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A kind of preparation method of metal phthalocyanine compound

A metal phthalocyanine and compound technology, which is applied in the field of preparation of metal phthalocyanine compounds, can solve the problems of complex post-processing operations of products, difficulty in mixing uniform raw materials, and insufficient reaction of raw materials, and achieve broad industrial application prospects, short reaction time, good thermal stability

Inactive Publication Date: 2016-05-25
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a preparation method of metal phthalocyanine compounds to solve the problem that raw materials are not easy to mix evenly, insufficient reaction of raw materials, low product yield and long reaction time Long and complex product post-processing operations

Method used

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  • A kind of preparation method of metal phthalocyanine compound
  • A kind of preparation method of metal phthalocyanine compound
  • A kind of preparation method of metal phthalocyanine compound

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Experimental program
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Effect test

Embodiment 1

[0018] 7.51g of tetrachlorophthalic anhydride, 1.52g of CoCl 2 ·6H 2 O, 12.6g urea, 0.50g p-toluenesulfonic acid (C 7 h 8 o 3 S·H 2 O) As for the Erlenmeyer flask, the mouth of the flask is sealed with a rubber stopper. Stir magnetically in an oil bath at 100°C for 10 minutes, take it out, and then place it in a Midea KD20C-CF(8)00001691 microwave oven (other microwave ovens can also be used) to heat for 3 minutes at 700W and 4 minutes at 350W, and a dark green powder appears. As for 40ml98% (mass concentration) concentrated H 2 SO 4 Dissolve, then pour into 1500ml of deionized water, and filter. Wash the filter cake with 20ml of 10% (mass concentration) NaOH solution, then wash with water to pH = 7, and wash with 10% BaNO 3 (mass concentration) test until no precipitation. The solid was dried at room temperature to give 3.87g. The yield was 70.02%.

[0019] The following figure shows the structural formula of metal phthalocyanine compounds:

[0020]

[0021] Th...

Embodiment 2

[0025] 4.90g of phthalic anhydride, 18.43g of urea, 2.45g of manganese acetate (C 4 h 6 MnO 4 4H 2 O), 0.8gC 7 h 8 o 3 S·H 2 O As for the Erlenmeyer flask, the mouth of the bottle is sealed with a rubber stopper. Stir magnetically in an oil bath at 100°C for 10 minutes, take it out, and then place it in a Midea KD20C-CF(8) 00001691 microwave oven for 3 minutes at 600W and 4 minutes at 350W, a blue-black powder appears, and put the powder in 25ml of 98% concentrated H 2 SO 4 Dissolve, pour into 1000ml of deionized water, and filter. Wash the filter cake with 20ml of 10% NaOH solution, then wash with water to pH = 7, and wash with 10% BaNO 3 The manganese phthalocyanine compound can be obtained by checking until there is no precipitation. The solid was dried at room temperature to give 3.54 g. The yield was 75.01%.

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Abstract

The invention discloses a preparation method for phthalocyanine compound. The preparation method for phthalocyanine compound comprises the following steps: firstly, adding raw materials of phthalic anhydride or derivative thereof, metallic compound, and carbamide into a cone-shaped bottle in a mixed manner, and adding 2wt% para-toluenesulfonic acid compound as catalyst; sealing the opening of the bottle, placing the bottle into an oil bath pan to heat and fuse, stirring for 10 minutes under 80-125 DEG C, and enabling the raw materials to uniformly mix; further placing in a domestic microwave oven to heat for 2-5 minutes in high power, using a glass rod to uniformly stir, and further placing in the domestic microwave oven to heat in low power, pouring into deionized water after using concentrated sulfuric acid to dissolve acquired products, using a vacuum pump to filter, using 10% sodium hydroxide (NaOH) solution to wash the products to a state that potential of hydrogen (pH) is equal to 7, and further using distilled water to wash until the 10% NaOH solution has no sediment through detections. Phthalocyanine compound is acquired after the products are dried. The preparation method for phthalocyanine compound has the advantages of being high in yield, short in reflection time, low in power consumption, high in heat stability, simple in final treatment, low in pollution and applicable to industrial production.

Description

technical field [0001] The invention relates to a method for preparing a metal phthalocyanine compound, in particular to a method for rapidly polymerizing reaction raw materials to synthesize a metal phthalocyanine compound in a household microwave oven. Background technique [0002] Phthalocyanine compound is an excellent functional material with good chemical properties, catalytic activity, thermal stability and light stability. The unique physical and chemical properties of phthalocyanines make them widely used in the frontier fields of catalytic chemistry, photochemistry, electrochemistry, nonlinear optics, crystal chemistry, superconducting physics, information materials and medicine. [0003] In recent years, there have been many studies on the synthesis methods of metal phthalocyanine complexes. There are usually two ways to synthesize them: one is the phthalocyanine method with phthalocyanine and the corresponding metal salt as the starting material; the other is the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/22
Inventor 张娟李俊盼任腾杰刘猛帅李润泽胡彦荟侯晓燕
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY