Process for preparing polycrystalline oxotitanium phthalocyanine in mixed crystal regulator

A technology of titanium phthalocyanine and regulator, applied in the direction of titanium organic compounds, etc., can solve the problems of complex process, low efficiency and long time, and achieve the effect of simple process, high efficiency and short time

Inactive Publication Date: 2005-03-16
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] To realize the preparation of the above-mentioned polycrystalline titanyl phthalocyanine, it needs to be carried out in different crystal regulators, the process is complicated, the time is long, and the efficiency is low

Method used

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  • Process for preparing polycrystalline oxotitanium phthalocyanine in mixed crystal regulator
  • Process for preparing polycrystalline oxotitanium phthalocyanine in mixed crystal regulator
  • Process for preparing polycrystalline oxotitanium phthalocyanine in mixed crystal regulator

Examples

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Effect test

example 1

[0013] In a 250 mL three-necked flask equipped with a stirrer and a thermometer, add 90 mL of o-dichlorobenzene and 10 mL of butanol, and then add 4 g of purified titanyl phthalocyanine. Stir at room temperature for 20min, then heat to 55°C and stir for 6h. Cool to room temperature, add 100 mL of water, stir for 30 min and then filter, wash the filter cake with a large amount of methanol, and dry to obtain Y-TiOPc.

example 2

[0015] In a 250 mL three-necked flask equipped with a stirrer and a thermometer, add 60 mL of o-dichlorobenzene and 40 mL of butanol, and then add 4 g of purified titanyl phthalocyanine. Stir at room temperature for 30min, then heat to 60°C and stir for 6h. After cooling to room temperature, 120 mL of methanol was added, stirred for 30 min and then filtered. The filter cake was washed with a large amount of methanol and dried to obtain β-TiOPc.

example 3

[0017] In a 250 mL three-necked flask equipped with a stirrer and a thermometer, add 20 mL of o-dichlorobenzene and 80 mL of butanol, and then add 4 g of purified titanyl phthalocyanine. Stir at room temperature for 40min, then heat to 65°C and stir for 6h. After cooling to room temperature, 150 mL of ethanol was added, stirred for 30 min and then filtered. The filter cake was washed with a large amount of methanol and dried to obtain α-TiOPc.

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Abstract

The invention provides a process for preparing polycrystalline form oxytitamium phthalocyanine from the miscible liquidof orthodichlorobenzene and butyl alcohol which consists of the steps of, using orthodichlorobenzene and different volume ratio of butyl alcohol mixed liquid as crystal system modifier, charging purified oxytitamium phthalocyanine, agitating, elevating the temperature to 40-80 deg. C, stirring 4-8h again, cooling down and charging water as precipitating agent, methanol, ethanol or propanol solvent, stirring and filtering, washing the filter cake and drying.

Description

technical field [0001] The invention relates to a method for preparing polymorphic titanyl phthalocyanine (TiOPc) with a mixed solution of o-dichlorobenzene and butanol. It belongs to the crystal form preparation technology of titanium phthalocyanine. Background technique [0002] Titanium phthalocyanine is an important class of organic photoconductive materials, and the crystal form has a great influence on its photoconductivity. Its crystal forms are as follows: α, β, γ, m, amorphous, Y, A, B. Among them, the existing preparation methods of α, β, and Y types are as follows: α-type samples are obtained by soaking crude products or sublimated samples in acetone or washing for 5 weeks with a Soxhlet extractor; β-type samples are obtained by using N-methyl Treat the α crystal sample with pyrrolidone for more than 15 hours, and wash it with methanol until there is no brown color; Y-TiOPc is prepared by treating the amorphous sample with 1,2-dich...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/28
Inventor 李祥高王文保王世荣侯薇
Owner TIANJIN UNIV
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