 molecular sieve at 500℃ for 4h to remove template TPAOH,...

Embodiment 2-10

[0080] Example 2-10 Preparation of metal@molecular sieve catalyst

[0081] M@ZSM-5 was prepared using the same steps as in Example 1, 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. ICP-OES is used to test the mass content of metals in M@ZSM-5.

[0082] Table 1 Specific synthesis conditions of each embodiment

[0083]

[0084]

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

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

[0087] figure 1 This is the XRD spectrum of the HBeta molecular sieve used in Example 1; the catalyst obtained in Examples 1 to 10 is ZSM-5 molecular sieve, a typical representative such as figure 2 The XRD spectrum of the catalyst in Example 1. The...

Embodiment 11-20

[0088] Example 11-20 Evaluation of reaction performance of metal@molecular sieve catalyst

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

[0090] After the reduction, the reactor temperature was reduced to 130°C, the reaction pressure was increased to 6.0Mpa, and H was respectively introduced into the reactor 2 , Liquid ammonia and adipaldehyde undergo reductive amination reaction, in which liquid ammonia and adipaldehyde are injected into the reactor through a high-pressure micro-feed pump respectively, and the mass space velocity of adipaldehyde is 1.0h -1 , H 2 :NH 3 : The molar ratio of adipaldehyde = 15:30:1, and the reaction was sampled for 10 hour...

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PUM

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Abstract

The invention discloses a catalyst for preparing hexamethylenediamine as well as a preparation method and application of the catalyst, wherein the catalyst for preparing hexamethylenediamine is an HZSM-5 molecular sieve packaged noble metal catalyst and is used as a catalyst to catalyze adipic dialdehyde to prepare hexamethylenediamine through reductive amination, the use of a highly toxic raw material adiponitrile is avoided, and the route is clean and environment-friendly; according to the catalyst, metal is encapsulated in molecular sieve pores, and the selectivity of a target product and the stability of the catalyst are effectively improved by utilizing the confinement effect of molecular sieve.

Description

Technical field [0001] The application relates to a ZSM-5 molecular sieve encapsulated metal catalyst for preparing hexamethylene diamine, and a preparation method and application thereof, belonging to the field of chemistry and chemical engineering. Background technique [0002] Nylon 66 can be used for injection molding, extrusion, blow molding, spraying, casting molding, machining, welding, and bonding. Nylon 66 can be made by polycondensation of hexamethylene diamine and adipic acid. About 90% of the hexamethylene diamine produced in the world every year is used in the production of nylon 66. [0003] Reaction with sebacic acid can produce polyhexamethylene sebacamide (PA610) products, 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 generated through photochemical reaction. HDI is a new type o...

Claims

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Application Information

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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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