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A method for synthesizing rare earth-heteropolyacid coordination polymers with heteropolyacid ligands

A technology of coordination polymers and heteropolyacids, which is applied in chemical instruments and methods, fluorescence/phosphorescence, instruments, etc., can solve the problems of low precision and sensitivity, achieve good luminescence performance, excellent channel characteristics, and overcome poor portability. convenient effect

Inactive Publication Date: 2019-03-01
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The purpose of the present invention is to overcome the problems and defects of low precision and sensitivity when the content of methanol in the determination sample is not high enough, prepare a rare earth-heteropolyacid coordination polymer with simple operation, good selectivity and high sensitivity, and provide rare earth-heteropolyacid coordination polymers. Preparation method of heteropolyacid coordination polymer

Method used

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  • A method for synthesizing rare earth-heteropolyacid coordination polymers with heteropolyacid ligands
  • A method for synthesizing rare earth-heteropolyacid coordination polymers with heteropolyacid ligands
  • A method for synthesizing rare earth-heteropolyacid coordination polymers with heteropolyacid ligands

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Embodiment 1

[0033] A method for synthesizing rare earth-heteropolyacid coordination polymers with heteropolyacid ligands, comprising the following steps:

[0034] The first step: heteropolyacid ligand (NH 4 ) 4 [(C 6 h 5 PO 3 )2 Mo 5 o 15 ]·5H 2 Preparation of O

[0035] Weigh 9.7g of ammonium heptamolybdate powder and 3.9g of phenylphosphoric acid in a beaker, add 65mL of water, the proportion of ammonium heptamolybdate to water is 15%, and the proportion of phenylphosphoric acid to water is 6%, heat the solution until its volume decreases to 40-45mL, cooled to room temperature, and filtered the slightly turbid solution after cooling. As the clear solution evaporates in air, large crystals separate out. Finally, the crystals were collected by filtration. The crystals were rinsed twice quickly with distilled water and dried in air. The yield of the compound is 12.1 g, and the yield is 92%;

[0036] Step 2: Crystal Preparation

[0037] Weigh a mixed sample of 0.07g of lanthanu...

Embodiment 2

[0041] A method for synthesizing rare earth-heteropolyacid coordination polymers with heteropolyacid ligands, comprising the following steps:

[0042] The first step: heteropolyacid ligand (NH 4 ) 4 [(C 6 h 5 PO 3 ) 2 Mo 5 o 15 ]·5H 2 Preparation of O

[0043] Weigh 10.4g of ammonium heptamolybdate powder and 4.5g of phenylphosphoric acid in a beaker, add 65mL of water, the proportion of ammonium heptamolybdate to water is 16%, and the proportion of phenylphosphoric acid to water is 7%, heat the solution until its volume decreases to 40-45mL, cooled to room temperature, and filtered the slightly turbid solution after cooling. As the clear solution evaporates in air, large crystals separate out. Finally, the crystals were collected by filtration. The crystals were rinsed twice quickly with distilled water and dried in air. Compound yield is 12.4g, yield rate is 88%;

[0044] Step 2: Crystal Preparation

[0045] Weigh a mixed sample of 0.09g of lanthanum nitrate an...

Embodiment 3

[0049] A method for synthesizing rare earth-heteropolyacid coordination polymers with heteropolyacid ligands, comprising the following steps:

[0050] The first step: heteropolyacid ligand (NH 4 ) 4 [(C 6 h 5 PO 3 ) 2 Mo 5 o 15 ]·5H 2 Preparation of O

[0051] Weigh 11.0g of ammonium heptamolybdate powder and 4.9g of phenylphosphoric acid in a beaker, add 65mL of water, the proportion of ammonium heptamolybdate to water is 17%, and the proportion of phenylphosphoric acid to water is 7.5%, heat the solution until its volume decreases to 40-45mL, cooled to room temperature, and filtered the slightly turbid solution after cooling. As the clear solution evaporates in air, large crystals separate out. Finally, the crystals were collected by filtration. The crystals were rinsed twice quickly with distilled water and dried in air. Compound yield is 13.4g, yield rate is 89%;

[0052] Step 2: Crystal Preparation

[0053] Weigh a mixed sample of 0.1g of lanthanum nitrate a...

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Abstract

The invention discloses a method for synthesizing a rare earth-heteropolyacid coordination polymer by means of a heteropolyacid ligand, and belongs to the field of new technology material synthesis. Ammonium heptamolybdate and phenyl phosphate serve as the raw materials, and lanthanum nitrate, isonicotinic acid and terbium nitrate serve as auxiliary synthesis materials. The preparation method of the coordination polymer comprises the main steps of preparation of the heteropolyacid ligand, crystal synthesis and ion exchange. The defects that the precision and sensitivity are low when the content of methanol in a measured sample is not high enough are overcome, the rare earth-heteropolyacid coordination polymer which is easy to operate, good in selectivity and high in sensitivity is prepared, a methanol detection means which is simple, efficient and low in cost is developed, and a new field is created for detection of methanol.

Description

technical field [0001] The invention belongs to the field of synthesis of new technology materials, and relates to a rare earth-heteropolyacid coordination polymer and a preparation method thereof. Background technique [0002] Methanol is highly toxic and has the greatest impact on the nervous system and blood system of the human body. It will produce toxic reactions if it is ingested through the digestive tract, respiratory tract or skin. Methanol vapor can damage human respiratory mucosa and vision. The symptoms of acute poisoning are: headache, nausea, stomach pain, fatigue, blurred vision and even blindness, and then difficulty breathing, eventually leading to paralysis of the respiratory center and death. Chronic poisoning reactions include: dizziness, lethargy, headache, tinnitus, loss of vigor, and digestive disorders. The discharge of industrial wastewater containing methanol into the environment will also cause irreversible damage to the environment. In methanol ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00G01N21/64C09K11/06
CPCC08G83/008C09K11/06C09K2211/183G01N21/6428G01N2021/6432
Inventor 田涛康春莉包思琪
Owner JILIN UNIV
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