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Hectogram-scale solution crystallization method for preparing [Ba(BTO)(H2O)]n barium-based energetic metal organic frameworks

A metal-organic framework and solution crystallization technology, applied in the production of bulk chemicals, etc., can solve the problems of large-scale synthesis processes that have not been reported, and achieve the effect of rapid preparation

Active Publication Date: 2021-04-02
INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the large-scale synthesis process of energetic metal-organic framework materials based on 5,5'-bitetrazolium-1,1'-dioxanion has not been reported

Method used

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  • Hectogram-scale solution crystallization method for preparing [Ba(BTO)(H2O)]n barium-based energetic metal organic frameworks
  • Hectogram-scale solution crystallization method for preparing [Ba(BTO)(H2O)]n barium-based energetic metal organic frameworks

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Step 1: Preparation of mother liquor of acidic 5,5'-bistetrazole-1,1'-dioxanol ammonium salt

[0028] Weigh 118.0 g of 5,5'-bitetrazolium-1,1'-dioxanol ammonium salt and transfer it to a clean flask, and add 500 ml of deionized water into the flask to form a cloudy liquid. Heat the turbid solution to 60°C and keep stirring until the 5,5'-bistetrazole-1,1'-dioxyhydroxyl ammonium salt is completely dissolved, and add concentrated hydrochloric acid (36.5%wt) to it to adjust the pH value to 5. Form the mother liquor of acidic 5,5'-bistetrazole-1,1'-dioxanol ammonium salt.

[0029] Step 2: Mother liquor preparation of inorganic metal barium salt

[0030] Weigh 104.1g of barium chloride and transfer it to a clean weighing bottle, add 500ml of deionized water to the weighing bottle, and stir continuously at room temperature until completely dissolved to form a barium chloride mother liquor.

[0031] Step 3: Mixing of mother liquor and aging of crystals

[0032] Slowly drop ...

Embodiment 2

[0037] Step 1: Preparation of mother liquor of acidic 5,5'-bistetrazole-1,1'-dioxanol ammonium salt

[0038] Weigh 118.0 g of 5,5'-bitetrazolium-1,1'-dioxanol ammonium salt and transfer it into a clean flask, and add 1000 ml of deionized water into the flask to form a cloudy liquid. Heat the turbid solution to 60°C and keep stirring until the 5,5'-bistetrazole-1,1'-dioxohydroxyl ammonium salt is completely dissolved, and add concentrated hydrochloric acid (36.5%wt) to it to adjust the pH value to 4. Form the mother liquor of acidic 5,5'-bistetrazole-1,1'-dioxanol ammonium salt.

[0039] Step 2: Mother liquor preparation of inorganic metal barium salt

[0040] Weigh 104.1g of barium chloride and transfer it to a clean weighing bottle, add 1000ml of deionized water to the weighing bottle, and stir continuously at room temperature until completely dissolved to form a barium chloride mother liquor.

[0041] Step 3: Mixing of mother liquor and aging of crystals

[0042]The compl...

Embodiment 3

[0047] Step 1: Preparation of mother liquor of acidic 5,5'-bistetrazole-1,1'-dioxanol ammonium salt

[0048] Weigh 118.0 g of 5,5'-bitetrazolium-1,1'-dioxol ammonium salt and transfer it to a clean flask, and add 500 ml of deionized water to the weighing bottle to form a cloudy liquid. Heat the turbid solution to 60°C and keep stirring until the 5,5'-bistetrazole-1,1'-dioxohydroxyl ammonium salt is completely dissolved, and add concentrated hydrochloric acid (36.5%wt) to it to adjust the pH value to 4. Form the mother liquor of acidic 5,5'-bistetrazole-1,1'-dioxanol ammonium salt.

[0049] Step 2: Mother liquor preparation of inorganic metal barium salt

[0050] Weigh 130.7g of barium nitrate and transfer it to a clean weighing bottle, add 500ml of deionized water to the weighing bottle, and stir continuously at room temperature until completely dissolved to form a barium nitrate mother liquor.

[0051] Step 3: Mixing of mother liquor and aging of crystals

[0052] The comp...

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Abstract

The invention discloses a hectogram-scale solution crystallization method for preparing [Ba(BTO)(H2O)]n barium-based energetic metal organic frameworks, which comprises the following steps: 1, preparing an acidic 5,5'-bistetrazol-1,1'-dioxo hydroxylamine salt mother solution; 2, preparing an inorganic metal barium salt mother solution; 3, mixing the two mother solutions through a peristaltic pump,and carrying out solventing-out crystallization and crystal aging of [Ba(BTO)(H2O)]n under certain reaction conditions; and 4, carrying out post-treatment on the [Ba(BTO)(H2O)]n crystal. According tothe preparation method, the energetic ligand 5,5'-bistetrazole-1,1'-dioxo anions and barium ions can rapidly form the metal organic framework material by utilizing solution acidity adjustment, the high-quality barium-based metal organic framework crystal is obtained through proper aging, and the preparation technology can realize rapid preparation of the barium-based metal organic framework crystal in hundred-gram order.

Description

technical field [0001] The invention relates to the technical field of novel energetic materials, more specifically to the preparation of [Ba(BTO)(H 2 O)] n A method for solution crystallization of barium-based energetic metal-organic frameworks on a hundred-gram scale. Background technique [0002] Bistetrazole derivatives not only inherit the advantages of tetrazole derivatives, but also further increase the stability of the system and provide multiple sites for subsequent modification. Compared with the single tetrazole ring, it has more coordination combinations, which provides more possibilities for the construction of multi-dimensional, porous and energetic MOFs. Bicyclic and polycyclic tetrazole compounds are expected to be used in new explosive rocket propellants, gas generating agents, and low-smoke or smokeless pyrotechnics due to their excellent properties such as a large number of tetrazole rings, high nitrogen content, and mostly N2 gas. And it has been widel...

Claims

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Application Information

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IPC IPC(8): C08G83/00
CPCC08G83/008Y02P20/54
Inventor 张祺陈东李洪珍
Owner INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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