Preparation method of Ni-based catalyst with adjustable selectivity/non-selectivity

A non-selective, catalytic technology, applied in the new field of catalysis, can solve the problems such as the inability to directly realize the selective and adjustable catalytic process, and achieve the effect of large-scale industrial production, simple technical principle, and easy preparation

Active Publication Date: 2017-01-11
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, based on the existing catalyst preparation technology and methods, people cannot directly realize the catalytic process with adjustable selectivity, and there are no relevant technical reports in domestic and foreign literature and patents, which forces people to develop new technologies and methods for catalyst preparation.

Method used

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  • Preparation method of Ni-based catalyst with adjustable selectivity/non-selectivity
  • Preparation method of Ni-based catalyst with adjustable selectivity/non-selectivity
  • Preparation method of Ni-based catalyst with adjustable selectivity/non-selectivity

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Dissolve the substrate p-nitroaniline (0.5mmol) and the active component precursor nickel nitrate (0.25mmol) in dimethyl sulfoxide (10mL), after ultrasonic dispersion and compounding for 25 minutes, add the functional monomer 7-octyl Acrylic acid (1.0mmol), cross-linking agent N, N methylenebisacrylamide (3.5mmol) and initiator azobisisobutyronitrile (0.1g), then nitrogen deoxygenation into the solution for 8 minutes, sealed and placed Polymerization was initiated by irradiation under ultraviolet light (24 hours) to form a catalyst precursor. The Ni ions in the catalyst precursor were reduced by an excessive amount of sodium borohydride (2.5mmol), and the obtained product was washed with water repeatedly after the imprinted p-nitroaniline was eluted with a mixed solution of ethanol (90vol-%)-acetic acid (10vol-%), and vacuum Drying to obtain a Ni-based catalyst with adjustable selectivity (for its technical principle, see figure 1 ; labeled "MIP-Ni-NA-L", where MIP is ...

Embodiment 2

[0041] Operated with Example 1, the long-chain functional monomer was changed from 7-octenoic acid to 6-heptenoic acid (1.0mmol), and the others were completely operated with Example 1 to obtain a Ni base with a phase transition point of about 39°C. Catalyst MIP-Ni-NA-L. Under the same catalytic test conditions as in Example 1, select 35 and 45°C higher and lower than the phase transition point for comparative measurement, the results are shown in Figure 8 . At 35°C, the prepared MIP-Ni-NA-L catalyst showed selective catalytic effect on the specific substrate p-nitroaniline; in contrast, at 45°C, MIP-Ni-NA -L shows no selectivity for the specific substrate p-nitroaniline and its analog m-nitroaniline. The prepared MIP-Ni-NA-L catalyst also exhibits the characteristics of "selective / non-selective" tunable catalysis.

Embodiment 3

[0043] The operation was the same as in Example 1, except that the specific substrate was changed to o-nitroaniline, and the other preparations were exactly the same as in Example 1 to obtain a Ni-based catalyst MIP-Ni-NA-L with a phase transition point of about 37°C. Under the same catalytic test conditions as in Example 1, the catalytic test substrate is changed to the specific substrate o-nitroaniline and analog m-nitroaniline, and the temperature is selected to be higher than and lower than the phase transition point at 25 and 40°C. For comparison, the results can be seen in Figure 9 . At 25 °C, the prepared MIP-Ni-NA-L catalyst exhibited selective catalytic effects on the specific substrate o-nitroaniline; in contrast, at 40 °C, MIP-Ni-NA -L shows no selectivity for the specific substrate o-nitroaniline and its analog m-nitroaniline. The prepared MIP-Ni-NA-L catalyst also exhibits the characteristics of "selective / non-selective" tunable catalysis.

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Abstract

The invention provides a preparation method of a Ni-based catalyst with adjustable selectivity / non-selectivity. The functional monomer adopted in the preparation method is a functional monomer which contains long molecular chain segments and is used for constructing a molecular chain segment mobility mechanism. According to the method, a substrate and an active component precursor are dissolved in dimethyl sulfoxide, the functional monomer, a cross-linking agent and an initiator are added after ultrasonic dispersion and matching, then nitrogen is introduced into the solution for deoxygenation, the solution is sealed and then put under an ultraviolet lamp for illumination to initiate polymerization, and a catalyst precursor is formed; Ni ions in the catalyst precursor is reduced by sodium borohydride, the obtained product is cleaned repeatedly with water after the printed substrate of the product is eluted with ethyl alcohol and acetic acid, vacuum drying is carried out, and the Ni-based catalyst with adjustable selectivity / non-selectivity is obtained and can be used for fractional reduction of a nitryl isomer and preparation of o-phenylenediamine. The preparation method has the advantages that the technical principle is simple, raw materials are easy to obtain, operation is convenient, and preparation is easy.

Description

technical field [0001] The invention belongs to the field of new catalytic technology, and in particular relates to a preparation method of Ni-based catalyst with adjustable "selectivity / non-selectivity". Background technique [0002] Catalysis is the cornerstone of the modern chemical industry. Realizing highly selective and specific catalysis is a major scientific and technological problem that the industry urgently needs to solve. The emergence of highly selective catalyst preparation methods based on molecular recognition, imprinted polymers as carriers, and metal nanoparticles as active components has created conditions for the realization of this goal. The reason is that this preparation method takes into account both the molecular recognition ability of the carrier material and the catalytic ability of the metal-based catalyst, thus paving the way for the realization of high selectivity and specific catalysis. [0003] It is known that the preparation of the above-me...

Claims

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Application Information

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IPC IPC(8): B01J31/06C07C209/36C07C211/51
CPCB01J31/067B01J2231/64C07C209/325C07C211/51
Inventor 李松军王姣袁新华朱脉勇申小娟吴述平张侃
Owner JIANGSU UNIV
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