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5,10,15,20-tetrakis(4-carboxyphenyl)porphyrin with nanostructure and preparation method thereof

A carboxyphenyl, nanostructure technology, which is applied in the field of controllable preparation of 5,10,15,20-tetraporphyrin, can solve problems such as difficult to control nanostructure morphology, and achieves the effect of simple and feasible method.

Inactive Publication Date: 2019-05-24
熊子达
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above methods are difficult to control the morphology of nanostructures

Method used

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  • 5,10,15,20-tetrakis(4-carboxyphenyl)porphyrin with nanostructure and preparation method thereof
  • 5,10,15,20-tetrakis(4-carboxyphenyl)porphyrin with nanostructure and preparation method thereof
  • 5,10,15,20-tetrakis(4-carboxyphenyl)porphyrin with nanostructure and preparation method thereof

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preparation example Construction

[0016] A preparation method of 5,10,15,20-tetrakis(4-carboxyphenyl)porphyrin with nanostructure, comprising the steps of:

[0017] S1, provide 5,10,15,20-tetrakis(4-carboxyphenyl)porphyrin ammonium salt (hereinafter referred to as TCPP ammonium salt) and metal salt, and obtain metal TCPP complex (hereinafter referred to as TCPP ammonium salt) by reaction synthesis of TCPP ammonium salt and metal salt Abbreviated as MTCPP complex);

[0018] S2, provide the aqueous solution of sulfur anion releasing agent, make MTCPP complex and the aqueous solution of sulfur anion releasing agent react under acidic conditions, and sulfur anion releasing agent can slowly release S 2- ions; and

[0019] S3, centrifuging, washing, and precipitating the reaction product of the above-mentioned MTCPP complex and the aqueous solution of the sulfide-anion releasing agent, thereby obtaining TCPP with a nanostructure.

[0020] Preferably, in step S1, the metal salt is an inorganic metal salt or an orga...

Embodiment 1-5

[0030] 1mL H 2 TCPP-(COONH 4 ) 4 (1.5×10 -4 M) aqueous solution and 2mL Zn(NO 3 ) 2 (1.0×10 -2 The aqueous solution of M) was uniformly mixed under ultrasonic conditions, and then left standing in an oil bath at 80° C. for 16 hours. After the reaction, centrifuge at 13000 rpm / min, wash the precipitate twice with secondary water and acetonitrile respectively, and then disperse it in acetonitrile to obtain the ZnTCPP complex.

[0031] Take five 25mL round bottom flasks, add ZnTCPP (0.0009mmol TCPP) and disperse in 6mL acetonitrile, add 10mL thiourea aqueous solution (0.01M) under ultrasonic conditions, and react at 80°C for 10h. 5 mL each of 0.002M, 0.01M, 0.04M, 0.1M and 0.4M HCl (respectively Examples 1-5) was slowly added dropwise, and the reaction was continued for 4h.

[0032] After the above reaction is over, centrifuge the above reaction product at 13000rpm / min for 15min, remove the supernatant, and continue centrifuging and washing with 0.1M HCl for 3 times to pre...

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Abstract

The invention relates to a preparation method of TCPP with a nano structure. The preparation method comprises the following steps: S1, providing TCPP soluble salt and metal salt, and carrying out reactive synthesis on the TCPP soluble salt and the metal salt to obtain a metal TCPP porphyrin complex; S2, providing a solution of a sulfur negative ion releasing agent, and enabling the metal TCPP complex to react with the solution of the sulfur negative ion releasing agent under the acidic condition, wherein the sulfur negative ion releasing agent can release S2- ions when dissolved; and S3, centrifuging, washing and depositing a reaction product of the metal TCPP complex and an aqueous solution of the sulfur negative ion releasing agent so as to obtain TCPP with the nano structure. The invention further provides TCPP with the nano structure prepared by the method. In the method, the morphology of the nano structure of porphyrin can be regulated by controlling reaction acidity. The method is simple and practicable.

Description

technical field [0001] The application belongs to the field of preparation of organic nanomaterials, and in particular relates to a controllable preparation method of 5,10,15,20-tetrakis(4-carboxyphenyl)porphyrin (hereinafter referred to as MTCPP) with nanostructure. Background technique [0002] Organic nanocrystals have been widely concerned by researchers due to their wide applications in photoelectric conversion, molecular devices, sensors, etc. Using non-covalent interactions such as hydrogen bonding, π-π stacking, and electrostatic interactions, organic nanostructures with different morphologies have been prepared. At present, the methods for controlling the size and morphology of organic nanomaterials mainly include template method, self-assembly method and chemical vapor deposition method. However, the aforementioned methods are difficult to control the morphology of the nanostructures. [0003] In view of this, the present application is proposed. Contents of th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/22
CPCC07D487/22
Inventor 熊子达李永绣
Owner 熊子达
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