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Fluorosilicate porous hybrid material as well as preparation method and application thereof

A technology of fluorosilicate and copper fluorosilicate is applied in the field of fluorosilicate porous hybrid materials and their preparation, which can solve the problems of high energy consumption and high cost, and achieve large adsorption capacity, enhanced identification, and separation selectivity. high effect

Pending Publication Date: 2021-02-02
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention is in order to overcome traditional separation C 2 h 2 / C 2 h 4 and C 2 h 2 / CO 2 The method has the problems of high energy consumption and high cost, and provides a method with large adsorption capacity, high separation selectivity, and simultaneous separation of C 2 h 2 / C 2 h 4 and C 2 h 2 / CO 2 Fluorosilicate porous hybrid materials

Method used

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  • Fluorosilicate porous hybrid material as well as preparation method and application thereof
  • Fluorosilicate porous hybrid material as well as preparation method and application thereof
  • Fluorosilicate porous hybrid material as well as preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Dissolve 54mg of 4,4'-dipyridyl disulfide in 2mL of methanol for 25min by ultrasonic (power 100W) vibration. Add 2 mL of copper hexafluorosilicate solution dropwise at a rate of 0.1 mL / s while stirring, the concentration of copper hexafluorosilicate solution is 0.1 mol / L, copper hexafluorosilicate and 4,4'-dipyridyl The molar ratio of disulfide is 1:1 (slight excess of ligand). The resulting mixed solution was continuously stirred at 25° C. for 72 h. After the reaction was completed, the mixture was filtered to obtain a blue powder, which was washed three times with anhydrous methanol to obtain a fluorosilicate porous hybrid material product.

[0034]Activation treatment to remove the guest solvent in the framework: first, the freshly synthesized fluorosilicate porous hybrid material product powder sample was subjected to at least 8 solvent exchanges with dry methanol within two days, and then on the Micromeritics ASAP 2020 instrument, at 50 ° C Vacuum for 24 hours unt...

Embodiment 2

[0043] Dissolve 54mg of 4,4'-dipyridyl disulfide in 2mL of methanol for 30 minutes by ultrasonic (power 80W) vibration. Add 2 mL of copper hexafluorosilicate solution dropwise at a rate of 0.05 mL / s while stirring, the concentration of copper hexafluorosilicate solution is 0.2 mol / L, copper hexafluorosilicate and 4,4'-dipyridyl The molar ratio of disulfide is 1:1.5 (slight excess of ligand). The resulting mixed solution was continuously stirred at 50° C. for 24 h. After the reaction, the mixture was filtered to obtain a blue powder, which was washed three times with anhydrous methanol to obtain a fluorosilicate porous hybrid material product.

Embodiment 3

[0045] Dissolve 54mg of 4,4’-dipyridyl disulfide in 2mL of methanol for 20min by ultrasonic (power 120W) vibration. Add 2 mL of copper hexafluorosilicate solution dropwise at a rate of 0.2 mL / s while stirring, the concentration of copper hexafluorosilicate solution is 0.15 mol / L, copper hexafluorosilicate and 4,4'-dipyridyl The molar ratio of disulfide is 1:2 (slight excess of ligand). The resulting mixed solution was continuously stirred at 35° C. for 48 h. After the reaction was completed, the mixture was filtered to obtain a blue powder, which was washed three times with anhydrous methanol to obtain a fluorosilicate porous hybrid material product.

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Abstract

The invention relates to the technical field of industrial gas separation, in particular to a fluosilicate porous hybrid material and a preparation method and application thereof. The structural general formula of the fluosilicate porous hybrid material is [Cu(dpds)2(SiF6)]n, and dpds is 4,4'-dipyridyl disulfide. A metal salt used by the fluosilicate porous hybrid material is copper hexafluorosilicate, the organic ligand is 4,4'-dipyridyl disulfide, and the fluosilicate porous hybrid material is an anionic pillared metal organic framework material with a proper pore diameter and a proper fluorination functional site; the preparation method is low in raw material price, cost-saving, simple to operate, easy to control conditions and easy to industrialize; and the fluosilicate porous hybrid material provided by the invention has appropriate pore diameter and fluorinated functional sites, can enhance the recognition of acetylene through the action of hydrogen bonds, can separate C2H2 / C2H4mixed gas and / or C2H2 / CO2 mixed gas at the same time, and has higher separation selectivity, larger adsorption capacity and higher separation performance than most existing solid adsorption materials.

Description

technical field [0001] The invention relates to the technical field of industrial gas separation, in particular to a fluorosilicate porous hybrid material and its preparation method and application. Background technique [0002] Ethylene and acetylene are basic chemical raw materials widely used in the production of synthetic chemical products such as synthetic fibers, rubber and plastics. However, due to its industrial production process, ethylene feed gas usually contains about 1% acetylene impurity, which may cause serious troubles in the next polymerization reaction. Because the presence of acetylene will deactivate the catalyst for ethylene polymerization, thereby reducing the quality of polyethylene. In addition, acetylene readily forms explosive metal acetylides. Therefore, it is necessary to control the content of acetylene in ethylene to a certain level (<40ppm) before use. [0003] Existing methods include solvent absorption of acetylene and selective catalyt...

Claims

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Application Information

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IPC IPC(8): B01J20/28B01J20/22B01D53/02C07C11/04
CPCB01J20/28054B01J20/226B01D53/02C07C7/12B01D2257/504B01D2256/24Y02P20/50Y02C20/40
Inventor 胡军李鑫温慧敏
Owner ZHEJIANG UNIV OF TECH
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