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Method for synthesizing metal-organic framework material mil-101-cr with carboxylate as organic ligand and its purification method

A metal-organic framework, organic ligand technology, applied in the separation/purification of carboxylic acid compounds, organic chemical methods, preparation of organic compounds, etc., can solve the problems of serious sample loss, harsh conditions, difficult processing, etc. The effect of chemical production, less post-processing steps and low reaction temperature

Active Publication Date: 2020-06-02
NANTONG VOCATIONAL COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] However, the unreacted terephthalic acid is blocked in the narrow pores, which makes the purification process of MIL-101-Cr more complicated
Hot ethanol and ammonium fluoride solution can effectively remove terephthalic acid, which is a blockage, but the conditions are very harsh, it is quite difficult to handle, and the purification process is long, and the sample loss is very serious, which is very unfavorable for the batch production of MIL-101-Cr Production

Method used

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  • Method for synthesizing metal-organic framework material mil-101-cr with carboxylate as organic ligand and its purification method
  • Method for synthesizing metal-organic framework material mil-101-cr with carboxylate as organic ligand and its purification method
  • Method for synthesizing metal-organic framework material mil-101-cr with carboxylate as organic ligand and its purification method

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Experimental program
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preparation example Construction

[0041] (1) Preparation of terephthalate: Slowly add the alkali solution dropwise to the dimethylformamide (DMF) solution dissolved in terephthalic acid to obtain a white powder, dimethylformamide (DMF) and A mixed solution of equal volume of water is used to recrystallize the white powder to obtain terephthalate crystals;

[0042] Among them, the preferred salt of terephthalate is potassium hydrogen terephthalate, which is prepared by slowly adding potassium hydroxide solution dropwise into dimethylformamide (DMF) solution dissolved with terephthalic acid to obtain white Powder, dimethylformamide (DMF) and water equal volume mixed solution to recrystallize the white powder to obtain potassium hydrogen terephthalate crystals.

[0043] The molar ratio of potassium hydroxide and terephthalic acid is 1:1.

[0044] (2) Synthesis of samples: take chromium nitrate nonahydrate and potassium hydrogen terephthalate with a molar ratio of 0.8~1.2:1, adjust the pH value of the system to 3...

specific Embodiment

[0050] Specific examples: Ratio of experimental raw materials Potassium hydrogen terephthalate: chromium nitrate nonahydrate = 1:1 (molar ratio), which is the best ratio of organic ligands and metal ions in the synthesis of MIL-101-Cr. Acetic acid was selected as the mineralizer. Acetic acid with monodentate ligands can induce the terephthalate radicals of the bidentate ligands to coordinate with metal ions, which is beneficial to the nucleation of crystals. Acetic acid can also adjust the pH value of the solution. When the pH is 3~4, it is beneficial to the formation of MIL-101-Cr.

[0051] Temperature is a very critical factor for the hydrothermal reaction, and the selected temperatures are 140°C, 160°C and 180°C for 12 hours, as shown in Table 1 below. It was found that the temperature at 140°C was too low, and no solids were produced except the recrystallization of terephthalic acid; the temperature at 180°C was too high, and the solids produced were detected as amorphous ...

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Abstract

The invention provides a method for synthesizing a metal-organic framework MIL-101-Cr with carboxylate as organic ligand and a purifying method for the MIL-101-Cr. The method comprises the following steps: preparation of terephthalate; synthesis of a sample; purification of the sample; etc. According to the invention, terephthalate is used for replacing terephthalic acid as organic ligand for hydro-thermal synthesis of the MIL-101-Cr, so the problem of obstruction of microchannels caused by difficulty in dissolving terephthalic acid in water can be overcome; nitrogen adsorption, XRD, TEM and other methods are employed for characterization of MIL-101-Cr synthesized with carboxylate as the organic ligand. Results show that an unpurified MIL-101-Cr product has a clear microporous structure and has a BET specific surface area of 2600 m<2> / g. The product has uniform particle sizes and is a crystal with a small particle size of 60 nm, which is far less than the particle size of a product prepared by using a traditional hydrothermal method. The MIL-101-Cr synthesized with carboxylate as the organic ligand has high purity without complex subsequent purification, and the yield of the MIL-101-Cr reaches 70%.

Description

technical field [0001] The invention belongs to the technical field of synthesis of metal organic framework materials, and in particular relates to a method for synthesizing metal organic framework material MIL-101-Cr with carboxylate as an organic ligand and a purification method thereof. Background technique [0002] Metal-organic frameworks (MOFs) are one-dimensional, two-dimensional or three-dimensional porous materials formed by the hybridization of metals or metal clusters with organic ligands. MOFs materials have an orderly and adjustable pore structure with a wide range of sizes. These special structural properties make it have a high specific surface area and a large pore volume. However, the hydrothermal stability of most MOFs materials is low, which limits their applications, while MIL-101-Cr still maintains good thermal stability at a high temperature of 350 °C, and MIL-101-Cr also has properties that other MOFs materials cannot Compared characteristics, such as...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/41C07C51/43C07C63/28C07F11/00
CPCC07B2200/13C07C51/418C07C51/43C07F11/005C07C63/28
Inventor 马正飞陶海军黄艳芳刘志军
Owner NANTONG VOCATIONAL COLLEGE
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