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Preparation method and application of zirconium-based metal-organic complex UiO-66/foam carbon composite material

A technology of organic complexes and composite materials, which is applied in the field of preparation of zirconium-based metal-organic complex UiO-66/foamed carbon composite materials, can solve the problems of reduced specific surface area of ​​adsorbents, affecting adsorption performance, and reduced durability. Easy to separate and recover, fast mass transfer rate, avoid aggregation effect

Inactive Publication Date: 2019-01-18
HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, the adsorption technology has the following technical defects: the specific surface area of ​​the adsorbent is reduced due to the agglomeration of the adsorbent caused by the long-term reaction, and the durability of the use is reduced, thereby affecting the adsorption performance; the adsorbent is dispersed in the treated water and is difficult to recover.

Method used

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  • Preparation method and application of zirconium-based metal-organic complex UiO-66/foam carbon composite material
  • Preparation method and application of zirconium-based metal-organic complex UiO-66/foam carbon composite material
  • Preparation method and application of zirconium-based metal-organic complex UiO-66/foam carbon composite material

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Embodiment 1

[0026] A kind of preparation method of zirconium-based metal-organic complex UiO-66 / foam carbon composite material, with ZrCl 4 As the metal source, terephthalic acid as the ligand, and adding foam carbon, adopts one-step hydrothermal synthesis, which specifically includes the following steps:

[0027] (1) Cut the melamine sponge into blocks, the size of which is 1.5cm×3cm×5cm, and put it in N 2 Calcined at 750°C for 1.5h in an atmospheric tube furnace, and acidified with 2.5mol / L nitric acid at 115°C for 1.5h to obtain foam carbon;

[0028] (2) 0.45mmol ZrCl 4 and 0.45mmol terephthalic acid were added to N,N-dimethylformamide, wherein every 1mmol of terephthalic acid used 60ml of N,N-dimethylformamide, followed by adding glacial acetic acid and stirring for 25min, wherein The molar ratio of terephthalic acid to glacial acetic acid is 1:8, and ZrCl is added to it 4 Foam carbon with 10% mass was treated with ultrasonic mixing for 25 minutes; then the mixed solution was put i...

Embodiment 2

[0030] A kind of preparation method of zirconium-based metal-organic complex UiO-66 / foam carbon composite material, with ZrCl 4 As the metal source, terephthalic acid as the ligand, and adding foam carbon, adopts one-step hydrothermal synthesis, which specifically includes the following steps:

[0031] (1) Cut the melamine sponge into blocks, the size of which is 1.5cm×3cm×5cm, and put it in N 2 Calcined at 800°C for 2h in a tubular furnace in the atmosphere, and acidified with 3.0mol / L nitric acid at 120°C for 2h to obtain foam carbon;

[0032] (2) 0.45mmol ZrCl 4 and 0.45 mmol of terephthalic acid were added to N, N-dimethylformamide, wherein 65 ml of N, N-dimethylformamide was used for every 1 mmol of terephthalic acid, followed by adding glacial acetic acid and stirring for 30 min, wherein The molar ratio of terephthalic acid to glacial acetic acid is 1:10, and ZrCl is added to it 4 Foam carbon with 10% mass was ultrasonically mixed for 30 minutes; then the mixed soluti...

Embodiment 3

[0044] A kind of preparation method of zirconium-based metal-organic complex UiO-66 / foam carbon composite material, with ZrCl 4 As the metal source, terephthalic acid as the ligand, and adding foam carbon, adopts one-step hydrothermal synthesis, which specifically includes the following steps:

[0045] (1) Cut the melamine sponge into blocks, the size of which is 1.5cm×3cm×5cm, and put it in N 2 Calcined at 850°C for 2.5h in a tubular furnace in the atmosphere, and acidified with 3.5mol / L nitric acid at 125°C for 2.5h to obtain foam carbon;

[0046] (2) 0.45mmol ZrCl 4 and 0.45 mmol of terephthalic acid were added to N, N-dimethylformamide, wherein 70 ml of N, N-dimethylformamide was used for every 1 mmol of terephthalic acid, followed by adding glacial acetic acid and stirring for 35 minutes, wherein The molar ratio of terephthalic acid to glacial acetic acid is 1:12, and ZrCl is added to it 4 Foam carbon with 10% mass was ultrasonically mixed for 35 minutes; then the mixe...

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Abstract

The invention discloses a preparation method of a zirconium-based metal-organic complex UiO-66 / foam carbon composite material. According to the preparation method, ZrCl4 is utilized as a metal source,terephthalic acid is utilized as ligand, foam carbon is added, and one-step hydrothermal synthesis is utilized. The preparation method specifically comprises the following operation steps: (1) cutting tripolycyanamide sponge into blocks, putting into an N2 atmosphere tubular furnace to be calcined and utilizing nitric acid to acidify the sponge to obtain foam carbon; (2) adding ZrCl4 and he terephthalic acid into N,N-dimethyl formamide, then adding glacial acetic acid to be stirred, then adding the foam carbon of 10% of the mass of ZrCl4 and performing ultrasonic mixing treatment; then putting a mixed solution into a reaction kettle to be reacted, cooling to the room temperature, cleaning a reaction product and vacuum drying to obtain the zirconium-based metal-organic complex UiO-66 / foamcarbon composite material. The composite material prepared by the preparation method disclosed by the invention can quickly, efficiently and selectively remove fluorine ions in a water body and further is convenient to separate and recycle.

Description

technical field [0001] The invention belongs to the technical field of water body pollutant removal, and in particular relates to a preparation method and application of a zirconium-based metal-organic complex UiO-66 / foam carbon composite material. Background technique [0002] Fluoride-containing groundwater is considered to be one of a series of serious problems worldwide. The World Health Organization believes that in addition to arsenic and nitrate, fluoride is one of the pollutants in human drinking water, and the concentration of fluoride in groundwater in many regions is gradually increasing. Fluorine pollution mainly comes from natural geological activities and human activities. Natural geological activities include the dissolution of fluorine-containing mineral rocks, marine substances, and volcanic eruptions, while human activities include electroplating, coal-fired power stations, extraction plants, brick factories, iron factories, aluminum Plants, semiconductor m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30C02F1/28C02F103/06C02F101/14
CPCB01J20/20B01J20/223B01J20/28045C02F1/288C02F2101/14C02F2103/06
Inventor 张云霞谢东华秦文秀张海民汪国忠赵惠军
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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