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Porous silica ceramic loaded cu-mof adsorbent and preparation method thereof

A technology supported by porous silica and ceramics, applied in chemical instruments and methods, and other chemical processes, can solve problems such as in-situ growth and compounding of MOF, destruction of MOF pore structure, and decrease in specific surface area, and achieve high strength and high stability Protective effect, improve adsorption performance, and improve utilization efficiency

Inactive Publication Date: 2019-03-19
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In summary, porous silica ceramic supports have been widely used as catalyst support materials, but have not been used in the in situ growth composite of MOFs.
However, the existing MOF molding technology will cause a certain degree of damage to the MOF pore structure, which will eventually lead to a decrease in the specific surface area.

Method used

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  • Porous silica ceramic loaded cu-mof adsorbent and preparation method thereof
  • Porous silica ceramic loaded cu-mof adsorbent and preparation method thereof
  • Porous silica ceramic loaded cu-mof adsorbent and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0048] This embodiment provides a method for preparing a porous silica ceramic loaded Cu-MOF adsorbent, which includes the following steps:

[0049] (1) Preparation of porous silica ceramic carrier

[0050] Mix 10g of silica powder, 0.3g of sodium polyacrylate, 19.44mL of camphene, 2.92mL of tert-butanol and 0.5g of yttrium oxide into a flask, and stir evenly at 75°C for 8h to obtain a slurry;

[0051] Pour the slurry into the mold and place it at -16°C for 1 hour to obtain a columnar silica ceramic particle preform;

[0052] The preform of silica ceramic particles was first placed at -16°C for 12h, then placed in a freeze dryer and dried at -60°C for 6h, and finally heated at a rate of 4°C / min for high-temperature sintering, and the temperature was raised to 1000°C, heat preservation for 3 hours, and obtain a porous silica ceramic carrier after cooling.

[0053] The pore size distribution curve of the porous silica ceramic carrier is as follows figure 1 As shown, the surfa...

Embodiment 2

[0062] This embodiment provides a method for preparing a porous silica ceramic loaded Cu-MOF adsorbent, which includes the following steps:

[0063] (1) The preparation process of the porous silica ceramic carrier is the same as in Example 1;

[0064] (2) In situ synthesis of Cu-BTC

[0065] Mix 1.26g of trimesic acid with 50mL of dimethylformamide and stir evenly to obtain an organic ligand solution;

[0066] Take 5g of the porous silica ceramic carrier and put it into the organic ligand solution prepared above, soak it for 12h, filter it with suction, put the obtained sample into 50mL ethanol solution with a mass fraction of 95%, add 2.85g nitric acid trihydrate Copper, stirred evenly, reacted at 80°C for 22h, filtered, washed, and dried at 100°C for 10h to obtain porous silica ceramic loaded Cu-MOF adsorbent (i.e. composite material Cu-BTC-SiO 2 ), according to the TG result calculation loading is 5.5wt%.

[0067] Porous silica ceramic supported Cu-MOF adsorbent (Cu-BTC-...

Embodiment 3

[0070] This embodiment provides a method for preparing a porous silica ceramic loaded Cu-MOF adsorbent, which includes the following steps:

[0071] (1) The preparation process of the porous silica ceramic carrier is the same as in Example 1;

[0072] (2) In situ synthesis of Cu-BTC

[0073] Mix 1.68 g of trimesic acid with 50 mL of ethanol solution with a mass fraction of 95%, and stir evenly to obtain a ligand solution;

[0074] Put 5g of porous silica ceramic carrier into the ligand solution, soak for 12h, filter with suction, put the filtered sample into 50mL of ethanol solution with a mass fraction of 95%, add 3.80g of copper nitrate trihydrate, and stir evenly , reacted at 80°C for 22h, filtered, washed, and dried at 100°C for 10h to obtain a porous silica ceramic supported Cu-MOF adsorbent (i.e. the composite material Cu-BTC-SiO 2 ). The loading was calculated to be 7.2 wt% based on the TG results.

[0075] Porous silica ceramic supported Cu-MOF adsorbent (Cu-BTC-Si...

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Abstract

The invention provides a porous silicon dioxide ceramic loaded Cu-MOF adsorbent and a preparation method thereof. The method comprises the steps that an organic ligand for synthesizing Cu-MOF and a solvent are mixed to obtain an organic ligand solution; a porous silicon dioxide ceramic carrier is dipped into a ligand solution, and filtering and washing are performed; the porous silicon dioxide ceramic carrier is placed into the solvent, a copper source is added for a synthesis reaction, after the reaction is ended, filtering, washing and drying are performed, and the porous silicon dioxide ceramic loaded Cu-MOF adsorbent is obtained, wherein the pore diameter of the porous silicon dioxide ceramic carrier is 0.1-100 micrometers, the porosity is 60-85% and the compressive strength is 1-7 MPa. The porous silicon dioxide ceramic loaded Cu-MOF adsorbent obtained through the method has the good liquid phase adsorption performance and can be applied to the fields of gas storage, adsorption separation, catalysis, liquid phase adsorption and separation and the like.

Description

technical field [0001] The invention relates to a porous silica ceramic loaded Cu-MOF adsorbent and a preparation method thereof, belonging to the technical field of organic-inorganic porous composite materials and preparation methods thereof. Background technique [0002] Metal-organic frameworks (MOFs) are porous crystalline materials assembled by metal ions and organic ligands. Since their pore size and surface properties can be tuned by changing the types of metal and organic ligands and synthesis conditions, MOF materials can be used as ideal adsorbents for adsorption separation. HKUST-1, as a typical Cu-MOF material, was first reported by Hong Kong University of Science and Technology Chui et al. ), HKUST-1 has a high specific surface area and excellent performance. It is a landmark compound in the MOF family and belongs to the face-centered cubic crystal. The three-dimensional network structure contains square pore openings with a diameter of 0.9nm, which expand alo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/22B01J20/30
CPCB01J20/0237B01J20/103B01J20/223
Inventor 张瑛高伟常青王珏杨道瑞张玉龙
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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