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pd/mpg-c 3 no 4 Catalyst recycling method in hbiw hydrogenolysis reaction

A mpg-c3n4, hydrogenolysis reaction technology, applied in metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve problems such as catalyst deactivation and achieve the realization of recycling application, reduce production costs, and improve the effect of application prospects

Active Publication Date: 2021-05-28
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to solve the problem of deactivation after use of catalysts in the prior art, and to provide a method for recycling Pd / mpg-C3N4 catalysts in HBIW hydrogenolysis reactions

Method used

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  • pd/mpg-c <sub>3</sub> no <sub>4</sub> Catalyst recycling method in hbiw hydrogenolysis reaction
  • pd/mpg-c <sub>3</sub> no <sub>4</sub> Catalyst recycling method in hbiw hydrogenolysis reaction
  • pd/mpg-c <sub>3</sub> no <sub>4</sub> Catalyst recycling method in hbiw hydrogenolysis reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Pd / mpg-C 3 N 4 Catalyst preparation

[0030] 1g mpg-C 3 N 4 Disperse in 100ml deionized water, stir for 15min, add 3.4ml PdCl 2 Aqueous solution (50mg / ml), stirred for 3h, then added 4.2ml NaBH 4 solution (2mg / ml), stirred for 1h, filtered, washed with water until neutral, and vacuum dried at 70°C for 10h to obtain Pd / mpg-C with a palladium content of 4.91%. 3 N 4 catalyst.

[0031] Hydrogenolysis of Hexabenzylhexaazaisowurtzitane

[0032] 3.4g HBIW, 346mg 4.91% Pd / mpg-C 3 N 4 Add the catalyst and 6ml DMF into the reaction flask, keep the temperature <10°C in a cold water bath, replace the gas in the reaction flask with nitrogen three times, then replace the gas in the reaction flask with hydrogen three times, add 0.06ml of bromobenzene and 6ml of acetic anhydride, and start the stirring reaction. Hydrogen is supplied continuously with a hydrogen balloon. Raise the temperature to 18°C ​​for 1 hour, and then raise the temperature to 45°C for 8 hours. After the...

Embodiment 2

[0034] 1g mpg-C 3 N 4 Disperse in 100ml deionized water, stir for 15min, add 5ml PdCl 2 Aqueous solution (50mg / ml), stirred for 3h, then added 6.2ml NaBH 4 solution (2mg / ml), stirred for 1h, filtered, washed with water until neutral, and vacuum dried at 70°C for 10h to obtain Pd / mpg-C with a palladium content of 7.44%. 3 N 4 catalyst.

[0035] Hydrogenolysis of Hexabenzylhexaazaisowurtzitane

[0036] 3.4g HBIW, 228mg 7.44% Pd / mpg-C 3 N 4 Add the catalyst and 6ml DMF into the reaction flask, keep the temperature <10°C in a cold water bath, replace the gas in the reaction flask with nitrogen three times, then replace the gas in the reaction flask with hydrogen three times, add 0.06ml of bromobenzene and 6ml of acetic anhydride, and start the stirring reaction. Hydrogen is supplied continuously with a hydrogen balloon. Raise the temperature to 18°C ​​for 1 hour, and then raise the temperature to 45°C for 8 hours. After the reaction, cool down to room temperature, filter, ...

Embodiment 3

[0038] 1g mpg-C 3 N 4 Disperse in 100ml deionized water, stir for 15min, add 6.7ml PdCl 2 Aqueous solution (50mg / ml), stirred for 3h, then added 8.3ml NaBH 4 solution (2mg / ml), stirred for 1h, filtered, washed with water until neutral, and vacuum dried at 70°C for 10h to obtain Pd / mpg-C with a palladium content of 11.13%. 3 N 4 catalyst.

[0039] Hydrogenolysis of Hexabenzylhexaazaisowurtzitane

[0040] 3.4g HBIW, 153mg 11.13% Pd / mpg-C 3 N 4 Add the catalyst and 6ml DMF into the reaction flask, keep the temperature <10°C in a cold water bath, replace the gas in the reaction flask with nitrogen three times, then replace the gas in the reaction flask with hydrogen three times, add 0.06ml of bromobenzene and 6ml of acetic anhydride, and start the stirring reaction. Continuous supply of hydrogen with a hydrogen balloon,. Raise the temperature to 18°C ​​for 1 hour, and then raise the temperature to 45°C for 8 hours. After the reaction, cool down to room temperature, filter, e...

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Abstract

The present invention relates to a Pd / mpg‑C 3 N 4 The invention relates to a recycling application method of catalyst in HBIW hydrogenolysis reaction, which belongs to the technical field of noble metal catalysis. The invention loads commonly used palladium metal on a novel carrier mpg-C 3 N 4 On the other hand, metal palladium in this catalyst has high dispersion and stability, and the catalyst has a graphite phase mesopore structure and unsaturated ‑NH and ‑NH 2 The group increases the adsorption of the catalyst to HBIW and improves the transfer efficiency of HBIW in the catalyst, realizes the efficient hydrogenation of HBIW under low pressure conditions, and the catalyst can be recycled, which overcomes the current industrial use of catalysts in the hydrogenolysis of HBIW The problem of post-inactivation greatly reduces the production cost of CL‑20, and has a very high application prospect.

Description

technical field [0001] The present invention relates to a kind of palladium (Pd / mpg-C) supported by mesoporous graphite phase carbon nitride 3 N 4 ) The cyclic application of catalyst in the hydrogenolysis reaction of hexabenzylhexaazaisowurtzitane (HBIW) belongs to the technical field of noble metal catalysis. Background technique [0002] Hexanitrohexaazaisowurtzitane (CL-20), as a cage-like high-energy and high-density material, is the fourth-generation explosive widely used in the world. At present, the production of CL-20 is mainly synthesized by hydrogenolysis and nitration of hexabenzylhexaazaisowurtzitane (HBIW). However, since the cage structure of HBIW is unstable after debenzyl grouping, its hydrogenolysis often occurs at It is carried out at normal temperature, and at the same time, acetyl reagent is used to protect the cage structure in the process of hydrogenolysis, so the catalyst is required to have higher catalytic activity. The currently widely used cata...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24B01J23/44B01J37/16C07D487/22
CPCB01J23/44B01J27/24B01J37/16C07D487/22Y02P20/584
Inventor 陈锟刘伟黎胜富陈树森金韶华李丽洁束庆海陈煜
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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