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Metal-organic framework material as well as preparation method and application thereof

An organic framework and metal technology, applied in the field of metal-organic framework materials and their preparation, can solve the problems of low specific surface area, poor pollutant removal rate and adsorption capacity, difficult surface modification, etc., and achieve high thermal and chemical stability , Large adsorption capacity and high adsorption rate

Active Publication Date: 2021-06-01
JIANGSU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, such materials have low specific surface area and some difficulties in surface modification, so the removal rate and adsorption capacity of pollutants are poor, and the material performance is not ideal.

Method used

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  • Metal-organic framework material as well as preparation method and application thereof
  • Metal-organic framework material as well as preparation method and application thereof
  • Metal-organic framework material as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Synthesis of organic ligand 4-(3,5-dimethylpyrazol-4-yl)-1,2,4-triazole Hpztr:

[0035] Synthesis of 4-amino-3,5-dimethylpyrazole ligand intermediate: 5.07g, 36mmol of 4-nitro-3,5-dimethylpyrazole and 40.0g KOH were dissolved in 100mL deionized water, Heat it to 90°C in an oil bath, weigh 27.57g, 122mmol of SnCl 2 2H 2 O, added to the above system in three times, the feeding interval is 1 hour, keep the temperature constant, continue to react for 6 hours, cool to room temperature, filter the solid product, wash with 3mL ice water, dry to get 4-amino-3,5 - 2.60 g of dimethylpyrazole ligand intermediate, the yield is about 65%;

[0036] Synthesis of 4-(3,5-dimethylpyrazol-4-yl)-1,2,4-triazole Hpztr ligand: 3.33g, 30mmol of 4-amino-3,5-dimethylpyrazole , 4.69g, 33mmol of N,N'-bis(dimethylaminomethylene)hydrazine and 0.24g, 1.3mmol of p-toluenesulfonic acid were dissolved in 25mL of o-xylene, stirred and refluxed for 24h, after the reaction was completed, the The sy...

Embodiment 2

[0049] (1) Synthesis of organic ligand 4-(3,5-dimethylpyrazol-4-yl)-1,2,4-triazole Hpztr:

[0050] Synthesis of 4-amino-3,5-dimethylpyrazole ligand intermediate: 5.07g, 36mmol of 4-nitro-3,5-dimethylpyrazole and 51.0g KOH were dissolved in 100mL deionized water, Heat it to 90°C in an oil bath, weigh 27.0g of SnCl 2 2H 2 O, added to the above system in three times, the feeding interval is 1 hour, keep the temperature constant, continue to react for 6 hours, cool to room temperature, filter the solid product, wash with 3mL ice water, dry to get 4-amino-3,5 - 2.10 g of dimethylpyrazole ligand intermediate, the yield is about 52%;

[0051] Synthesis of 4-(3,5-dimethylpyrazol-4-yl)-1,2,4-triazole Hpztr ligand: 3.33g, 30mmol of 4-amino-3,5-dimethylpyrazole , 3.50g of N,N'-bis(dimethylaminomethylene)hydrazine and 0.16g of p-toluenesulfonic acid were dissolved in 25mL of o-xylene, stirred and refluxed for 24h, after the reaction was completed, the system was cooled to room temperat...

Embodiment 3

[0059] (1) Synthesis of organic ligand 4-(3,5-dimethylpyrazol-4-yl)-1,2,4-triazole Hpztr:

[0060] Synthesis of 4-amino-3,5-dimethylpyrazole ligand intermediate: 5.07g, 36mmol of 4-nitro-3,5-dimethylpyrazole and 40.0g KOH were dissolved in 100mL deionized water, Heat it to 90°C in an oil bath, weigh 27.57g, 122mmol of SnCl 2 2H 2 O, added to the above system in three times, the feeding interval is 1 hour, keep the temperature constant, continue to react for 6 hours, cool to room temperature, filter the solid product, wash with 3mL ice water, dry to get 4-amino-3,5 - 2.60 g of dimethylpyrazole ligand intermediate, the yield is about 65%;

[0061] Synthesis of 4-(3,5-dimethylpyrazol-4-yl)-1,2,4-triazole Hpztr ligand: 3.33g, 30mmol of 4-amino-3,5-dimethylpyrazole , 4.69g 33mmol of N,N'-bis(dimethylaminomethylene)hydrazine and 0.24g, 1.3mmol of p-toluenesulfonic acid were dissolved in 25mL of o-xylene, stirred and refluxed for 24h, after the reaction was completed, the system ...

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Abstract

The invention discloses a metal-organic framework material as well as a preparation method and application thereof. The chemical formula of the metal-organic framework material is [Cu (btr) 2 (hpztr) 2 (pztr<-1>) 2 (NO3<->) 3] n, wherein Hpztr is 4-(3, 5-dimethylpyrazole-4-yl)-1, 2, 4-triazole, and btr is 4, 4'-bis-1, 2, 4-triazole. The preparation method of the material comprises the following steps of: (1) synthesizing Hpztr; (2) synthesizing btr; (3) dissolving copper salt, Hpztr and btr by using a mixed solvent to obtain a mixed solution; and (4) placing the mixed solution in a constant-temperature drying box at 90-100 DEG C for reaction, cooling to room temperature, filtering, washing and drying to obtain the metal-organic framework material. The material can be applied to removal of ions in water. The material has relatively high thermal stability and chemical stability. Anions in water can be effectively adsorbed and enriched at normal temperature and normal pressure, and particularly, the adsorption rate is high and the adsorption capacity is large. The material can be used as an efficient water purifying adsorbent for removing water from water.

Description

technical field [0001] The present invention relates to a material and its preparation method and application, more specifically, to a metal-organic framework material and its preparation method and application. Background technique [0002] As one of the most precious natural resources on the earth, water is of irreplaceable importance to the survival and development of human beings, animals and plants. However, with the expansion of the scope of human activities and the rapid development of modern industry, water pollution has become increasingly serious and has become a serious problem faced by the whole world. Disposal of industrial waste, discharge of chemical wastewater, leakage of nuclear waste and excessive use of pesticides have introduced various harmful substances into water bodies. Common heavy metal ions in wastewater mainly include arsenic, copper, chromium, lead, mercury, nickel and zinc ions. Excessive levels of these ions will pose a huge threat to the sur...

Claims

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Application Information

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IPC IPC(8): C08G83/00C07F1/00B01J20/22B01J20/30C02F1/28C02F101/22
CPCC08G83/008C07F1/005B01J20/226C02F1/285C02F2101/22
Inventor 高强张艳梅陆楠陈祥陈立庄
Owner JIANGSU UNIV OF SCI & TECH
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