Synthetic method of unsubstituted zinc phthalocyanine

A synthesis method and technology of zinc phthalocyanine, applied in the field of synthesizing unsubstituted zinc phthalocyanine, can solve the problems of complex purification method, long reaction time, high reaction temperature, etc., and achieve the effects of low production cost, simple synthesis method and low reaction temperature

Inactive Publication Date: 2015-12-09
LIAONING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But these three kinds of methods not only all need to add catalyst, reaction temperature is higher, reaction time is longer, and purification method is complicated, therefore, it is very important to develop a kind of simple, economical, efficient new method to prepare metal phthalocyanine to satisfy market demand necessary

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  • Synthetic method of unsubstituted zinc phthalocyanine
  • Synthetic method of unsubstituted zinc phthalocyanine
  • Synthetic method of unsubstituted zinc phthalocyanine

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Experimental program
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Embodiment 1

[0018] Embodiment 1 The synthetic method of unsubstituted zinc phthalocyanine

[0019] Add 0.878g (4.0mmol) of zinc acetate dihydrate and 2.05g (16.0mmol) of phthalonitrile to 30ml of DMF solvent in sequence, and react in a hydrothermal reaction kettle at 150°C for 4h, stop the reaction and cool to At room temperature, the color of the solution was bright blue, and 300ml of ether was added. That is, a large amount of solid precipitated out and was suction filtered. The precipitate was repeatedly washed with dichloromethane and filtered with suction to obtain a large amount of purple-black solid, which was dried in vacuo to obtain 1.78 g of solid powder with a yield of 77%.

[0020] Elemental analysis (C 32 h 16 N 8 Zn), measured value (theoretical value) %: C66.82 (66.51), H2.69 (2.79), N19.14 (19.39).

[0021] figure 1 is the UV-Vis absorption spectrum of unsubstituted zinc phthalocyanine in DMF solvent. It can be seen from the figure that 600-800nm ​​is the Q-band cha...

Embodiment 2

[0022] The synthetic method of embodiment 2 unsubstituted zinc phthalocyanines

[0023] Add 0.878g (4.0mmol) of zinc acetate dihydrate and 2.05g (16.0mmol) of phthalonitrile to 30ml of DMF solvent in sequence, and react in a hydrothermal reaction kettle at 150°C for 4h, stop the reaction and cool to At room temperature, the color of the solution was bright blue, and 300ml of acetone was added. That is, a large amount of solid precipitated out and was suction filtered. The precipitate was repeatedly washed with dichloromethane and filtered with suction to obtain a large amount of purple-black solid, which was dried in vacuo to obtain 1.6 g of solid powder with a yield of 69%.

Embodiment 3

[0024] The synthetic method of embodiment 3 unsubstituted zinc phthalocyanines

[0025] Add 0.878g (4.0mmol) of zinc acetate dihydrate and 2.05g (16.0mmol) of phthalonitrile to 30ml of DMF solvent in sequence, and react in a hydrothermal reaction kettle at 150°C for 4h, stop the reaction and cool to At room temperature, the color of the solution was bright blue, and 300ml of ethyl acetate was added. That is, a large amount of solid precipitated out and was suction filtered. The precipitate was repeatedly washed with dichloromethane and filtered with suction to obtain a large amount of purple-black solid, which was dried in vacuo to obtain 1.55 g of solid powder with a yield of 67%.

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Abstract

The invention relates to a synthetic method of unsubstituted zinc phthalocyanine. The synthetic method is characterized by comprising the steps of using metallic zinc salt and phthalic nitrile as raw materials, using DMF as a solvent, and performing a reaction of the metallic zinc salt and the phthalic nitrile in the DMF at the temperature of 130-170 DEG C in a hydrothermal reaction kettle so as to obtain target products. The synthetic method disclosed by the invention is low in reacting temperature and short in reacting time, does not need any catalysts; and the method is simple, low in production cost, high in yield and purity and good in repeatability, so that the synthetic method can meet requirements for large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, in particular to a method for synthesizing unsubstituted zinc phthalocyanine. Background technique [0002] Metal phthalocyanine is a symmetrical complex of planar conjugated aromatic system with 18 π electrons, which has high stability, structural flexibility and good spectral properties. In 1907, it was accidentally discovered by Braun and Tchemiac in England in an experiment, and it has a history of more than 100 years. This kind of compound is a very important variety in organic synthetic pigments. They have excellent color strength and fastness, and are widely used in the fields of plastics, coatings and inks, and are also important raw materials for the production of electrophotographic photoreceptors and optical discs. At present, there are three main methods for the preparation of phthalocyanine: ammonium molybdate solid-phase catalytic method, inert solvent method and DBU liquid-phase ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/22
CPCC07D487/22
Inventor 张薇李国琴孙颖于媛媛宋溪明
Owner LIAONING UNIVERSITY
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