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Mesoporous Zr-based coordination polymer and preparation method and application thereof

A coordination polymer and mesoporous technology, applied in water pollutants, other chemical processes, water/sludge/sewage treatment, etc., can solve problems such as difficulty in increasing the adsorption capacity of adsorbents, complicated preparation process, and environmental pollution. Achieve the effect of high yield, simple preparation method and large specific surface area

Active Publication Date: 2017-12-26
山西立铂隆新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, at present, Zr-based porous coordination polymers are mostly synthesized in organic solvents, such as DMF. The preparation process is relatively complicated, the cost is high, and it will cause further pollution to the environment, and the obtained materials are microporous materials, so it is difficult to increase the adsorption capacity of the adsorbent.

Method used

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  • Mesoporous Zr-based coordination polymer and preparation method and application thereof
  • Mesoporous Zr-based coordination polymer and preparation method and application thereof
  • Mesoporous Zr-based coordination polymer and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0040] 0.114 grams of terephthalic acid and 0.16 grams of ZrCl 4 Disperse in 50 ml of polytetrafluoroethylene liner containing 20 ml of ultrapure water, then put it into a reaction kettle, and react in an oven at a reaction temperature of 120° C. for 24 hours. After the reaction, cool down to room temperature naturally, wash repeatedly three times with saturated triethylamine aqueous solution and absolute ethanol, and vacuum-dry in a vacuum oven at 60°C for 24 hours to obtain the Zr-based coordination polymer with an average pore size of 3.8 nm, the specific surface area is 157m 2 / g.

Embodiment 2

[0042] 0.114 grams of terephthalic acid and 0.055 grams of sodium hydroxide, and 0.16 grams of ZrCl 4 Dissolve each in 10mL of ultra-pure water, then mix the two solutions and stir well, then put them into a 50mL polytetrafluoroethylene liner and put them in a reaction kettle, and react in an oven at a reaction temperature of 120°C for 12h . After the reaction, cool down to room temperature naturally, then wash repeatedly with saturated triethylamine aqueous solution and ethanol several times, and vacuum-dry in a vacuum oven at 60°C for 24 hours to obtain the Zr-based coordination polymer with an average pore size of 3.7nm , the specific surface area is 135m 2 / g.

Embodiment 3

[0044] 0.114 grams of terephthalic acid and 0.055 grams of sodium hydroxide, and 0.16 grams of ZrCl 4 Each was dissolved in 10 mL of ultrapure water, and then the two solutions were mixed and fully stirred at room temperature for 24 h. After the reaction, it was naturally cooled to room temperature, then repeatedly washed with saturated triethylamine aqueous solution and ethanol for several times, and vacuum-dried in a vacuum oven at 60°C for 24 hours to obtain the Zr-based coordination polymer. Its scanning electron microscope picture The resulting product was shown to be an aggregate composed of 500 nm particles (see figure 1 ),Infrared spectra( figure 2 A) show that institute's product is terephthalic acid and ZrCl The coordination polymer that forms through coordination, powder X-ray diffraction pattern ( figure 2 B) shows that the product is amorphous, and the thermogravimetric curve ( image 3 ) shows that the ratio between terephthalic acid and Zr is about 1:1; N ...

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Abstract

The invention relates to a mesoporous Zr-based coordination polymer, the coordination polymer is a mesoporous material, the average aperture is 3.8-6 nm, and the specific surface area is 125-157 m<2> / g. A preparation method comprises the following steps: respectively preparing a ZrCl4 aqueous solution and an aqueous solution of terephthalic acid and alkali (or organic amine), mixing the components to obtain a sample system, reacting the sample system for 1-24 h, performing centrifugation, using triethylamine and acetone for repeatedly washing for 2-3 times in order, and performing vacuum drying for 12 h at the temperature of 60 DEG C to obtain the mesoporous Zr-based coordination polymer. The mesoporous Zr-based coordination polymer has the characteristics of high specific surface area and meso pore, the preparation method has the advantages of simple process, no pollution, and high yield, and is suitable for large-scale production. The mesoporous Zr-based coordination polymer has high adsorption quantity on a dye (methylene blue and methyl orange) and heavy metal ions (Fe<3+>, Co<2+>, Ni<2+> and Cu<2+>), is reusable, and can still reach 93.4% of the primary adsorption quantity after 5-time repetition.

Description

(1) Technical field [0001] The invention relates to a mesoporous Zr-based coordination polymer, a preparation method thereof, and an application thereof as an adsorbent. (2) Background technology [0002] Sewage treatment, especially the treatment of organic dyes and heavy metals, is an urgent problem in the field of environmental protection. Adsorption methods are widely used due to their simple operation, small amount of sample and low cost. Commonly used adsorbents include activated carbon and porous coordination polymers. The latter has the characteristics of high surface area, adjustable composition and pore size, and has attracted great attention at home and abroad in recent years. Porous coordination polymers generally refer to coordination polymers with single-size and shape cavities obtained from transition metal ions or metal clusters and organic ligands by means of molecular assembly and crystal engineering. Among them, Zr-based porous coordination polymers have...

Claims

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Application Information

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IPC IPC(8): B01J20/26B01J20/30C02F1/28C02F101/20C02F101/30
CPCB01J20/264C02F1/285C02F2101/20C02F2101/308
Inventor 霍甲金硼李兴月王双印
Owner 山西立铂隆新材料有限公司
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