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Complexing-type metallic nickel catalyst and preparing method and application thereof

A metal nickel and catalyst technology, applied to complex metal nickel catalyst and its preparation and application fields, can solve the problems of inability to recover and apply, high production cost, unsuitable for industrial production and the like

Inactive Publication Date: 2019-03-01
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalyst is expensive, cannot be recycled and applied mechanically, and the production cost is high, so it is not suitable for industrial production

Method used

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  • Complexing-type metallic nickel catalyst and preparing method and application thereof
  • Complexing-type metallic nickel catalyst and preparing method and application thereof
  • Complexing-type metallic nickel catalyst and preparing method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] No. I catalyst preparation:

[0022] Weigh 58g of RaneyNi catalyst (type KNAW-II), with an average particle size of 5 μm. The above RaneyNi catalyst and MoCl 5 Join in the aqueous sodium hydroxide solution of 500mL (the mass fraction of aqueous sodium hydroxide solution is 30%, the following examples are equal) and activate at room temperature, the metal aluminum in the Raney Ni catalyst is dissolved in the aqueous sodium hydroxide solution to form porous metallic nickel. MoCl during activation 5 Adsorbed on the surface of metallic nickel, filter, and filter residue is dried, and the particle diameter of catalyst is controlled with sieve, and the control average particle diameter is 5 μ m, obtains passivation pre-catalyst (the doping mass content of Mo metal element is 6% in the passivation pre-catalyst) ).

[0023] Add the passivation pro-catalyst prepared above to 100 mL of a mixed solvent of sulfide anisole, methyl phosphate and triethylamine in a volume ratio of ...

Embodiment 2

[0025] No. I-1 catalyst preparation:

[0026] The preparation process of No. I-1 catalyst repeats the preparation process of Example 1, but is different from the preparation process of Example 1: when the passivation front catalyst is added in the mixed solution of sulfide anisole, methyl phosphate and triethylamine , and stirred the reaction at -20°C for 60 days.

[0027] In the passivated catalyst finally prepared in this embodiment, the mass content of the complexing agent was 72%.

Embodiment 3

[0029] No. I-2 catalyst preparation:

[0030] The preparation process of No. I-2 catalyst repeats the preparation process of Example 1, but is different from the preparation process of Example 1: the volume ratio of 100mL is sulfide anisole, methyl phosphate and triethylamine of 1:1:1 The mixture was replaced with 100 mL of sulfide anisole. The reaction was stirred at -20°C for 30 days.

[0031] In the passivated catalyst finally prepared in this embodiment, the mass content of the complexing agent is 51%.

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Abstract

The invention discloses a complexing-type metallic nickel catalyst. The complexing-type metallic nickel catalyst comprises a porous-structure metallic nickel, a doped metallic element and a complexingagent, wherein the doped metallic element is doped on the surface of the metallic nickel, and the complexing agent is combined with the metallic nickel to form a complex, wherein the doped metallic element is one or more mixed metallic elements of Cr, Na, Fe, Mo, Mg, Ce, V, Ti, Nb, W, Re, Ru, Co, Mn, Rh, Ir, Bi, Au, Ag, Pd and Pt; in the complexing-type metallic nickel catalyst, the average particle size is 5 microns to 350 microns, the doping amount of each doped metallic element is 0.01 wt% to 8 wt%, and the content of the complexing agent is 1 wt% to 72 wt%. Through the complexing-type metallic nickel catalyst prepared with a preparing method, corresponding amine or hydroxylamine or mixtures is / are generated under the condition that a halogen-containing nitro-compound is catalyzed andhydrogenated, and dehalogenation is inhibited; corresponding amine or hydroxylamine or mixtures is / are generated under the condition that a benzyloxy-containing nitro-compound is catalyzed and hydrogenated, and debenzylation benzyloxy is inhibited.

Description

technical field [0001] The invention relates to a complex metal nickel catalyst and its preparation method and application Background technique [0002] The hydrogenation of aromatic nitro compounds or nitro compounds containing halogen, benzyloxy or unsaturated functional groups while inhibiting the reaction of dehalogenation, debenzyloxy or reduction of unsaturated functional groups is a key step for many current pharmaceutical intermediates. Although many current catalysts can reduce nitro groups to amines or hydroxylamines, they inevitably produce a large number of dehalogenated or debenzylated products, which greatly affects the yield and quality of the products, and directly affects the cost of the products. It is proposed in U.S. Patent US6423872 that by improving the activation strength of the Al-Ni alloy and changing the ratio of aluminum in the Al-Ni alloy, the content of aluminum is reduced to less than 5.5%, but a large amount of alumina will still be produced in...

Claims

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Application Information

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IPC IPC(8): B01J25/02B01J23/883B01J23/889B01J23/887B01J23/86B01J33/00C07C239/10C07C209/36C07C211/52C07D233/76
CPCB01J23/866B01J23/883B01J23/8878B01J23/8892B01J25/02B01J33/00C07C209/36C07C239/10C07D233/76C07C211/52
Inventor 苏为科徐峰余志群
Owner ZHEJIANG UNIV OF TECH
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