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Alkali metal cation doping-based NH1-MIL-125 (Ti) material and preparation method thereof

A technology of NH2-MIL-125 and alkali metal cations, applied in the direction of alkali metal compounds, alkali metal oxides/hydroxides, chemical instruments and methods, etc., can solve the problem of unstable impregnation environment, large influence on samples, and preparation cycle Long and other problems, to achieve the effect of shortening the synthesis time, increasing the reaction temperature, and improving the purity

Active Publication Date: 2018-08-17
CHANGAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, at present, the preparation cycle of aminated MIL-125(Ti) is long and the efficiency is low, and the post-functional impregnation method is usually used for alkali metal doping, which limits the effect of doping to a certain extent, and the impregnation environment is limited. Unstable, great influence on the sample

Method used

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  • Alkali metal cation doping-based NH1-MIL-125 (Ti) material and preparation method thereof
  • Alkali metal cation doping-based NH1-MIL-125 (Ti) material and preparation method thereof
  • Alkali metal cation doping-based NH1-MIL-125 (Ti) material and preparation method thereof

Examples

Experimental program
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Embodiment 1

[0042] Step 1) The solute ratio in the solvent is 8g / mL, and the volume ratio of 45% N,N-dimethylformamide and 55% methanol is stirred at room temperature for 10 minutes to obtain a mixed organic solvent;

[0043] Step 2) Weighing 2-aminoterephthalic acid with a mass fraction of 56 wt%, slowly adding it to the prepared organic solvent, and stirring for 20 minutes to obtain a mixed solution of nitrogen-containing ligands;

[0044] Step 3) adding the dry chlorine salt containing alkali metal cations, lithium chloride with a mass fraction of 1 wt% to the solvent prepared in step 2, and stirring at room temperature for 20 min to obtain a mixed solution containing alkali metal cations and nitrogen ligands ;

[0045] Step 4) Slowly add 43wt% titanium isopropoxide into the mixed solution under the condition of ice-water bath, and the stirring time is 30 minutes to obtain a uniformly mixed reddish-brown liquid;

[0046] Step 5) Transfer the uniformly stirred mixture into a 40mL polyt...

Embodiment 2

[0048] Step 1) The solute ratio in the solvent is 8g / mL, and the volume ratio of 45% N,N-dimethylformamide and 55% methanol is stirred at room temperature for 10 minutes to obtain a mixed organic solvent;

[0049] Step 2) Weighing 2-aminoterephthalic acid with a mass fraction of 56 wt%, slowly adding it to the prepared organic solvent, and stirring for 20 minutes to obtain a mixed solution of nitrogen-containing ligands;

[0050] Step 3) adding the dry chloride salt containing alkali metal cations, sodium chloride with a mass fraction of 1 wt% to the solvent prepared in step 2, and stirring at room temperature for 20 min to obtain a mixed solution containing alkali metal cations and nitrogen ligands ;

[0051] Step 4) Slowly add 43wt% titanium isopropoxide into the mixed solution under the condition of ice-water bath, and the stirring time is 30 minutes to obtain a uniformly mixed reddish-brown liquid;

[0052] Step 5) Transfer the uniformly stirred mixture into a 40mL polyte...

Embodiment 3

[0054] Step 1) The solute ratio in the solvent is 8g / mL, and the volume ratio of 45% N,N-dimethylformamide and 55% methanol is stirred at room temperature for 10 minutes to obtain a mixed organic solvent;

[0055] Step 2) Weighing 2-aminoterephthalic acid with a mass fraction of 55wt%, slowly adding it into the prepared organic solvent, and stirring for 20 minutes to obtain a mixed solution of nitrogen-containing ligands;

[0056] Step 3) adding the dry chlorine salt containing alkali metal cations, lithium chloride with a mass fraction of 2wt% to the solvent prepared in step 2, and stirring at room temperature for 20 min to obtain a mixed solution containing alkali metal cations and nitrogen ligands ;

[0057] Step 4) Slowly add 43wt% titanium isopropoxide into the mixed solution under the condition of ice-water bath, and the stirring time is 30 minutes to obtain a uniformly mixed reddish-brown liquid;

[0058] Step 5) Transfer the uniformly stirred mixture into a 40mL polyt...

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Abstract

The invention discloses an alkali metal cation doping-based NH1-MIL-125 (Ti) material and a preparation method thereof. The alkali metal cation doping-based NH1-MIL-125 (Ti) material is prepared by heating in oven, activating through organic solvent, centrifuging, washing and drying 2-aminoterephthalic acid, isopropyl titanate, lithium chloride, sodium chloride, N, N-dimethyl formamide and methylalcohol under neural conditions. The specific surface area range of the alkali metal cation doping-based NH1-MIL-125 (Ti) material is 808.138-1470.044 m<2> / g<-1>. The preparation method of the alkalimetal cation doping-based NH1-MIL-125 (Ti) material comprises 1) preparation of organic solvent, 2) doping of nitrogen-containing ligands, 3) doping of alkali metal cations, 4) doping of metal centerand 5) preparation of the alkali metal cation doping-based NH1-MIL-125 (Ti) material. Compared with the shortcomings of low reaction time and poor microwave synthesizing precision in the prior art, the alkali metal cation doping-based NH1-MIL-125 (Ti) material has the outstanding advantage of increasing the reaction temperature through a solvothermal method to achieve synthesis within a short time, and adopting a simple alkali metal cation doping method to greatly increase the specific surface area, thereby having a broad application prospect in the field of metal-organic frameworks.

Description

technical field [0001] The invention belongs to the technical field of metal-organic framework materials, and in particular relates to an alkali metal cation-doped NH 2 -MIL-125(Ti) material and its preparation method. Background technique [0002] With the rapid economic growth, the impact of "greenhouse gas" emissions on the global climate has become a serious problem, among which CO 2 The emission problem is the most prominent. Metal-based organic frameworks (MOFs) are a class of solid adsorbents with great potential, and they are a class of porous materials with excellent coordination, structural diversity, and physical and chemical properties. The development of MOFs can be traced back to 1897. It was not until 1990, when Robison and Hoskins systematically reported the structure design method of coordination polymers, and Kitagawa’s research group reported the gas adsorption properties of porous coordination polymers, that MOFs received everyone’s attention. extensiv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30C08G83/00
CPCB01J20/226B01J20/28064B01J20/28066B01J20/28071B01J20/2808B01J20/28083C08G83/008
Inventor 宋莉芳薛程夏慧芸安鑫孙增智高莉宁陈华鑫
Owner CHANGAN UNIV
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