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Alkaline molecular sieve supported catalyst and preparation method and application thereof

A catalyst and molecular sieve technology, applied in molecular sieve catalyst, catalyst activation/preparation, reductive alkylation preparation, etc., can solve the problems of high price, dependence on imports, high toxicity of adiponitrile, etc., to achieve easy operation and meet industrial application requirements , excellent selective effect

Active Publication Date: 2020-05-01
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] The raw material adiponitrile in the route of industrialized hydrogenation of adiponitrile to hexamethylenediamine is highly toxic and depends on imports and the price is high

Method used

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  • Alkaline molecular sieve supported catalyst and preparation method and application thereof
  • Alkaline molecular sieve supported catalyst and preparation method and application thereof
  • Alkaline molecular sieve supported catalyst and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-10

[0053] The preparation of embodiment 1-10 basic molecular sieve

[0054] Step 1): dissolving an alkali metal salt in water to obtain a precursor solution with a concentration of 0.2-0.6 mol / L, the alkali metal salt being selected from one of potassium nitrate, rubidium nitrate, and cesium nitrate;

[0055] Step 2): Weighing 30g molecular sieves, the molecular sieves are selected from one of NaX, NaY, KL, and NaBeta molecular sieves;

[0056] Step 3) According to the solid-to-liquid ratio of 10:1, use the alkali metal ion precursor solution in step 1) to carry out ion exchange on the molecular sieve weighed in step 2), exchange at 80°C for 4 hours, suction filter and wash 1. After drying, the obtained solid is roasted at 550° C. in a muffle furnace for 6 hours;

[0057] Step 4) Change the object of ion exchange in step 3) from the molecular sieve weighed in step 2) to the molecular sieve obtained after roasting, repeat step 3) twice to obtain a basic molecular sieve sample, an...

Embodiment 11-10

[0062] The preparation of the metal catalyst supported by the basic molecular sieve of embodiment 11-10

[0063] Dissolve a certain amount of metal salt solution in water, and set the volume to 12mL. Take 10g of basic molecular sieve and use the equal volume impregnation method to load metal elements on the basic molecular sieve, dry it in an oven at 100°C for 12h, and then place it in a muffler at 500°C. Roasting in the furnace for 4h. The types and qualities of carriers and metal salts are shown in Table 2.

[0064] Table 2 Preparation parameters of basic molecular sieve supported metal catalysts

[0065]

[0066]

[0067] Among them, in the catalyst nA@B, A represents the transition metal, B represents the basic molecular sieve, and n represents the mass loading of the transition metal.

Embodiment 25-38

[0068] The reaction performance evaluation of the metal catalyst supported by the basic molecular sieve of embodiment 25-38

[0069] Pack 2.0g of the above-mentioned catalyst in a stainless steel fixed-bed reactor with an inner diameter of 10m 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 for 4 hours. , wherein the reducing gas consists of H 2 / N 2 Composition by volume ratio 1 / 4.

[0070] 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, reaction 10h sampling analysis, re...

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Abstract

The invention discloses an alkaline molecular sieve supported catalyst and a preparation method and application thereof. The catalyst is an alkaline molecular sieve supported metal catalyst. The alkaline molecular sieve supported metal catalyst is adopted to catalyze reductive amination of adipic dialdehyde to prepare hexamethylenediamine, the use of a highly toxic raw material, namely adiponitrile is avoided, and a route is clean and environment-friendly; and since the catalyst is the metal catalyst supported by an alkaline molecular sieve, the generation of macromolecular amination productsis effectively inhibited by utilizing the shape-selective effect of the molecular sieve and the hydrogenation effect of metal, and the catalyst shows excellent selectivity in the reaction of preparinghexamethylenediamine by reductive amination of adipic dialdehyde. The preparation method provided by the invention is simple and convenient to operate, meets industrial application requirements and is convenient for large-scale industrial production.

Description

technical field [0001] The application relates to a catalyst supported by basic molecular sieves, a preparation method and application thereof, and 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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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/08B01J29/12B01J29/14B01J29/60B01J29/62B01J29/70B01J29/74B01J37/02B01J37/30C07C209/26C07C211/12
CPCB01J29/082B01J29/084B01J29/123B01J29/126B01J29/143B01J29/60B01J29/62B01J29/7007B01J29/7415B01J37/0207B01J37/30B01J2229/18C07C209/26C07C211/12
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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