Hyperbranched CTP-TPY (Cyclotriphosphazene Terpyridyl), preparation method and recognition method of metal ions

A technology of terpyridine and tripolymer phosphazene, which is applied in chemical instruments and methods, organic chemistry, fluorescence/phosphorescence, etc., can solve the problems of weak recognition ability and single recognition site, and achieve rapid response, high selective recognition ability, Simple operation effect

Active Publication Date: 2017-02-22
CHONGQING UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the commonly used carriers in zinc ion fluorescent sensors are pyridine derivatives such as BPA

Method used

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  • Hyperbranched CTP-TPY (Cyclotriphosphazene Terpyridyl), preparation method and recognition method of metal ions
  • Hyperbranched CTP-TPY (Cyclotriphosphazene Terpyridyl), preparation method and recognition method of metal ions
  • Hyperbranched CTP-TPY (Cyclotriphosphazene Terpyridyl), preparation method and recognition method of metal ions

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0034] Example 1: Preparation of hexa(4-carbaldehyde phenoxy) cyclophosphazene (CTP-CHO):

[0035] In a 250ml single-necked flask, 100ml of tetrahydrofuran, 2.50g (7.19mmol) of hexachlorocyclotriphosphazene, 6.30g (51.59mmol) of p-hydroxybenzaldehyde, 11.38g (82.30mmol) of potassium carbonate, and 11.38g (82.30mmol) of potassium carbonate were added to the flask with heating and stirring at 66 degrees. Condensate and reflux for 48h.

[0036] After the reaction is complete, change to a distillation device to distill off the solvent tetrahydrofuran, then add the product to 1000ml of distilled water, stir for half an hour, get a white precipitate at rest, filter with suction, wash with distilled water three times, and place it in a vacuum drying cabinet to dry at 60 degrees. The product was recrystallized from ethyl acetate to obtain the product hexa(4-formaldehyde phenoxy) cyclophosphazene (CTP-CHO). The reaction equation is as follows:

[0037]

[0038] As attached figure 1 It can b...

Example Embodiment

[0039] Example 2: Preparation of hyperbranched polyphosphazene terpyridine CTP-TPY:

[0040] Add 4.04 g (4.14 mmol) of hexa(4-formaldehyde phenoxy) cyclophosphazene, 7.18 g (55.68 mmol) of 2-acetylpyridine, 120 ml of absolute ethanol and 200 ml of tetrahydrofuran to a 500 ml three-necked flask to completely dissolve Then a light yellow solution was obtained, then 3.894g (55.68mmol) of potassium hydroxide KOH and 90ml of ammonia were added, and stirred at room temperature. The solution became light brown. After 12 hours of reaction, the reaction was stopped and the tetrahydrofuran was removed by rotary evaporation with a rotary evaporator to obtain A large amount of milky yellow precipitate was filtered, and then washed 2-3 times with a large amount of absolute ethanol to obtain a milky yellow powder, which was placed in a vacuum drying oven at 60°C and dried overnight. The reaction process is as follows:

[0041]

[0042] As attached figure 2 It can be seen from the mid-infrared ...

Example Embodiment

[0045] Example 3: The selective recognition of various metal ions by hyperbranched trimeric phosphazene terpyridine CTP-TPY, the fluorescence titration process is as follows:

[0046] 1. Use a 50ml volumetric flask to prepare supramolecular trimeric phosphazene terpyridine CTP-TPY solution, the solvent is tetrahydrofuran, and the concentration of the solution is 1×10 -4 mol / L.

[0047] 2. Use a 50ml volumetric flask to prepare Zn separately 2+ , Ni 2+ , K + , Mg 2+ , Na + , Fe 3+ , Ca 2+ , Ba 2+ , Pd 2+ , Hg + , Cu 2 + , Li + , Co 2+ , Eu 3+ , Tb 3+ 15 kinds of metal cation ethanol solutions, the concentration of the solution is 1×10 -2 mol / L.

[0048] 3. All fluorescence titration experiments are carried out under the condition of 25±0.5℃, the body (CTP-TPY) used in each titration experiment is 3mL, and the metal cation solution is gradually dripped from 5ul, 10ul, 20ul, 30ul, and 60ul. After each instillation, use a dropper to mix well and then perform the fluorescence test 3 minut...

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Abstract

The invention relates to Hyperbranched CTP-TPY (Cyclotriphosphazene Terpyridyl), a preparation method and a recognition method of metal ions, and belongs to the field of luminescent materials. Firstly, a CTP-TPY multi-core ligand is compounded; then, fluorescence spectrum titration on various metal ions by a cyclotriphosphazene derivative and a hyperbranched triphosphazene derivative is researched, ultraviolet and fluorescent responses of the cyclotriphosphazene derivative and the hyperbranched triphosphazene derivative on different metal ions are detected, and a result verifies that rare earth europium ions and zinc ions can be well recognized by CTP-TPY. The hyperbranched CTP-TPY disclosed by the invention has better photoluminescence performance and electroluminescence performance, high stability, good solubility and low cost; the preparation method is relatively low in cost, simple in operation, low in risks and easy to promote and use. The hyperbranched CTP-TPY has six coordination sites, so that metal Eu<3+> and Zn<2+> can be more effectively recognized, the selective recognition ability is high, and response is rapid.

Description

technical field [0001] The invention relates to the field of luminescent materials, in particular to a hyperbranched tripolyphosphazene terpyridine, a synthesis method thereof, and a method for identifying metal ions. Background technique [0002] Supramolecular chemistry can imitate many special functions of substances that already exist in nature and form some new materials. Now it has developed into supramolecular science that intersects with life science, material science, nanoscience, information science and other disciplines. Supramolecular devices, supramolecular biomaterials, supramolecular capsules, liquid crystal materials, tissue or organ substitutes, nanomaterials, new polymers and LB membrane materials all have broad application prospects, and are new materials and high-tech in the 21st century. important development. In the process of developing supramolecular materials, how to make good use of the unique properties of supramolecular materials to develop more ...

Claims

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Application Information

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IPC IPC(8): C07F9/6593G01N21/64
CPCC07F9/65815G01N21/643G01N2021/6443
Inventor 杨朝龙苏艳李又兵王国霞陈少棚邓伟梁迎春
Owner CHONGQING UNIV OF TECH
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