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Metal organic framework and its preparation method and application

A metal-organic framework and reaction technology, which is applied in the field of compounds and their preparation, can solve the problems such as the decrease of the specific surface area and pore size of the adsorbent, the influence of the adsorption and desulfurization performance, and the blockage of the pores, so as to enhance the desulfurization adsorption performance, improve the adsorption and desulfurization performance, and the pore size Increased effect

Active Publication Date: 2021-06-25
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

is the CuCl 2 Loaded on the SBA-15 carrier, and then using ethylene as a reducing agent, the Cu 2+ reduced to Cu + , so that the load is Cu + The adsorbent has high adsorption and selective regeneration of thiophene sulfides in fuel oil, and the Ag + with Cu 2+ Directly introduced into the molecular sieve, but if the ion concentration is too high when using this method, the pores will be blocked, which will reduce the specific surface area and pore size of the adsorbent and affect the adsorption and desulfurization performance.

Method used

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  • Metal organic framework and its preparation method and application
  • Metal organic framework and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0040] 1. Preparation of metal-organic frameworks

[0041] Mix copper chloride dihydrate and trimesic acid in 500mL polytetrafluoroethylene liner, stir at room temperature for 5 hours, add N,N-dimethylacetamide, the molar ratio of the three is 2:1:0.1, and stir Mix evenly until all the solids are dissolved, put the liner into the autoclave, react at 100°C for 48 hours to obtain the reaction mother liquor, after cooling to room temperature, filter and wash with ethanol, and dry in vacuum to obtain Cu-BTC-DMA;

[0042] Under light-shielded conditions, dissolve Cu-BTC-DMA in silver nitrate acetonitrile solution with a concentration of 0.01mol / L, stir at room temperature under light-shielded environment, and the reaction time is 6h. °C for 24 hours in vacuum to obtain the metal-organic framework Ag@Cu-BTC-DMA.

[0043] 2. Detection of metal organic framework

[0044] The mass percentage of Ag ions measured by inductively coupled plasma mass spectrometry ICP is 3.95%; figure 2 ...

Embodiment 2

[0048] 1. Preparation of metal-organic frameworks

[0049] Mix copper chloride dihydrate and trimesic acid in 500mL polytetrafluoroethylene liner, stir at room temperature for 2 hours, add N,N-dimethylacetamide, the molar ratio of the three is 2.25:1.25:0.25, and stir Mix evenly until the solids are completely dissolved, put the liner into the high-pressure reactor, react at 120°C for 72 hours to obtain the reaction mother liquor, cool to room temperature, filter with suction, dry in vacuum, and wash with N,N-dimethylacetamide to obtain Cu-BTC-DMA;

[0050] Under dark conditions, dissolve Cu-BTC-DMA in silver nitrate acetonitrile solution with a concentration of 0.03mol / L, stir at room temperature under dark conditions, and the reaction time is 12h. °C under vacuum to obtain the metal-organic framework Ag@Cu-BTC-DMA.

[0051] 2. Detection of metal organic framework

[0052] The mass percentage of Ag ions measured by inductively coupled plasma mass spectrometry ICP is 3.66%;...

Embodiment 3

[0056] 1. Preparation and application of metal-organic frameworks

[0057] Mix copper chloride dihydrate and trimesic acid in 500mL polytetrafluoroethylene liner, stir at room temperature for 4 hours, add N,N-dimethylacetamide, the molar ratio of the three is 2.5:1.5:0.5, and stir Mix evenly until all the solids are dissolved, put the liner into the autoclave, react at 100°C for 48 hours to obtain the reaction mother liquor, cool to room temperature, filter with suction, wash, vacuum dry, and wash with methanol with suction to obtain Cu-BTC-DMA;

[0058] Under light-shielded conditions, dissolve Cu-BTC-DMA in silver nitrate acetonitrile solution with a concentration of 0.02mol / L, stir at room temperature under light-shielded environment, and the reaction time is 8h. ℃ vacuum drying for 24h, the metal organic framework Ag@Cu-BTC-DMA was obtained.

[0059] 2. Detection of metal organic framework

[0060] Inductively coupled plasma mass spectrometry ICP measured the mass percen...

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Abstract

The invention provides a metal organic framework and its preparation method and application, the molecular formula of the metal organic framework is: Ag@[(Cu 4 Cl) 3 (BTC) 8 ] · 9DMA, wherein the mass percentage of Ag in the metal-organic framework is 3.66-4.27%. The present invention adopts the hydrothermal synthesis method to synthesize Cu-BTC-DMA, and the reaction method is more severe than the traditional reflux reaction, which can make the synthesis more sufficient, the yield higher, and the crystal structure more complete; the silver ion exchange reaction is used to modify Cu-BTC-DMA ‑BTC‑DMA, at low concentrations of AgNO 3 The ion exchange reaction in acetonitrile solution for a certain period of time can avoid the strong oxidizing AgNO 3 Destroy the structure of Cu‑BTC‑DMA and enhance the desulfurization adsorption performance of Ag@Cu‑BTC‑DMA to thiophene.

Description

technical field [0001] The invention relates to a compound and its preparation method and application, in particular to an organic metal skeleton, its preparation method and its application in π-complex adsorption desulfurization. Background technique [0002] With the shortage of petroleum resources and the limitation of sulfur content in fuel oil in various countries in the world, the development of environmentally friendly and energy-saving deep desulfurization adsorbents is one of the hotspots of research. Fuel oil contains two types of sulfides, one is highly active components such as mercaptans, sulfides and disulfides, which are easy to remove; the other is thiophene, benzothiophene, dibenzo Thiophene and its derivatives are difficult to remove. In fact, the traditional hydrodesulfurization method has a good removal effect on mercaptans, sulfides and disulfides, but has a poor removal effect on thiophene, benzothiophene, dibenzothiophene and their derivatives, and ca...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/22B01J20/30C10G25/00
CPCB01J20/0233B01J20/0296B01J20/226C10G25/003C10G2300/202
Inventor 曾勇平曹亚南李凯
Owner YANGZHOU UNIV
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