A method of obtaining a fine crystalline copper phthalocyanine

 

(57) Abstract:

(57) the Invention relates to a process for the production of copper phthalocyanine (PcCu), which can be used as Krasotel sensor, the component of the photosensitive layer. The purpose of the invention is to simplify the process, obtaining PcCu in fine crystalline form. The aim is achieved in that the synthesis PcCu is carried out at a temperature of 20 - 40oC in N,N-dimethylformamide interaction 1,3-diaminoethane (HAI) with the ultrafine copper powder (UDP Cu) with a specific surface area greater than 30 m2/g, obtained by electrical explosion of the conductor in a nitrogen atmosphere, and mixing UDP Cu and INDIA is carried out in a dry form.

The invention relates to a method for phthalocyanine copper (PcCu), which is known as a pigment for coloring polymeric and composite materials used in the manufacture of sensors, photosensitive layers.

There is a method by which PcCu get from phthalimide, urea, copper or odnoklasniki copper, ammonium molybdate in the solvent at 170 - 210oC in the presence of cyanuric acid or its derivatives [1]. The disadvantages of this method are the high temperature and the duration of the process (45 hours), as well as neobhodimee closest to the present invention is a method of obtaining PcCu, includes heating the salts 1,3-diaminopentane with copper or copper compounds at 80 - 250oC in the presence of alkaline substances (or without) in a solvent that does not cause crystal growth PcCu or changes crystallographic modifications, for example, glycerol, polypropylenglycol, water or NH4OH. The output of CuPc is 80% [2]. The disadvantages of this method are the high temperature, the formation of relatively large crystals of the pigment micron sizes.

The aim of the invention is to reduce the reaction temperature, the simplification process and the receipt of copper phthalocyanine in fine crystalline form.

This objective is achieved in that the synthesis PcCu is carried out at a temperature of 20 - 40oC in N, N-dimethylformamide interaction 1,3-diaminoethane (HAI) with the ultrafine copper powder (UDP Cu) with a specific surface area greater than 30 m2/g, obtained by electrical explosion of the conductor in a nitrogen atmosphere, and mixing UDP Cu and INDIA carried out dry. The use of copper powder in ultra-fine condition obtained by electrical explosion of conductors in a nitrogen atmosphere, makes it a special status. In the ultra-small particle number energy in total energy of the particle becomes comparable to the contribution of bulk energy. The explosion of the metal conductor is at a voltage of tens of kilovolts in the gas environment and is accompanied by formation on the surface of the particles is unstable and unusual chemical conditions of the conductor material and components in this environment.

Example 1. To 0.5 g (0,0079 mol) of ultra-fine copper powder (UDP Cu) obtained in nitrogen atmosphere with a specific surface area Sbeats30 m2/g add equimolecular amount of 1,3-diaminoethane (HAI) (4.6 g, 0,0316 m), the mixture is stirred, placed in the reaction vessel, add 30 ml of N,N-dimethylformamide (DMF) and stirred at 20oC for 3 hours. Then the reaction mixture was filtered through a glass filter. The precipitate successively washed with 1% hydrochloric acid, water, methanol, acetone until the discoloration of wash liquid. The product is dried at a temperature of 60 - 80oC. Yield 4.0 g (88%). The IR spectrum of the obtained copper phthalocyanine (PcCu) are identical in the number and position of the vibration frequencies literature data for PcCu [3]. Electronic spectrum of the product in 1-chloronaphthalene contains an intensive absorption band at 679 mm shoulder at 679 mm shoulder at 611 mm Position of these bands is consistent with the spectrum in the visible region data by the method of electron microscopy correspond fine needle shape with dimensions of length not more than 0.2 μm in width < 0.05 microns.

Example 2. Into the reactor containing 10 ml of DMF, add the mixture prepared as in example 1 from 0.05 g (0,79 mmol) UDP Cu (N2, Sbeats30 m2/g) and 0.46 g (3,16 mmol) of INDIA, and mix it with the 30oC for 2 hours. Then the reaction mass is passed through a glass filter, the precipitate washed with 1% HCl, water, methyl alcohol, acetone, and then dried. The yield of 0.41 g (90%). Spectral characteristics, elemental analysis and dispersion of the product correspond to the data of example 1.

Example 3. UDP Cu (N2, Sbeats30 m2/g), HAI and DMF are mixed in the amounts and order of priority as described in example 1. Stirred at 40oC for 1.5 hours. Phthalocyanine copper allocate analogously to example 1. Yield 89%. The spectral characteristics, the results of the elemental analysis and the pigment dispersion are consistent with the characteristics of the product of example 1.

Example 4. The reactor is placed DMF and add a mixture of INDIA and UDP Cu (N2, Sbeats70 m2/g) in amounts as in example 2. Maintain the reaction mixture at 40oC for one hour and produce similarly to the procedure described in example 2. The yield of 0.42 g (95%). The spectral characteristics, the results of elemental analysis, weliswaar mild conditions opens the possibility to control the process of obtaining PcCu, free from high temperature impurities in fine condition with a high yield.

A method of obtaining a fine of copper phthalocyanine by the interaction of 1,3-diaminoethane with copper powder in the environment of the solvent, characterized in that the quality of the copper powder used ultra-fine copper powder with a specific surface area greater than 30 m2/g, obtained by electrical explosion of the conductor in a nitrogen atmosphere, the interaction of lead in N,N-dimethylformamide at 20 40oC, and the mixing ultrafine copper powder and 1,3-diaminoethane carried out in a dry form.

 

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