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A technology of iron phthalocyanine and iron salt, which is applied in the field of compound preparation and can solve problems such as health hazards
Inactive Publication Date: 2015-01-28
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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However, the traditional solvent method mostly uses trichlorobenzene or p-nitrotoluene as a solvent, and the use of these two solvents has serious harm to human health.
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[0026] In a 250 mL three-neck flask, add 2 g of iron salt (ferrous chloride, 10 mmol), 4 g of phthalic anhydride (27 mmol), 8.1 g of urea (133 mmol), and 24 mL of dioctyl phthalate in sequence, and feed After completion, heat and stir. When the temperature reaches 130°C, add 0.12 g ammonium molybdate (0.6 mmol) and 0.147 g ammonium chloride (2.7 mmol) and keep the reaction for 2 h until the reactant has no bubbles, then you can proceed to the next step Reaction; the heating process is about 1°C / min, and the temperature is directly raised to 190°C, and the reaction is held for 6 hours. After the reaction, the reaction temperature will be lowered to room temperature; Put it into 100 mL ethanol, stir and heat to 40°C and filter, then put the filter cake into 100 mL water, add 0.5 g sodium dodecylbenzenesulfonate at the same time, heat to 80°C and stir for 30 min, filter and dry to get the product iron phthalocyani...
[0029] In a 250 mL three-necked flask, 1.7 g of iron salt (ferrous sulfate, 10 mmol), 4 g of phthalic anhydride (27 mmol), 8.1 g of urea (133 mmol), and 26 mL of recovered dioctyl phthalate were successively added. After the feeding is completed, heat and stir. When the temperature reaches 120~140°C, put in 0.12 g ammonium molybdate (0.6 mmol) and 0.147 g ammonium chloride (2.7 mmol), and keep it warm for 1 hour until the reactant has no bubbles, then it can be carried out The next step of the reaction: the reaction product of a, the heating process is about 1°C / min, the temperature is directly raised to 180°C, and the temperature is kept for 4 hours. After the reaction, the reaction temperature will be lowered to room temperature; the product is filtered, and the filtrate is recovered. Dioctyl phthalate About 21 mL, put the filter cake into 100 mL ethanol, stir and heat to 40°C for filtration, then...
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Abstract
The invention discloses a preparation method of iron phthalocyanine, and relates to a preparation method of a compound, the method uses ferrous metal salt, phthalic anhydride and urea as raw materials, phthalic acid ester as a solvent, ammonium molybdate as a catalyst, and ammonium chloride as a catalyst aid, and a solvent synthesis method is used. The synthetic method comprises two stages: (1) reacting for 0.5-2 h at 120 to 140 DEG C; and (2) reacting for 2-8 h at 180 to 240 DEG C. The reaction solvent is the phthalic acid ester such as dioctyl phthalate which is greener and more environmentally friendly compared with a traditional solvent such as paranitrotoluene and trichlorobenzene, the high yield of the reaction proves that the method is effective in industrialization. Through use of the dioctyl phthalate (DOP) as the green solvent, reaction condition is improved, the whole production process is more environmentally friendly, by use of the dioctyl phthalate (DOP) as the solvent, a higher yield is ensured, and at the same time, the dioctyl phthalate can also be recycled.
Description
technical field [0001] The invention relates to a compound preparation method, in particular to a method for preparing iron phthalocyanine. Background technique [0002] Phthalocyanine compound is a compound accidentally obtained by Braun and Tchemia in an experiment in 1907. The new term Phthalocyanine (phthalocyanine) was created by the famous British scholar Professor Linstead in 1933. It has been less than 100 years since its discovery. , People have invented more than 5000 kinds of phthalocyanine compounds. The structure of phthalocyanine is as follows: [0003] [0004] Phthalocyanine is a two-dimensional planar macrocyclic conjugated molecule with 18 electron aromatic structures, and the two hydrogen atoms in the center of the ring (no metal phthalocyanine, such as a, can be replaced by a large number of chemical elements (metal phthalocyanine, Such as b. At the same time, the sixteen hydrogen atoms on the four benzene rings around the phthalocyanine molecule...
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