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Bispyrazole functionalized lead imprinted fdu-12 material and its preparation method and application

A FDU-12, functionalized technology, applied in the field of mesoporous materials, can solve the problems of low selective adsorption of Pb(II), weak anti-interference ability of coexisting ions, poor regeneration ability of materials, etc., and achieve good chemical stability , improved selectivity, good effect

Active Publication Date: 2020-09-08
上海海关工业品与原材料检测技术中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical problem to be solved by the present invention is to overcome the disadvantages of poor adsorption stability, low selective adsorption to Pb(II), weak anti-interference ability to coexisting ions, and poor material regeneration ability of the adsorption materials in the prior art. Defects, providing a bispyrazole functionalized lead imprinted FDU-12 material and its preparation method and application

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  • Bispyrazole functionalized lead imprinted fdu-12 material and its preparation method and application
  • Bispyrazole functionalized lead imprinted fdu-12 material and its preparation method and application
  • Bispyrazole functionalized lead imprinted fdu-12 material and its preparation method and application

Examples

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Effect test

Embodiment 1

[0066] Synthesis of bispyrazole-functionalized lead imprinted MCM-41 material (namely Pb-IIMS-MCM-41)

[0067] Dissolve 1 mmol of lead complex (0.811 g) in 80 mL of tetrahydrofuran under stirring, and add 1 mmol of anhydrous K to the solution 2 CO 3 (0.138g). After two hours, 1 mmol (0.247 g) of TEPIC was added dropwise to the solution. The whole mixture was heated at reflux at 65°C for 12 hours and the solvent was dried under vacuum. The obtained solid was dissolved in 20 mL of toluene, then 973 mg of MCM-41 was added, and the mixture was heated under reflux at 110° C. for 48 hours. After filtration and vacuum drying, the obtained solid was repeatedly washed with dichloromethane, distilled water, ethanol and ethyl acetate, and then dried to obtain a white solid substance. Use 10mL for every 5mg of Pb(II) ion imprinting material, 3mol L -1 HCl washes to elute template lead. After drying, a Pb(II) ion-imprinted mesoporous silica material, namely Pb-IIMS-MCM-41, was obtain...

Embodiment 2

[0071] Synthesis of bispyrazole-functionalized lead-imprinted SBA-15 material (namely Pb-IIMS-SBA-15)

[0072] Dissolve 1 mmol of lead complex (0.811 g) in 80 mL of tetrahydrofuran under stirring, and add 1 mmol of anhydrous K to the solution 2 CO 3 (0.138g). After two hours, 1 mmol (0.247 g) of TEPIC was added dropwise to the solution. The whole mixture was heated at reflux at 65°C for 12 hours and the solvent was dried under vacuum. The obtained solid was dissolved in 20 mL of toluene, then 973 mg of SBA-15 was added, and the mixture was heated under reflux at 110° C. for 48 hours. After filtration and vacuum drying, the obtained solid was repeatedly washed with dichloromethane, distilled water, ethanol and ethyl acetate, and then dried to obtain a white solid substance. Use 10mL for every 5mg of Pb(II) ion imprinting material, 3mol L -1 HCl washes to elute template lead. After drying, a Pb(II) ion-imprinted mesoporous silica material, namely Pb-IIMS-SBA-15, was obtain...

Embodiment 3

[0076] Synthesis of bispyrazole-functionalized lead-imprinted FDU-12 material (namely Pb-IIMS-FDU-12)

[0077] Dissolve 1 mmol of lead complex (0.811 g) in 80 mL of tetrahydrofuran under stirring, and add 1 mmol of anhydrous K to the solution 2 CO 3 (0.138g). After two hours, 1 mmol (0.247 g) of TEPIC was added dropwise to the solution. The whole mixture was heated at reflux at 65°C for 12 hours and the solvent was dried under vacuum. The obtained solid was dissolved in 20 mL of toluene, then 973 mg of FDU-12 was added, and the mixture was heated under reflux at 110° C. for 48 hours. After filtration and vacuum drying, the obtained solid was repeatedly washed with dichloromethane, distilled water, ethanol and ethyl acetate, and then dried to obtain a white solid substance. Use 10mL for every 5mg of Pb(II) ion imprinting material, 3mol L -1 HCl washes to elute template lead. After drying, a Pb(II) ion-imprinted mesoporous silica material, namely Pb-IIMS-FDU-12, was obtain...

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Abstract

The invention discloses a bis-pyrazol functional lead-imprinted FDU-12 material as well as a preparation method and application thereof. The preparation method comprises the following steps: adding TEPIC into a mixture of a DPP lead complex, alkali and tetrahydrofuran, heating for reflux, completely extracting a solvent under a vacuum state, adding toluene and a mesoporous material FDU-12 for reaction, and carrying out acid pickling to remove lead, so as to obtain the bis-pyrazol functional lead-imprinted FDU-12 material. The bis-pyrazol functional lead-imprinted FDU-12 material disclosed by the invention has high selective adsorbability to lead ions, strong disturbance resistance to co-existing ions and strong regeneration capacity. A developed detection method has the advantages of highdetection precision, good precision and high detection efficiency.

Description

technical field [0001] The invention relates to the field of mesoporous materials, in particular to a bispyrazole functionalized lead imprinted FDU-12 material, a preparation method and an application. Background technique [0002] Lead is a heavy metal element that seriously threatens the physiological health of the human body. It has serious harm to the digestive system, central nervous system, especially the liver and urinary system of the organism. The toxicity of lead to the human body is cumulative. Lead can be enriched in the food chain through polluted aquatic products and crops, causing harm to the human body. Therefore, the enrichment and separation of trace lead elements in water is an essential link in the treatment and analysis of lead-containing wastewater, and has received widespread attention. [0003] Ion imprinted technique (IIT) is a new technology developed on the basis of molecular imprinted technology in recent years, integrating the advantages of many...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30B01D15/08C02F1/28G01N21/73C02F101/20
CPCB01D15/08B01J20/103B01J20/22B01J20/28083C02F1/285C02F2101/20G01N21/73
Inventor 刘曙沈康俊蔡婧
Owner 上海海关工业品与原材料检测技术中心