Application of palladium-based bimetallic catalyst in catalytic hydrogenolysis reaction of HBIW

A bimetallic catalyst, isowurtzitane catalyzing hydrogen technology, which is applied in the directions of metal/metal oxide/metal hydroxide catalyst, physical/chemical process catalyst, organic chemistry, etc., can solve the problem of high production cost and achieve low production cost , Good application prospect, low content effect

Active Publication Date: 2017-07-14
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem actually solved by the present invention is to overcome the defect that the conventionally used catalyst in the catalytic hydrogenolysis reaction of HBIW is a precious metal palladium carbon catalyst in the prior art, resulting in higher production costs, and provides a palladium-based bimetallic catalyst in HBIW Applications in catalytic hydrogenolysis reactions

Method used

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  • Application of palladium-based bimetallic catalyst in catalytic hydrogenolysis reaction of HBIW
  • Application of palladium-based bimetallic catalyst in catalytic hydrogenolysis reaction of HBIW

Examples

Experimental program
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Effect test

Embodiment 1

[0042] Preparation of palladium-based bimetallic catalyst:

[0043] Put the mixed solution of 10mg / mL chloropalladium acid and ferrous chloride into 200mL water, stir evenly, then add 1.0g of silicon oxide, stir for 1h, then add precipitant (sodium hydroxide), adjust the pH value to 13, in After mixing and reacting in a water bath at 60°C for 5h, add a reducing agent (sodium borohydride, the amount is 30 times the total molar amount of palladium and iron), stir for 0.5h, filter, wash, and vacuum dry at 60°C to obtain SiO 2 Supported Pd-Fe bimetallic catalyst, the molar ratio of palladium to iron is 1:1, and the total loading is 10%.

[0044] Hydrogenolytic debenzylation of hexabenzylhexaazaisowurtzitane (HBIW):

[0045] Put 1.0g of HBIW, 2.5mL of DMF, 1.5mL of acetic anhydride, 0.02mL of bromobenzene, and 0.05g of the above-mentioned catalyst into the reaction vessel, charge and discharge hydrogen, then charge the hydrogen to 4bar, react at 18°C ​​for 4h, then raise the tempe...

Embodiment 2

[0047] In the preparation process of the palladium-based bimetallic catalyst of this embodiment, the carrier used is TiO 2 , other operations and parameters are the same as in Example 1.

[0048] The operation and parameters of the hydrogenolysis debenzylation reaction of hexabenzylhexaazaisowurtzitane (HBIW) in this example are the same as those in Example 1.

Embodiment 3

[0050] In the preparation process of the palladium-based bimetallic catalyst of this embodiment, the carrier adopted is Al 2 o 3 , other operations and parameters are the same as in Example 1.

[0051] The operation and parameters of the hydrogenolysis debenzylation reaction of hexabenzylhexaazaisowurtzitane (HBIW) in this example are the same as those in Example 1.

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Abstract

The invention discloses an application of a palladium-based bimetallic catalyst in the catalytic hydrogenolysis reaction of HBIW. The HBIW is an intermediate hexabenzylhexaazaisowurtzitane in the synthesis process of an energetic material CL-20. The palladium-based bimetallic catalyst is prepared through substituting precious metal with cheap transition metal and adopting oxide as a carrier, and has high catalytic reaction activity, high yield, high selectivity and high stability in the catalytic hydrogenolysis debenzylation reaction of the HBIW; and the palladium-based bimetallic catalyst has the advantages of easily available raw materials, low content of the precious metal palladium, low production cost, simple process, effective reduction of the industrial production cost, and very good application prospect.

Description

technical field [0001] The invention relates to the application of an oxide-loaded palladium-based bimetallic catalyst in the catalytic hydrogenolysis reaction of hexabenzylhexaazaisowurtzitane (HBIW). Background technique [0002] During the synthesis of high-density energetic material CL-20, the intermediate product hexabenzylhexaazaisowurtzitane (HBIW) is the precursor for the synthesis of high-energy density material CL-20, and its hydrogenolytic debenzylation reaction is the key to the synthesis of this compound step. However, because the cage structure of HBIW is very unstable, the hydrogenolysis reaction can only be carried out under mild conditions, so the activity of the catalyst is required to be high. The commonly used catalyst is palladium carbon catalyst. For example, the catalyst with better catalytic effect for HBIW hydrogenolysis debenzylation is Degussatype E101NE / W (US P WO 97 / 20785). However, palladium-carbon catalysts have problems such as high amount o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/22B01J23/89
CPCB01J23/8906B01J23/892C07D487/22
Inventor 杨军刘爽
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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