Titanium-based coordination compound crystalline material based on thiacalix[4]arene, and preparation method thereof, and application in light degradation of methylene blue

A technology of methylene blue and thiacalix, applied in titanium organic compounds, organic compound/hydride/coordination complex catalysts, 4/14 group organic compounds without C-metal bonds, etc., can solve Heinz body anemia, Changes in red blood cell morphology, necrotic thickening, etc.

Active Publication Date: 2020-10-20
XUZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although methylene blue has a good curative effect in many aspects, when the dose of methylene blue is too high, it can cause Heinz body anemia, changes in the shape of red blood cells, and necrotic thick swelling.

Method used

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  • Titanium-based coordination compound crystalline material based on thiacalix[4]arene, and preparation method thereof, and application in light degradation of methylene blue
  • Titanium-based coordination compound crystalline material based on thiacalix[4]arene, and preparation method thereof, and application in light degradation of methylene blue
  • Titanium-based coordination compound crystalline material based on thiacalix[4]arene, and preparation method thereof, and application in light degradation of methylene blue

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1 Preparation method of titanium-based complex crystalline material

[0026] Weigh 36mg (0.05mmol) thiacalix [4] arene p-tert-butylthiacalix [4] arene (abbreviated as H 4 BTC4A), 21mg (0.3mmol) lithium nitrate and 0.5mL (5mmol) isopropyl titanate in a polytetrafluoroethylene liner, add 5ml N,N-dimethylacetamide and 1mL ethanol to this mixture, ultrasonic After mixing evenly for 0.5 hours, put the polytetrafluoroethylene liner in the stainless steel reactor jacket and tighten it, put it in a constant temperature oven at 80°C for 5 days, take it out and let it cool down to room temperature naturally, open the polytetrafluoroethylene liner to get a yellow block Transparent crystals. Rinse the crystals with distilled water, collect the crystals by filtration, and dry them at room temperature to obtain a titanium-based complex crystalline material based on thiacalix[4]arene, whose molecular formula is [Ti 4 (BTC4A)(OH - ) 4 (EtO - ) 6 ( i PrO - ) 2 ].

Embodiment 2

[0027] Example 2 Structural characterization of titanium-based complex crystalline materials

[0028] The crystal structure of the target material is obtained by analyzing the X-ray single crystal diffraction data. Single crystal test results show that the target material crystallizes in the monoclinic system P2 1 / c space group. The asymmetric unit contains 2 titanium ions, 2 hydroxyl groups, 3 protonated alcohols, 1 protonated isopropanol and 0.5 thiacalix[4]arene ligand molecules ( figure 1 a). The thiacalix[4]arene shows a rare 1,2-alternating configuration, two titanium ions are coordinated to the thiacalix[4]arene through sulfur and oxygen atoms, and the other two titanium atoms are respectively protonated by ethanol and isopropanol are linked to the above units to form Ti 4 (BTC4A) molecule. Ti 4 (BTC4A) molecules form AB stacks through weak intermolecular interactions ( figure 1 b). For detailed structure information of the target material, please refer to the ...

Embodiment 3

[0029] Embodiment 3 Characterization of thermal stability of titanium-based complex crystalline material

[0030] The characterization of the thermal stability of the target material is to use a thermogravimetric analyzer to heat the sample to 800°C in a nitrogen environment, and judge its stable temperature range through the weight loss during the heating process of the sample. Such as image 3 As shown, the target material gradually loses crystallization solvent molecules and coordination solvent molecules before 372 °C, while the core structure of the target material remains stable. The core structure of the target material starts to collapse after 372°C.

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Abstract

The invention discloses a preparation method of a titanium-based coordination compound crystalline material based on thiacalix[4]arene. The preparation method comprises the following steps: adding a ligand H4BTC4A, lithium nitrate and isopropyl titanate into a mixed solution composed of N,N-dimethylacetamide and ethanol, uniformly mixing, carrying out a heating reaction in a reaction kettle for aperiod of time to obtain a yellow blocky transparent crystal, cleaning, filtering, and airing to obtain the thiacalix[4]arene-based titanium-based coordination compound crystalline material. Accordingto the invention, the titanium-based coordination compound crystalline material is a titanium-based coordination compound based on thiacalix[4]arene, wherein thiacalix[4]arene is coordinated in a rare 1,2-alternating configuration; the titanium-based coordination compound disclosed by the invention has good stability, can be stored in air for a long time, and is low in the forbidden band width; the synthesis method disclosed by the invention is simple and rapid, low in cost, high in yield, high in repeatability and easy for mass production, popularization and use; and the titanium-based coordination compound crystalline material disclosed by the invention can drive methylene blue to be photodegraded under sunlight irradiation, and has important significance in treatment of methylene bluein industrial wastewater.

Description

technical field [0001] The invention relates to a titanium-based complex crystalline material based on thiacalix[4]arene, its preparation method and its application in the degradation of methylene blue light. Background technique [0002] A complex is a class of compounds with a characteristic chemical structure, which is formed by a central atom (or ion, collectively referred to as a central atom) and surrounding molecules or ions (called ligands / ligands) through coordination bonds. . Complexes are a relatively large subcategory of compounds and are widely used in daily life, industrial production and life sciences; they are not only related to inorganic compounds and organometallic compounds, but also to atomic cluster chemistry and coordination catalysis and molecular biology have a great intersection. The titanium-based complex is a complex formed with a titanium atom as the center, and the central titanium atom is combined with a ligand or other ions through a coordin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/28B01J31/22C02F1/30C02F101/30C02F101/38
CPCC07F7/003C07F7/28B01J35/004B01J31/1691B01J31/226C02F1/30C02F2305/10C02F2101/40C02F2101/308Y02W10/37
Inventor 王雅婷熊克才李鑫朱怡闫朝越张琰佘梓婧
Owner XUZHOU NORMAL UNIVERSITY
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