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Strontium titanate supported palladium catalyst for CL-20 synthesis, preparation and application thereof

A palladium catalyst, catalyst technology, applied in catalyst activation/preparation, physical/chemical process catalyst, metal/metal oxide/metal hydroxide catalyst, etc.

Active Publication Date: 2021-09-10
SHANGHAI UNIV OF ENG SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the literature and patents reported so far, the HBIW debenzylation catalyst supports are mainly carbon or titanium oxide, and there are no other reports on other supports.

Method used

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  • Strontium titanate supported palladium catalyst for CL-20 synthesis, preparation and application thereof
  • Strontium titanate supported palladium catalyst for CL-20 synthesis, preparation and application thereof
  • Strontium titanate supported palladium catalyst for CL-20 synthesis, preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Preparation of strontium titanate support (marked as: STOHT) by hydrothermal method:

[0041] Add 0.265mL titanium tetrachloride to the mixed solution of 1g ethylene glycol and 24mL water, stir evenly, add 30mL lithium hydroxide (3M) and 10mL strontium chloride (0.24M) and continue stirring for half an hour, transfer to the reaction kettle , and placed in a drying oven at 180°C for 48 hours, and then the white precipitate obtained by filtration was washed and dried to obtain a strontium titanate carrier, which was denoted as STOHT.

[0042] Preparation of 2% palladium supported strontium titanate catalyst (label: Pd-STOHT-2):

[0043] Put 0.5 g of the above carrier into 200 mL of deionized water, add the calculated amount of palladium chloride solution (10 mg / mL) and stir evenly, add sodium hydroxide solution to adjust the pH of the mixed solution to 10-11, and then continue to stir in a water bath at room temperature for 5 h , filtered, washed, dried at 60°C for 12h, ...

Embodiment 2

[0049] The loading of palladium was 2.5%, and the rest of the preparation process was the same as that in Example 1, which was denoted as Pd-STOHT-2.5.

[0050] Pd-STOHT-2.5 was used for the HBIW hydrogenolysis debenzylation reaction test. The experimental conditions, experimental parameters, and raw material weighing amount were the same as those in Example 1. The yields of the Pd-STOHT-2.5 catalyst in the above two-step reactions were respectively 85% and 84%, see Table 1.

Embodiment 3

[0052] The loading of palladium was 0.1%, and the rest of the preparation process was the same as that in Example 1, which was denoted as Pd-STOHT-0.1.

[0053] Pd-STOHT-0.1 was used for the HBIW hydrogenolysis debenzylation reaction test. The experimental conditions, experimental parameters, and raw material weighing amount were the same as those in Example 1. The yields of the Pd-STOHT-0.1 catalyst in the above two-step reactions were respectively 10% and 20%, see Table 1.

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Abstract

The invention relates to a one-step and two-step hydrogenolysis debenzylation catalyst for a key intermediate hexabenzylhexaazaisowurtzitane (HBIW) for synthesizing a high-energy density material hexanitrohexaazaisowurtzitane (CL-20) and preparation of the catalyst. The preparation method comprises the following steps: adopting strontium titanate as a carrier, and loading noble metal palladium with the palladium loading amount of 0.1-10% (mass percent). The catalyst provided by the invention has the characteristics of low usage amount of noble metal, high activity, high selectivity, good cycle stability and the like, adopts a novel carrier, not only improves the dispersity of noble metal palladium, but also improves the cycle stability of the catalyst, and has the advantages of easily available raw materials, simple process and good application prospect.

Description

technical field [0001] The invention relates to a high-energy density material hexanitrohexaazaisowurtzitane (CL-20) synthesis key intermediate hexabenzylhexaazaisowurtzitane (HBIW) one-step and two-step hydrogenolysis debenzylation catalyst and its Preparation and application. Background technique [0002] Hydrogenolytic debenzylation of hexabenzylhexaazaisowurtzitane (HBIW) is a key step in the synthesis of high energy density material CL-20. HBIW has a high-tension cage structure, which not only requires complex reaction conditions, but also requires auxiliaries and acylating reagents. These reagents will produce acidic substances, which are easy to corrode the catalyst, and must have low temperature and high activity, otherwise high temperature (>25°C) will easily break the cage. The activity is low, and the yield cannot be guaranteed. Therefore, HBIW debenzylation puts higher requirements on the catalyst, that is, the catalyst needs to provide higher catalytic acti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/02B01J23/58B01J35/00B01J37/03C07D487/22
CPCB01J23/58B01J37/035B01J23/02C07D487/22B01J35/394
Inventor 刘爽陈淑媛牛晓达熊良敏郭凯梁门勇
Owner SHANGHAI UNIV OF ENG SCI
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