CN102443008A - Hydrothermal synthesis method of copper phthalocyanine - Google Patents

Abstract

The invention discloses a hydrothermal synthesis method of copper phthalocyanine, belongs to the technical field of organic synthesis, and relates to a contract method of copper phthalocyanine. The method comprises the following steps: (1) taking 0.1mmol copper salt and 0.4mmol indole as starting materials, putting the starting materials into a steel bomb with a polytetrafluoroethylene lining, and adding 4mmL water; (2) tightening the steel bomb; (3) putting the steel bomb in an oven, controlling the temperature at 60-90 ℃, reacting for 50-70min, and cooling to room temperature; (4) cooling, filtering, and washing with methanol to obtain purple acicular copper phthalocyanine. The method greatly shortens the growth time of the single crystal, and has high success rate; the single crystal with the thickness of about 10.0mm can be grown in a short time, the success rate is 100%, the equipment is simple, and the cost is low.

Description

Hydrothermal Synthesis of Copper Phthalocyanine

technical field

The invention belongs to the technical field of organic synthesis, and relates to a contract method of copper phthalocyanine, in particular to a hydrothermal synthesis method of copper phthalocyanine.

Background technique

Phthalocyanine is a highly stable two-dimensional aromatic system with 18π electrons. More than 70 different metals and nonmetals can be used as the central atom of phthalocyanine. Generally, the conjugated system of phthalocyanine refers to a system composed of 18-π electron aromatic cloud delocalization system, which is composed of nine carbon-nitrogen conjugated double bonds, and these nine carbon-nitrogen or carbon-carbon conjugated double bonds "Surround" the central cavity of phthalocyanine molecules. The unique molecular structure of phthalocyanine or metal phthalocyanine determines that they can be substituted by various groups in different ways. So far, more than 5,000 kinds of phthalocyanine compounds have been synthesized. Group substitution changes the structure of the molecule, and the difference in structure causes changes in properties and functions.

At present, single crystals of phthalocyanine compounds cannot be directly obtained from synthesis, and the method of recrystallization of concentrated sulfuric acid solution is often used to cultivate single crystals of phthalocyanine compounds; vapor phase physical deposition method, the growth of single crystals by vapor phase physical deposition method is relatively short, the longest is 5mm; solution gradient cooling method, the method of liquid gradient cooling has a long growth cycle, about 80 hours. In short, these methods all have the disadvantage of long growth period, and because of the small size of the obtained crystal, low success rate, loss of solution or carrier gas during the crystal growth process, and difficulty in separating the crystal from the medium, etc. Crystal growth is inconvenient.

Contents of the invention

The object of the present invention is in order to provide a kind of hydrothermal synthesis method of copper phthalocyanine.

The present invention is achieved through the following technical solutions:

The hydrothermal synthesis method of copper phthalocyanine comprises the following steps:

(1) Using 0.1mmol copper salt and 0.4mmol indole as the starting material, put the starting material into a steel bomb with a Teflon liner, and add 4mmL of water;

(2) Tighten the steel bullet;

(3) Put the steel bomb in an oven, control the temperature at 60-90°C, react for 50-70 minutes, and cool to room temperature;

(4) After cooling, filter and rinse with methanol to obtain purple needle-shaped copper phthalocyanine.

Further, the copper salt is copper chloride.

The present invention uses copper salt and indole as raw materials, heats in water, and directly synthesizes the metal phthalocyanine compound, and the chemical reaction equation is as follows:

The molecular formula of purple needle-shaped copper phthalocyanine is C ₃₂ H ₁₆ CuN ₈ , the yield can reach 70%, and the single crystal is about 10.0mm in size.

The method of the invention solves the problems of long growth period, low success rate and high cost of phthalocyanine compound crystals, and further provides a new approach for preparing related organic functional molecular material single crystal samples and optoelectronic devices using single crystals as materials.

The method of the invention greatly shortens the single crystal growth time, and the success rate is very high; a single crystal of about 10.0mm can be grown in a short time, and the success rate is 100%, and the equipment is simple and the cost is low.

Description of drawings

Fig. 1 is a molecular structure diagram;

Figure 2 is a molecular packing structure diagram.

Detailed ways

Example 1

The hydrothermal synthesis method of copper phthalocyanine comprises the following steps:

(1) Using 0.1mmol copper salt and 0.4mmol indole as the starting material, put the starting material into a steel bomb with a Teflon liner, and add 4mmL of water;

(2) Tighten the steel bullet;

(3) Put the steel bomb in an oven, control the temperature at 60°C, react for 70 minutes, and cool to room temperature;

(4) After cooling, filter and rinse with methanol to obtain purple needle-shaped copper phthalocyanine.

The molecular structure diagram is shown in Figure 1. The molecular formula of copper phthalocyanine is CuN ₈ C ₃₂ H ₁₆ , the single crystal space group is P2(1)/n, and the parameters are: a =14.668(3), b= 4.8109(10), c=19.515(7), α=90, β=121.04(2), γ=90, unit volume is 1179.91(Å) ³ , according to the above parameters, this crystal form belongs to β-form.

The molecular packing structure diagram is shown in Fig. 2 .

Example 2

The hydrothermal synthesis method of copper phthalocyanine comprises the following steps:

(1) Using 0.1mmol copper chloride and 0.4mmol indole as starting materials, put the starting materials into a steel bomb with a Teflon liner, and add 4mmL water;

(2) Tighten the steel bullet;

(3) Put the steel bomb in an oven, control the temperature at 70°C, react for 50 minutes, and cool to room temperature;

(4) After cooling, filter and rinse with methanol to obtain purple needle-shaped copper phthalocyanine.

Example 3

The hydrothermal synthesis method of copper phthalocyanine comprises the following steps:

(1) Using 0.1mmol copper salt and 0.4mmol indole as the starting material, put the starting material into a steel bomb with a Teflon liner, and add 4mmL of water;

(2) Tighten the steel bullet;

(3) Put the steel bomb in an oven, control the temperature at 90°C, react for 60 minutes, and cool to room temperature;

(4) After cooling, filter and rinse with methanol to obtain purple needle-shaped copper phthalocyanine.

Claims (1)

1. the hydrothermal synthesis method of a CuPc is characterized in that may further comprise the steps:

(1) is starting raw material with 0.1mmol mantoquita and 0.4mmol indoles, is put into starting raw material and has in the teflon-lined steel bomb, add 4mmL water;

(2) tighten steel bomb;

(3) be placed on steel bomb in the baking oven, controlled temperature behind the reaction 50-70min, is cooled to room temperature at 60-90 ℃;

(4) cooled and filtered is used washed with methanol then, promptly gets the acicular CuPc of purple.

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