Nitrogen-doped titanium dioxide supported palladium catalyst for TADBIW hydrogenolysis debenzylation and preparation and application of catalyst

A titanium dioxide and palladium catalyst technology, applied in the directions of physical/chemical process catalysts, organic chemistry, chemical instruments and methods, etc., can solve the problem of difficulty in ensuring high atomic utilization and high catalytic activity of noble metals, limiting large-scale mass production, and difficult preparation processes. Large and other problems, to achieve the effect of reducing synthesis cost, high yield and high selectivity

Active Publication Date: 2021-05-28
SHANGHAI UNIV OF ENG SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this patent, the inventor mixed TiN and Pd precursors, roasted them, and then electroreduced them to obtain palladium / nitrogen-doped titanium dioxide. This preparation method not only involves complex raw materials, such as titanium nitride, but also has a difficult and cumbersome preparation process. Both high-temperature roasting and electrical reduction will limit large-scale mass production. At the same time, high-temperature roasting will inevitably cause agglomeration and sintering of precious metals, reducing the degree of dispersion, and it is difficult to ensure high atomic utilization and high catalytic activity of precious metals.

Method used

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  • Nitrogen-doped titanium dioxide supported palladium catalyst for TADBIW hydrogenolysis debenzylation and preparation and application of catalyst
  • Nitrogen-doped titanium dioxide supported palladium catalyst for TADBIW hydrogenolysis debenzylation and preparation and application of catalyst
  • Nitrogen-doped titanium dioxide supported palladium catalyst for TADBIW hydrogenolysis debenzylation and preparation and application of catalyst

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preparation example Construction

[0032] A kind of preparation method of nitrogen-doped titania supported palladium catalyst as described above, described preparation method specifically comprises the following steps:

[0033] (a) Take the titanium precursor and add it to the solvent and stir it, then add a nitrogen source to form a mixture, stir until it is completely hydrolyzed, then age and post-treat to obtain a nitrogen-doped titanium dioxide carrier. The titanium precursor is selected from isopropyl titanate, One or more mixtures of tetrabutyl titanate, titanium acetate or titanium tetrachloride, the solvent is selected from one or more mixtures of water, methanol, ethanol, isopropanol or ethylene glycol, and the nitrogen source is selected from Since one or more of ammonium chloride, ammonia water, ammonium carbonate, ammonium bicarbonate or ethylenediamine are mixed, the temperature of hydrolysis is room temperature, the temperature of aging is room temperature, and the aging time is 15h. The post-treat...

Embodiment 1

[0037] A nitrogen-doped titanium dioxide-supported palladium catalyst for TADBIW hydrogenolysis and debenzylation, with nitrogen-doped titanium dioxide as a carrier, palladium as an active component, palladium loaded on the carrier, and the doping amount of nitrogen is 5wt.% of the total amount of the carrier , through XRD characterization analysis, see Figure 4 , No diffraction peak of any palladium was found, indicating that the particle size of palladium was no more than 3nm, palladium was in granular form, and the loading of palladium was 2wt.% of the total amount of the catalyst. Prepared by the following steps:

[0038] First, a 5wt.% nitrogen-doped titanium oxide support was prepared by the sol-gel method:

[0039] Add 4ml of isopropyl titanate to 10ml of isopropanol, stir, take 0.2252g of ammonium chloride and dissolve it in 0.7ml of deionized water to form an ammonium chloride solution, and add the ammonium chloride solution to the above-mentioned isopropanol , sti...

Embodiment 2

[0046] A nitrogen-doped titanium dioxide-supported palladium catalyst for TADBIW hydrogenolysis and debenzylation, with nitrogen-doped titanium dioxide as a carrier, palladium as an active component, palladium loaded on the carrier, and the doping amount of nitrogen is 1wt.% of the total amount of the carrier , the loading of palladium is 2wt.% of the total amount of catalyst, that is, in the catalyst, except that the nitrogen doping amount is different from that of Example 1, all the others are the same as the materials shown in Example 1, due to the nitrogen doping of the catalyst The impurity is 1wt.%, so the catalyst is recorded as Pd / N 1 TiO 2 -2, the weighing amount of raw materials in the preparation step is weighed as required, and the rest are the same as in Example 1. Among them, the intermediate product 1% nitrogen-doped titanium oxide N 1 TiO 2 The color of the powder sample is yellow, see the photo figure 1 . Pd / N 1 TiO 2 -2 is used for the TADBIW hydrogeno...

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Abstract

The invention relates to a nitrogen-doped titanium dioxide supported palladium catalyst for TADBIW hydrogenolysis debenzylation and preparation and application of the catalyst. The catalyst takes nitrogen-doped titanium dioxide as a carrier and palladium as an active component, the palladium is supported on the carrier, the doping amount of nitrogen is 0-10 wt.%, but not 0,of the total amount of the carrier, and the loading amount of the palladium is 0.1-10 wt.% of the total amount of the catalyst. The preparation method specifically comprises the following steps: (a) adding a titanium precursor into a solvent, stirring, adding a nitrogen source to form a mixture, stirring until the mixture is completely hydrolyzed, aging, and carrying out post-treatment to obtain a nitrogen-doped titanium dioxide carrier; and (b) adding the nitrogen-doped titanium dioxide carrier obtained in the step (a) into a solvent, stirring, adding a palladium precursor, stirring, adding a precipitator, adjusting the pH value to be alkaline, and performing post-treatment to obtain the nitrogen-doped titanium dioxide supported palladium catalyst. Compared with the prior art, the catalyst provided by the invention has the characteristics of high hydrogenolysis debenzylation reaction activity, high yield, high selectivity, good stability and the like.

Description

technical field [0001] The invention belongs to the field of catalyst application, and in particular relates to a nitrogen-doped titania-supported palladium catalyst for hydrogenolysis and debenzylation of TADBIW and its preparation and application. Background technique [0002] The process of hydrogenolytic debenzylation of tetraacetyldibenzylhexaazaisowurtzitane (TADBIW) is a key step in the synthesis of high energy density material CL-20 (scientific name hexanitrohexaazaisowurtzitane). TADBIW has a stable cage structure, can withstand a certain high temperature (>30°C), and has a stable molecular structure, especially the chemical bond C-N bond in the nitrogen-benzyl group is stable and not easy to break, which requires the catalyst to have sufficient Catalytic activity, reducing the activation energy, can break the C-N bond. At the same time, the solubility of TADBIW is extremely low, and the molecule is not easy to be dissolved. At present, the most researched solve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24C07D487/22
CPCB01J27/24C07D487/22
Inventor 唐展通刘双朱璇嘉熊良敏牛晓达刘维钱慧宇刘爽门勇
Owner SHANGHAI UNIV OF ENG SCI
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