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Method for one-step preparation of manganese phthalocyanine crystal through solvothermal reaction

A solvothermal reaction and manganese phthalocyanine technology is applied in the field of preparation of metal phthalocyanine crystals, which can solve the problems of complex operations such as synthesis and purification of manganese phthalocyanine, high viscosity, etc., and achieves easy control of the reaction process, low energy consumption and low cost. Effect

Active Publication Date: 2014-08-20
XUCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the above methods can prepare manganese phthalocyanine, the preparation methods introduced in the above papers and monographs require relatively cumbersome operations to realize the synthesis and purification of manganese phthalocyanine
In addition, the solvent propylene glycol used is a low-toxic reagent, and the solvent has a relatively high viscosity, so the product purification in the later stage requires a sufficient amount of water and alcohol to clean it.

Method used

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  • Method for one-step preparation of manganese phthalocyanine crystal through solvothermal reaction
  • Method for one-step preparation of manganese phthalocyanine crystal through solvothermal reaction
  • Method for one-step preparation of manganese phthalocyanine crystal through solvothermal reaction

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Add 6 millimoles of phthalonitrile (769 mg), 1.5 millimoles of manganese acetate tetrahydrate (368 mg) into a 50 milliliter polytetrafluoroethylene material reactor liner, add 37.5 milliliters of absolute ethanol (The filling degree of the system is 75%). After stirring the reactants evenly with a glass rod, put the reaction kettle into a stainless steel jacket and close it tightly. The reaction kettle was placed in an oven at 190° C., and a solvothermal reaction was carried out at this temperature for a reaction time of 1 hour. After the reaction was completed, the heating was stopped, and the reaction was naturally cooled to room temperature. Use a small key to carefully take the black needle-shaped manganese phthalocyanine crystals out of the reactor, use hot water and hot ethanol to repeatedly rinse the remaining reactants adsorbed on the surface of the manganese phthalocyanine crystals, and vacuum dry at 100°C for 4 hours to obtain manganese phthalocyanine crystals ...

Embodiment 2

[0032] The preparation process and purification method are the same as in Example 1, only the solvothermal reaction time is 3 hours. SEM such as Image 6 shown by Image 6 It can be seen that the length of manganese phthalocyanine crystals has reached the order of millimeters.

Embodiment 3

[0034] The preparation process and purification method are the same as in Example 1, only the solvothermal reaction time is 6 hours. SEM such as Figure 7 shown by Figure 7 It can be seen that the manganese phthalocyanine quadrangular prism crystal is smooth and even.

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Abstract

The present invention relates to a method for one-step preparation of a manganese phthalocyanine crystal through a solvothermal reaction. The method comprises: adding phthalonitrile and manganese acetate tetrahydrate to a reaction kettle according to a molar ratio of 4:1, adding an anhydrous ethanol solution, uniformly stirring, sealing the reaction kettle, carrying out a solvothermal reaction for not less than 1 h at a temperature of 180-200 DEG C, stopping heating after completing the reaction, naturally cooling to a room temperature, taking out the prepared sample, adopting hot water and hot ethanol to repeatedly wash the remaining reactant adsorbed on the manganese phthalocyanine crystal surface, and drying to obtain the manganese phthalocyanine crystal. According to the present invention, the manganese phthalocyanine crystal prepared by using the method has the regular crystal appearance, and the whole preparation process has characteristics of simple operation, low cost, no harmful pollutant generation and easily controllable reaction process, and meets actual production requirements.

Description

technical field [0001] The invention relates to a method for preparing metal phthalocyanine crystals, in particular to a one-step rapid preparation method of manganese phthalocyanine (Manganese Phthalocyanine) or solvothermal reaction of manganese phthalocyanine crystals. Background technique [0002] Manganese phthalocyanine is a complex with planar macrocyclic structure with manganese ion as the coordination center and phthalocyanine skeleton as the ligand. Its molecular formula is C 32 h 16 MnN 8 . The manganese phthalocyanine molecule contains 16 π electrons, and all the atoms (C, N, H atoms) contained in the phthalocyanine skeleton are located in the same plane. This highly conjugated structure endows manganese phthalocyanine with unique properties, such as Acid and alkali resistance, water immersion resistance, light resistance and heat resistance, with highly stable physical and chemical properties. Manganese phthalocyanine can not only be used in traditional chem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/22
CPCC07D487/22
Inventor 李大鹏葛素香孙国富何琴黄保军郑直卢威玉田桂忠刘诗炎
Owner XUCHANG UNIV
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