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Supported nano nickel-based catalyst as well as preparation method and application thereof

A nano-nickel and supported technology, which is applied in the field of supported nano-nickel-based catalysts and their preparation, can solve the problems of easy fires caused by the operation of Raney nickel catalysts, high production costs of chloroquine side chain compounds, and loss of catalyst production. The effect of large-scale industrial production, simplified production operation process and improved production efficiency

Pending Publication Date: 2020-08-04
LANZHOU 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

The Raney nickel catalyst is made by dissolving aluminum in nickel-aluminum alloy under strong alkali, which produces a large amount of aluminum-containing waste alkali and causes serious environmental pollution.
Although the Raney nickel catalyst achieves a yield of more than 88% in the reductive amination reaction of 5-diethylamino-2-pentanone, there is loss and deactivation of the catalyst during the production process, and the production efficiency of the batch reaction process is low , high energy consumption, resulting in high production costs of the target chloroquine side chain compound
In addition, improper operation of Raney nickel catalysts can easily cause fires, and the use of liquid ammonia also poses a major safety hazard

Method used

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  • Supported nano nickel-based catalyst as well as preparation method and application thereof
  • Supported nano nickel-based catalyst as well as preparation method and application thereof
  • Supported nano nickel-based catalyst as well as preparation method and application thereof

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preparation example Construction

[0031] Another aspect of the embodiments of the present invention also provides the aforementioned method for preparing the supported nano-nickel-based catalyst, which includes: preparing the supported nano-nickel-based catalyst by co-precipitation and / or deposition-precipitation.

[0032] In some more specific embodiments, the preparation method may specifically include: mixing the mixed metal salt solution containing the main active component and the auxiliary agent, the lye and the metal salt solution of the carrier, the carrier oxide powder solution, the carrier Any one of the colloidal particle solutions is mixed, and then subjected to precipitation, aging, roasting and reduction treatment to obtain the supported nano-nickel-based catalyst.

[0033] Further, the lye is any one or a combination of two or more of sodium hydroxide solution, potassium hydroxide solution, sodium carbonate solution, and potassium carbonate solution, and is not limited thereto.

[0034] Further,...

Embodiment 1

[0059] Embodiment 1: Preparation and characterization of supported nanometer nickel-based catalyst

[0060] The supported nano-nickel-based catalyst of the present invention is prepared by co-precipitation method, and the active metal nickel and the metal salt of the auxiliary agent are weighed in proportion at room temperature, and deionized water is added to prepare a catalyst with a total concentration of the active metal and the auxiliary agent salt of 0.1mol / L. Solution A; prepare NaOH concentration of 4mol / L, Na 2 CO 3 Concentration is the mixed alkali B of 1mol / L; Add the metal salt of carrier or commercially available oxide powder or colloid particle in proportion in reaction tank, add deionized water (addition amount is carrier metal salt or commercially available oxide powder or colloid 10 times the size of the particles) fully stir and mix evenly, then add salt solution A and alkali solution B dropwise to the reaction tank at the same time under rapid stirring, kee...

Embodiment 2

[0065] The preparation process and composition of the catalyst were the same as those of Catalyst 1, except that the concentration of metal salt solution A was 0.5moL / L, the catalyst was aged at 100°C for 2h, washed and dried, then calcined at 800°C for 2h, and reduced and activated at 750°C for 2h to obtain Catalyst 8. XRD characterization results show that the grain size of the reduction-activated catalyst is 6.2nm;

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Abstract

The invention discloses a supported nano nickel-based catalyst as well as a preparation method and an application thereof. The catalyst comprises a carrier, and a main active component and an auxiliary agent which are loaded on the carrier, wherein the main active component comprises Ni; wherein the auxiliary agent comprises any one or a combination of more than two of Fe, Co, Cu, Zn, Mn, Ca, La,Y, Ce and Ga; wherein the carrier comprises any one of Al2O3, ZrO2, SiO2 and MgO or a combination of more than two of Al2O3, ZrO2, SiO2 and MgO. According to the invention, 5-diethylamino-2-pentanoneobtained through conversion of 5-chloro-2-pentanone is used as a raw material, a continuous reductive amination reaction is carried out under the action of a supported nano Ni-based catalyst and ammonia water, and a target product with the purity larger than 99% is obtained; the catalyst used in the method is low in cost, high in production efficiency, good in stability, simple to operate, good insafety and convenient for industrial production.

Description

technical field [0001] The invention belongs to the technical field of synthesis of pharmaceutical intermediates, specifically relates to a supported nano-nickel-based catalyst and its preparation method and application, and more specifically relates to the continuous production of the key intermediate N,N-diethyl-1,4- Applications in pentamethylenediamine. Background technique [0002] Chloroquine phosphate is a white crystalline powder, odorless and bitter. Gradient color when exposed to light; aqueous solution shows acidic reaction, easily soluble in water, almost insoluble in ethanol, chloroform, ether. Its chemical name is N', N'-diethyl-N4-(7-chloro-4-quinolyl)-1,4-pentanediamine diphosphate, and its molecular formula is: C 18 h 26 ClN 3 2H 3 PO 4 , the molecular weight is 515.87, and its structural formula is as follows: [0003] [0004] It is used to treat malaria such as chloroquine-sensitive Plasmodium falciparum and Plasmodium vivax, and it can also be ...

Claims

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Application Information

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IPC IPC(8): B01J23/755B01J23/83B01J23/80B01J23/889B82Y30/00C07C209/26C07C211/09
CPCB01J23/755B01J23/80B01J23/83B01J23/889B82Y30/00C07C209/26C07C211/09
Inventor 黄志威李雪梅
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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