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Functionalized MOFs material for improving stability of AlH3 as well as preparation method and application of functionalized MOFs material

A functional and stable technology, applied in the field of functionalized MOFs materials and their preparation

Active Publication Date: 2021-09-10
SHANGHAI JIAO TONG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The currently reported elevated AlH 3 The stability method although improved to some extent by the AlH 3 Stability, but to really solve the AlH 3 The stability problem still needs a more effective method

Method used

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  • Functionalized MOFs material for improving stability of AlH3 as well as preparation method and application of functionalized MOFs material
  • Functionalized MOFs material for improving stability of AlH3 as well as preparation method and application of functionalized MOFs material

Examples

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preparation example Construction

[0029]The present invention also provides a preparation method of the functionalized MOFs material, comprising the following steps:

[0030] Step1: Dissolve zirconium tetrachloride, 2-aminoterephthalic acid, and benzoic acid in the DMF solution at a molar ratio of 1:1:20, then put them into a stainless steel hydrothermal reaction kettle and mix evenly. React for 24 hours, cool slowly until the temperature drops to room temperature, and obtain a yellow powder. Centrifuge the powder with DMF solution for 3 to 4 times to remove unreacted ligands and metal ions; use ethanol as the extraction agent, and extract with Soxhlet for three days , remove the residual DMF solution to obtain a solid powder; dry and activate the obtained solid powder at 60°C for 8 hours to obtain a nanoscale metal-organic framework material matrix UiO-66-NH 2 ;

[0031] Step2: The prepared nanoscale metal organic framework material matrix UiO-66-NH 2 Stir and react with isocyanate at a specific temperature...

Embodiment 1

[0036] The synthesis of the TEMPO functionalized MOFs material of the present embodiment is as follows:

[0037] 8g metal organic framework material matrix UiO-66-NH 2 Dissolve the powder in 30ml of anhydrous DMF, add 15ml of isocyanate, and stir for 6 hours at 30°C in a closed and anhydrous environment to prepare an active MOFs solution whose terminal group is isocyanate, and repeatedly centrifuge and wash it with anhydrous DMF solution 4 to 5 times to obtain solid active MOFs. see figure 1 , is the electron paramagnetic resonance (EPR) spectrum of the MOFs material before and after the TEMPO functionalization; the triple broad peak at g=2.006 place in the spectrum coincides with the spectrum peak of the TEMPO free radical, indicating that by the functionalization method of Example 1, the TEMPO free radical is successfully Grafted onto the surface of MOFs material. figure 2 It is the X-ray diffraction (XRD) pattern of MOFs material before and after TEMPO functionalization...

Embodiment 2

[0041] The preparation method of TEMPO functionalized MOFs material described in this embodiment is the same as embodiment 1, when grafting TEMPO on the surface of MOFs, H 2 The molar ratio of N-TEMPO and MOFs is also consistent with Example 1, but the reaction condition is 40°C.

[0042] Integrating TEMPO-functionalized MOFs with AlH 3 Grind and mix well according to the mass ratio of 1:100, then heat at 60°C for 48 hours in an air atmosphere, and measure the modified AlH by the drainage method 3 hydrogen release volume.

[0043] After heating for 72 hours at 60°C in an air atmosphere, AlH with functionalized modified MOFs materials was measured by the drainage method. 3 The hydrogen release volume is 91ml.

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Abstract

The invention belongs to the field of AlH3 hydrogen-containing energy storage materials, and discloses a TEMPO free radical scavenger functionalized MOFs material for improving the stability of AlH3 as well as a preparation method and an application method of the TEMPO free radical scavenger functionalized MOFs material. The functional MOFs material is prepared from a metal organic framework material matrix UiO-66-NH2 and a free radical trapping agent 2, 2, 6, 6-tetramethylpiperidine nitrogen oxide (TEMPO). The preparation method comprises the following steps: enabling the metal organic framework material matrix UiO-66-NH2 to react with diisocyanate, so as to obtain active MOFs of which the end group is isocyanato; and then carrying out esterification reaction on the isocyanato and amino-substituted TEMPO. The invention discloses the preparation method of the functionalized MOFs material. The functionalized MOFs material is applied to improvement of the stability of AlH3, and the effectiveness of the functionalized MOFs material is verified through related characterization tests. The functionalized MOFs material has the characteristics of low cost, easy preparation, nanoscale and the like, can improve the stability after being ground and mixed with AlH3, and is especially suitable for the application of AlH3 in solid rocket propellants.

Description

technical field [0001] The invention belongs to the field of hydrogen storage high-energy materials, and relates to a functionalized MOFs material suitable for improving the stability of AlH3 and its preparation method and application. Background technique [0002] Replacing the commonly used aluminum powder fuel with higher energy fuel is an important way to improve the energy performance of solid propellants. Aluminum hydride (AlH 3 ) has significant advantages such as high hydrogen content, large combustion heat, good gas production performance, environmental protection and non-toxicity, and low flame signal. AlH 3 Replacing aluminum powder can significantly increase the specific impulse of solid propellants, so the development of AlH-based 3 Solid propellants for high-energy fuels are of great importance. [0003] H 3 The Al and H atoms in the crystal are connected by covalent bonds, but this covalent bond is unstable, and the covalent bond will gradually break under...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00C01B3/00
CPCC08G83/008C01B3/001Y02E60/32
Inventor 魏良明李伟庞爱民
Owner SHANGHAI JIAO TONG UNIV
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