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Preparation method and application of mil-101(cr) crude sample and mil-101(cr) material

A sample and reaction technology, applied in the preparation of organic compounds, nanotechnology for materials and surface science, carboxylate preparation, etc., can solve the problems of uncontrollable product particle size, complicated synthesis process, and low quality, and achieve Excellent thermochemical stability, simple preparation method, and high porosity

Active Publication Date: 2022-03-01
HUNAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the nano-scale MIL-101(Cr) synthesized by other scientists has a complex synthesis process, low yield (<40%), and low quality, and the particle size of the product is uncontrollable.

Method used

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  • Preparation method and application of mil-101(cr) crude sample and mil-101(cr) material
  • Preparation method and application of mil-101(cr) crude sample and mil-101(cr) material
  • Preparation method and application of mil-101(cr) crude sample and mil-101(cr) material

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Experimental program
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Effect test

Embodiment 1

[0036] The present embodiment provides a kind of preparation method of MIL-101 (Cr) crude sample, is based on MIL-101 (Cr) hydrothermal synthesis, comprises the following steps:

[0037] S1 Add 400g of chromium nitrate nonahydrate, 166g of terephthalic acid and 5L of water into the hydrothermal reaction kettle, stir at room temperature for 10min, then add 40g of acetic acid to react;

[0038] S2. Raise the temperature of the reactor to 200°C at a rate of 1°C / min; keep the temperature at this temperature for 8 hours; finally control the cooling rate, and lower the reactor to room temperature at a rate of 0.5°C / min to obtain MIL-101 ( Cr) crude sample.

[0039] Wherein, the water described in step S1 is deionized water.

[0040] Wherein, the volume of the hydrothermal reaction tank described in step S1 is 3L.

Embodiment 2

[0042] The present embodiment provides a kind of preparation method of MIL-101 (Cr) crude sample, is based on MIL-101 (Cr) hydrothermal synthesis, comprises the following steps:

[0043] S1 Add 400g of chromium nitrate nonahydrate, 166g of terephthalic acid and 5L of water into the hydrothermal reaction kettle, stir at room temperature for 20min, then add 40g of acetic acid to react;

[0044] S2. Raise the temperature of the reactor to 220°C at a rate of 1°C / min; keep the temperature at this temperature for 20 hours; finally control the cooling rate, and lower the reactor to room temperature at a rate of 0.5°C / min to obtain MIL-101 (Cr) crude sample.

[0045] Wherein, the water described in step S1 is distilled water.

[0046] Wherein, the volume of the hydrothermal reaction tank in step S1 is 10L.

Embodiment 3

[0048] The present embodiment provides a kind of preparation method of MIL-101 (Cr) crude sample, is based on MIL-101 (Cr) hydrothermal synthesis, comprises the following steps:

[0049] S1 Add 400g of chromium nitrate nonahydrate, 166g of terephthalic acid and 5L of water into the hydrothermal reaction kettle, stir at room temperature for 10min, then add 40g of acetic acid to react;

[0050] S2. Raise the temperature of the reactor to 300°C at a rate of 1°C / min; keep the temperature at this temperature for 8 hours; finally control the cooling rate, and lower the reactor to room temperature at a rate of 0.5°C / min to obtain MIL-101 ( Cr) crude sample.

[0051] Wherein, the water described in step S1 is deionized water.

[0052] Wherein, the volume of the hydrothermal reaction tank described in step S1 is 3L.

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Abstract

The invention relates to a metal-organic framework material, and discloses a crude sample of MIL-101 (Cr) and a preparation method and application of the MIL-101 (Cr) material. The present invention proposes an industrialized large-scale preparation method of high-quality MIL‑101 (Cr) for the first time, and the preparation method is simple and has no pollution to the environment. In addition, the present invention uses acetic acid as the mineralizer prepared by MIL-101 (Cr), and can obtain nanoparticles ranging from 30 to 100 nm. It solves the problem that it is difficult to obtain uniform nanoscale materials in the preparation of MIL‑101 (Cr). The MIL‑101 (Cr) nanomaterials prepared by the preparation method proposed by the present invention have pore sizes of 2.9nm and 3.4nm, particle diameters of 30nm to 100nm, and BET specific surface areas of 3000 to 3500m 2 / g, the morphology under the microscopic scanning electron microscope is a uniform regular octahedron, the particle size of the material is controllable, the thermochemical stability is excellent, and the porosity is high. Moreover, the aftertreatment of the material is simple and environmentally friendly, and only ethanol and water are used as detergents.

Description

technical field [0001] The present invention relates to metal-organic framework materials, more specifically, to the preparation method and application of MIL-101(Cr) crude samples and MIL-101(Cr) materials. Background technique [0002] In 2005, the Férey laboratory in France synthesized the MIL-101(Cr) material for the first time in a small scale (5mL) by adding hydrofluoric acid at 220°C by hydrothermal reaction method. Its naming was also proposed by Professor Férey, MIL=Materials Institute Lavoisier's structure is similar to the enhanced MTN zeolite topology. MIL-101(Cr) has two different types of inner cages, the diameters of which are and Aperture window diameter up to Has a very high specific surface area (BET specific surface area reached 4000m 2 / g). MIL-101 (Cr) has a terminal water molecule attached to the octahedral Cr(III) building block, and this water molecule is removable under high vacuum conditions, thus creating potential Lewis acid sites. MIL-10...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/41C07F11/00C07C63/28B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C07C51/418C07F11/005C07C63/28
Inventor 赵田杨玲刘跃军
Owner HUNAN UNIV OF TECH